Microwave Materials PDF
Microwave Materials PDF
Microwave Materials PDF
Microwave Materials
EDITORS
V.R.K. Murthy
S. Sundaram
B. Viswanathan
All rights reserved. No part of this publication may be reproduced, stored in a retrieval
system or transmitted in any form or by any means, electronic, mechanical, photocopying,
recording or otherwise, without the prior permission of the publisher
All export rights for this book vest exclusively with Narosa Publishing House.
Unauthorised export is violation of Copyright Law and is subject to legal action
V.R.K. MURTHY
S. SUNDARAM
B. VISWANATHAN
Contents
Preface v
T. Rs. Reddy
Hybrid Microelectronics Division
Defence Electronics Research Laboratory
Hyderabad. India
1. INTRODUCTION
Microwave Integrated Circuits (MICs), more precisely Hybrid Microwave
Integrated Circuits represent an important and significant step towards the
integration and miniaturization of the microwave subsystems and systems when
compared to those based on the waveguide/coaxial components. But the level
of integration is less than that encountered in the Monolithic Microwave Integrated
Circuits (MMICs). In spite of the advent of MMICs, however, MICs continued
to assert their place in the microwave systems due to some of their unique
features which cannot be fully met otherwise. Also MIC technology adopted
itself to the integration of MMICs functional chips in realising the microwave
systems. MICs span the range from printed circuit board where the integration
is limited to realising the conductor pattern, to the hybrid circuits (thin and
thick film) where some or all of the passive components are integrated along
with the conductor pattern. Since at microwaves frequencies the circuit dimensions
tend to be of the order of the wavelength, every element of the microwave
circuit influences its performance (Bhat and Koul1989 and Van Nie, Goedbloed
and Kersuzan 1981). This in tum reflects on the choice of the materials that
are used to fabricate the MICs. The quality requirements are more demanding
for the materials used for the fabrication of MICs than for the low frequency
circuits. In the present chapter efforts are made to highlight various aspects
related to some of the materials used for the fabrication of MICs.
2. TYPES OF MICs
Different types of circuit configuration have been used for the propagation of
microwaves and in realising various circuit elements such as inductors, capacitors
and resistors. Broadly these can be classified into two categories namely
distributed element and lumped element. While in the former case the realisation
of inductor and capacitor is related to specific configuration of the transmission
2 MICRowAVE MATERIALS
line, in the latter case these are realised as lumped elements analogous to those
in the low frequency circuits. 1n order that these behave as lumped elements
it should be ensured that their overall sizes do not exceed 1/10 of the wave-
length of the microwaves in the medium in which the elements are realised. In
real situation however the circuit tends to have mixed features while predominantly
tending to be either one of these types.
Most commonly employed circuit configurations include: (I) Suspended
line (strip line), (2) Microstrip line, (3) Coplanar line, (4) Slot line and (5)
Finline. Typical circuit configurations for some of these are shown in Fig. 1.
In almost all cases there is a conductor circuit pattern laid out on a dielectric
substrate. In some cases the passive components such as inductors, capacitors
and resistors are realised in situ and in others are attached to the circuit as
discrete components. Invariably the active components (devices) are attached
as separate elements and interconnections are made to the circuit lines
through one of the several means discussed below. Active devices can
Coplanar
Slot Line
D Dielectric Substrate
_ Metallization
3. SUBSTRATE
The substrate supporting the circuit is a dielectric with metallisation on either
side. The circuit pattern is printed on one or both sides by photolithographic
process. A brief description of the photolithographic fabrication process is in
order to appreciate the requirement of the materials for the substrate and the
metallization.
4. High DC resistance.
S. Easy machinability for sizing, making holes etc.
6. Provide smooth surface for metallization.
7. High thermal conductivity for high power applications.
8. Uniformity of these properties over the substrate area.
fmm:mi!m~m:m~ <- Metallization
Clean Substrate
<- Dielectric Base
W//##//////##//#M
<- Photoresist
~#//####///#/##//M
W####////###///#/#
UV UGHT
1111111
~=:;:;::;:;:::;:=;;;:::;:;:;;=;;;;;;;;;! <- Photo Mask
W/##///##//#///////M
UV Exposure through
Photo Mask (Positive)
containing the Circuit
Pattern W#//###//////####n
Develop Photoresist
Pattern
and Post Bake
W////#///////#/#////#n:
Etching of the
Metallization
to delineate the
~//////##//////#//////#
Circuit Pattern
~////////#//////#/////h
Soft substrates are typically glass fibre reinforced and/or ceramic filled
(loaded) teflon based materials. The fillers or reinforcement materials control
the dielectric constant which ranges from 2.2 to 10. The teflon base provides
low dielectric loss. Mechanical working with these substrates is relatively easy
and lends itself for sizing and for making holes (Taconic Tech Topic). However,
when the thickness is small because of their flexible nature these substrates
need mechanical support which is normally provided by the aluminium base
(in some cases top as well) plate of the package. To provide perfect ground it
is necessary to hold the substrate to the base plate with screws at several
locations avoiding, of course, the circuit lines.
6 MICROWAVE MATERIALS
Table 2. Typical properties of hard substrates used for microwave Integrated circuits
Copper (ElectroplatedlRolled
1/8 to 2 oz)
Fig. 3. Commercial soft substrate (PTFE based dielectric) with integral
ground plane (MIs Rogers Corporation. USA).
Cr/250 Au/3-8
Cr/250 Cu/3-7 Au/0.5-1
Cr/250 Cu/3-7 Ni!250 Au/0.5-1
NiCr/1500 Au/3-8
TiW/250 Au/3-8
TaN/3000 TiW/250 Au/3-8
VACUUM ICHAMBER
TO HIGH
<-- - ..
VACUUM L..=:==~;:::====== <-- GASES IN
ARGON
NEEDL£ VALVE NllROGEN
lHROTTlE VALVE OXYGEN
discharge set up between the two electrodes bombard the source material placed
on the cathode and dislodge (sputter) the material which in tum gets deposited
on the substrate placed on the anode which is closely placed. There are several
variants to this simple arrangement and systems. The discharge can be produced
by DC or AC (RF). The discharge can be enhanced by placing the plasma in
a magnetic field. In this case, it is referred to as magnetron sputtering. This
helps in improving rate of deposition for a given power. Gases other than
argon such as nitrogen, oxygen can be employed for reactive sputtering wherein
the gaseous ions react with the source (target) material to form a compound!
composite film. For example, tantalum target with oxygen results in tantalum
oxide film and the desired stoichemetry is achieved by adjusting the oxygen
partial pressure and the power.
Extremely well adhering films can be produced by sputtering due to the
simple fact that the energy of the sputtered atom is orders of magnitude more
than the evaporated ion. In either case, it is essential that the substrates are
heated to a temperature anywhere between 150°C and 300°C for improved
adhesion and to achieve films with good crystallinity and grain structure.
Throughput of the evaporation process is much higher than that in a sputtering
process. But this is not a real drawback with the advent of automatic cassette
to cassette loading through vacuum load locks. Another specific advantage of
sputtering is to be able to deposit composite, compound or alloy films true to
the composition existing in the source material, with the added ability to
manipulate the composition with reactive sputtering where possible.
Normally the sputtering or vacuum deposition is used to deposit the conductor
layer to a thickness of about 1 micron. Build up of this to 5-8 micron is done
by electroplating.
Electroless deposition followed by electroplating provide a cheaper alternative
for the metallization of the hard substrates. However, the quality of the film is
not as good as those prepared by sputtering or vacuum deposition. Good adhesion
is one of the main problems which in turn reflects on the difficulty in realising
fine line structures in the photolithographic fabrication~ Normally thin layer of
metallization is deposited by electroless process and the thickness is build up
by electroplating. Special formulations of electro less baths are available which
obviate the need for electroplating. Most of the commonly used metallization
structures can be deposited by the electroless technique. The surface of the subs-
trate is to be suitably prepared to initiate the electroless deposition. Typical process
steps for electroless deposition of copper on teflon substrate is given in
Table S (Prasad and Vijayaraghavan 1987). One of the main drawbacks of this
process is the difficulty in controlling the thickness of the film and its texture.
formulations the thickness of the film obtained with organo metallic formulations
is of the order of 1 micron or less. Building up of the thickness can be achieved
by electroplating. As of now organo metallic formulations are available for
gold metallization (Haskard 1988).
In either case best results are obtained by screen printing the conductor over
the full substrate and realising the circuit pattern photolithographically.
Historically NiCr (nichrome) is,the material used for the resistive layer though
to some extent chromium layer itself served the purpose. Tantalum nitride is
the newer material offering greater flexibility in controlling the sheet resistance
and better stability due to self passivation by the formation of thin oxide layer.
Tantalum oxinitride has been experimented with to arrive at low TCR values.
Added advantage being that these films as well as the dielectric layer tantalum
pentoxide (Ta20s) can be deposited by reactive sputtering with nitrogen and
oxygen using a single tantalum target. Table 6 summarises the characteristics
of different resistive films used in realising MICs.
Nichrome 10-500 < ±20 to ±150 Most popular and stable resis-
(Ni:Cr/80:20) tance material. But susceptible to
contamination
Tantalum upto 100 ±SO to ±150 Resistor trimming can be done
by partial anodising
Tantalum 30-200 - 60 to -200 Resistivity and TCR can be
nitride manipulated by incorporating
oxygen. Very stable resistors
Cr/SiO upto 600 < ±20 to ±200 Stable high resistivity cermets
4 ASSEMBLY
Having realised the circuit pattern on the substrate the next step involves
populating the printed circuit with discrete devices viz., the active components
like transistors, diodes and in some cases the passive components like capacitors,
resistors, inductors if these could not be conveniently integrated in the circuit.
Conventional leaded package types for these components that are used in the
14 MICROWAVE MATERIALS
fabrication of the normal Printed Circuit Boards (PCBs) are not suitable for the
hybrids to get the full benefits of miniaturization. This is particularly so for
MICs which are meant to operate at higher frequencies. All the add on components
are to be surface mountable and at the high end of microwaves it is preferable
to integrate the passive components in the circuit and to use the active components
in the chip form. All the passive components are now available in the surface
mountable package or 'chip' form. Typical outline of some of these passive
components are shown in Figs. 8 and 9. In addition to the bare chip or 'die',
the active components also come in a variety of package types or with leads
attached (beam lead type) for use in MICs. Some of these types are shown in
Fig. 10.
The process of assembly of these components in the circuit involves: (a)
attaching the components on the circuit board to provide mechanical suppOrt,
and (b) to establish electrical contact between the component terminals and the
circuit conductor pattern.
Except in the case where the active components are used in the bare chip
form or in some types of passive chip components, the attachment of the
component terminals to the conductor circuit pattern for providing electrical
contact gives the necessary mechanical support and no additional mechanical
fixing is necessary. The bare chip mounted on the metallization provides the
mechanical support as well as electrical 'ground' or earthing or in some cases
electrical connection to active terminals of the component for example to the
collector terminal of transistor. The electrical connection between the connector
pads (bonding pads) on the die and the conductor lines on the circuit is done
by "wire bonding" a process by which fine dia wires or ribbons are attached
to the 'bonding' pads on the die and the conductor lines. Different methods
employed for attaching the components to the circuit and for interconnections
are summarised in Table 8 (Edwards 1991).
4.1 Soldering
This is one of the oldest and most common methods used for attaching the
discrete components to the circuit boards and a large varieties of materials and
Materials and Processes in MICs Fabrication 15
GLASS
PASSIVATION
HIGH ADHESION
METALIZATION--+--
CERAMIC_---~-'C
SUBSTRATE
GLASS _ _ _ _ __ TION
PASSIVATION ~:::-:S-c:::::::~
CERA~.1IC-------')
SUBSTRATE
techniques have been evolved over the years to suit the specific needs. Soldering
is a process by which two metal parts are joined together by the use of a low
melting point alloy which when melted forms an intermetallic compound with
either of the metal surfaces and bonds the two surfaces when cooled. Tin-lead
alloy has been the most commonly used solder for joining copper terminals and
lead commonly used in the electronic circuits. Important characteristics of
solder materials are:
1. Its melting point should be compatible with the components to be soldered
and the environment in which the circuit is to function.
2. It should be able to wet the surfaces to be soldered to enable intermetallic
diffusion/bonding to take place to establish good adhesion.
3. It should not leach or scavenge the materials being soldered. In this
regard the conventional tin-lead solders are not suitable for use with
gold metallization. The problem of leaching is overcome to a great extent
with the addition of 2% silver in the solder. Better alternatives are the
indium orland gold based solders but at a higher cost.
16 MICRowAVE MATERIALS
A large variety of solder materials have been evolved to meet specific requi-
rements. The characteristics of some typical solders used for the MIC applications
are listed in Table 9.
Different techniques used for carrying out soldering in MIC are: (1) Manually,
using soldering iron and (2) Reflow with hot gas, hot plate, IR, Vapour Phase,
Laser. Such methods as wave soldering and dip soldering, more common in the
case of PCB assembly, are not generally used in the fabrication of MICs.
_1~
,------------- -------------I-~
k .100 ~
-T
.035
~~-~~~
W .030
INDUCTOR
(DIMENSIONS IN INCHES)·
TERMINATIONS
ELECTRODES
For good solder joints it is important that the surfaces to be soldered are
clean and free from oxide layers. To help the process of cleaning and to present
virgin surface to the solder material, flux materials are used along with the solder
material. Both resin based and water soluble (organic or inorganic) fluxes are
used. The latter are more active than the resin based fluxes but arc easily
removed by water cleaning which however is not always possible. Synthetic
W
---------7 \ ~
CI======~IL-~~~~========~r
0.05 3 - -t 0.Q15
0.12
r--' I
,I
l
..t'
(DIMENSIONS IN mm)'
GATE
SOURCE
A---...J
S
DRAIN
1.27,. [.51
f-6.35~ T
TYP
Fig. 10. Outline of surface mount active components (MIs California Eastern
Laboratories, USA and MIs Avantek Inc., USA).
18 MICROWAVE MATERIALS
activated fluxes combine the high activity level typical of water soluble organic
fluxes with the benefit of solvent cleanability. The solvent cleaners normally
comprise of a blend of polar and nonpolar solvents like propyl alcohol and
chlorinated/fluorinated hydrocarbons.
The form in which the solder materials are used depends on the technique
used for the soldering. Table 10 summarises the same. The solder preform
mainly used for fixing the dies/chips to the substrate is nothing but a disc of
solder material with thickness in the range upto 500 microns and is either
circular or rectangular (square) in shape with sizes matching those of the dies.
It is essential that the die has metallization at the bottom.
Solder paste/cream is similar in characteristics to the thick film paste in the
sense that the solder material in the form of fine spherical particles is dispersed
in a thixotropic organic polymer along with a solvent to control the viscosity.
The paste of course does not contain any glass frit. The flux material is also
blended with the paste.
The solder paste can be applied by (1) sharp pin, (2) syringe and (3) screen
printing, to the circuit conductor terminations where the components have to
be attached.
Application using pin head is essentially a manual process and is only
acceptable for laboratory scale activity. There is: however absolutely no control
over the quantity of solder paste that is being applied and precise control of the
location is entirely dependent on the skill of the operator. Application through
Materials and Processes in MICs Fabrication 19
syringe affords a better contrdl over the quantity of paste. Equipments are
available which precisely control the amount of the solder paste to be applied.
This can be predetermined by the choice of the nozzle and the other parameters
like the pressure in the cylinder. Simpler systems require the nozzle to be
moved to the desired location manually and the paste dispensed automatically.
More sophisticated systems are available where the nozzle is held on a movable
carriage of an X- Y table and its precise location over the substrate is computer
controlled. With such systems, the demand on the operator's skill is minimised.
Screen printing affords a precise control of both the quantity of the paste as
well as the location. This is a preferred method if a large number of identical
circuits are to be fabricated, but is essential if the circuit involves soldering
large number of compqnents or components with large number of pins with
narrow spacings/gaps. After application of solder cream/paste the components
to be soldered are placed in position and the paste is allowed to dry in air to
drive off the solvents. The adhesive nature of the paste helps in holding the
components in place before it goes for reflow.
Temperature of reflow, time and rate of heating are important in achieving
good solder joints. Rapid heating and/or cooling would result in the formation
of blisters and voids due to entrapment of volatile organic matter in the paste.
For large volume applications conveyerised reflow is convenient. IR reflow is
faster without heating too much the other circuit portions. But there is always
a danger of excessive heating of some components which have higher absorption
in the IR frequencies used for reflow. Vapour phase reflow enables uniform
heating of the whole circuit due to the intimate contact of the hot vapour of the
liquid. Flourinert fluorinated hydrocarbon with boiling point at 215°C is the
most common liquid used for vapour phase reflow. This has the added advantage
of cleaning the flux residues of the substrates.
Hot gas reflow involves directing hot gas (air) at the solder points through
a specially designed heated tool similar to soldering iron. Special tool tips are
provided so that all the leads of the component are heated simultaneously and
reflowed. Hot gas reflow has the advantage of heating only the solder points.
But basicallY,this is a slow process and useful for repair work wherein one
does not heat up the other solder joints in the circuits.
The advantage of laser reflow is also that the laser energy is directed only
to the solder joints. The energy and pulse width are so chosen that it is just
right for ensuring the reflow without causing the surrounding circuit/components
to heat up. Thus any heat sensitive components are protected. Different soldering
techniques are compared in Table 10.
this case the silicon die does not have any metallization on the bottom. The die
is brought into intimate contact with the metallization under gentle pressure
and rub to aid the eutectic bonding. Eutectic bonding provides very good
mechanical strength accompanied with good electrical and thermal conductivity.
Table 10. Comparision or dirrerent soldering techniques
Melt Soldering
Soldering Thin wire-plain Strictly manual Localised heat- Laboratory scale
iron or flux cored ing of the term- assembly and
Preform inals to be sold- rework
ered
Reflow Soldering
Hot gas Preform Semi-automatic Only localised Laboratory scale
Cream/Paste heating of the assembly or batch
terminals to be production. Mainly
soldered useful for rework
Hot plate Preform Manual to total Whole circuit is From batch produ-
Cream/Paste automation by raised to the ction to full scale
use of convey- reflow tempera- production by inte-
erised system ture grating with auto-
mated dispensing
system for appli-
cation of solder
paste and compo-
nent pick and place
equipment
Laser Cream/Paste Best utilised Only the solder Best suited for large
when automated terminals are production for the
with computer heated investment
control
Materials and Processes in MICs Fabrication 21
The disadvantages however are: (1) the need to use high temperature for bonding
and (2) the strain on the die due to differential thermal expansion between the
die material and the substrate-particularly severe for large size dies.
expansion between the component and the substrate during thermal cycling.
This is particularly severe if the difference is appreciable and if the component
to be mounted is relatively large in size. This material is also available in
solution form in consistencies suitable for use with standard dispensing
equipments.
When the adhesive has to replace a solder it has to be conductive. This is
achieved by loading the adhesive with metal powder, usually silver or gold.
Silver-palladium filled adhesives can be used where silver migration is a severe
problem at the cost of lower conductivity. The metallic fillers in excess of
70% are used. The adhesives, in particular epoxies can be of two component or
single component type; solvent based or solid formulation. Curing time is
dependent on temperature. Higher temperature promotes fast curing. Single
component adhesives are convenient to use but need special storage conditions
to increase the shelf life. Adhesives are available in paste form to enable easy
and controlled dispensing through syringe or for screen printing. Important
characteristics that decide the choice of a good adhesive apart from providing
good adhesion are: (1) minimum shrinkage during curing, (2) minimum out-
gassing, (3) high stability over wider operating temperature range and (4) low
chloride ion content.
Minimum shrinkage during curing is important otherwise the component
will be under great stress. For high reliability, circuits are invariably hermetically
sealed in a metal or ceramic package. It is therefore essential that there is
minimum out-gassing of harmful substances like water vapour or ionic impurities
such as chloride ions which will corrode the aluminium metallization and fine
bonding wires. New epoxy formulations which are referred to as 'moisture
lock' are being introduced which act as getters to moisture (Estes et al 1985).
The requirement of low chloride ion content in the adhesives, as required by
new US Military specifications, has been questioned by one of the established
epoxy adhesive supplier and is still open to discussion on the acceptable limit
(Estes 1986 and Estes and Pernice 1989). Entrapment of the solvents within the
adhesive films during curing is one of the greatest problems in attaching the
component to the substrate, particularly so when a large size die is to be
attached. This not only causes poor performance but also results in reliability
problems (Estes 1984). Special epoxy adhesives have been devised which can
withstand continuous operating temperature of more than 175°C and intermittent
operating temperature of 300-400°C (Estes and Pernice 1989). The main
advantage of these over the polyimide formulation is· that these epoxies have
dual glass transition temperature. The lower Tg value around 80 to 900C imparts
non-brittle or resilient character to the adhesive thereby allowing for thermal
cycling from -55 to +155°C without micro cracks developing in the bond line.
The higher Tg (160 to 180°C) imparts high temperature strength to the adhesive
to enable thermosonic/thermocompression wire bonding to be successfully
completed without die floating occurring.
Successful use of adhesives for the Microwave Integrated Circuits operating
upto millimeter wave bands has been demonstrated (Hernandez 1974). One
point to note is the precise control of the amount of the adhesive to be used
Materials and Processes in MICs Fabrication 23
and the curing schedule. It should be noted that longer curing schedule at
higher temperatures does not necessarily result in the best bond. One should
strictly follow the guidelines given by the manufacturers and supplement the
information with experimentation. To take care of large thermal expansion
mismatch one has to recourse to the elastomeric adhesives based on the silicones,
compromising on the tensile shear strength.
In addition to the electrically conductive adhesives, there are several occasions
to use electrically insulating and thermally conductive adhesive. In these cases
the adhesives are loaded with fine powders of alumina or boron nitride. The
latter provides- a higher conductivity by a factor of two. Another advantage of
the use of adhesives is that there are no flux residues to be cleaned which could
be detrimental to the reliability of the circuit.
Methods used for adhesive application are similar to those used for solder
paste or cream. Precise control in dispensing the adhesive is essential to avoid
bleedout of the excessive adhesive covering the bonding pads on and around
the chips. This hampers proper wire bonding. The curing is normally done at
elevated temperatures as prescribed by the suppliers in a thermostatically
controlled oven or on a hot plate. The latter may be preferable in preventing
crust formation on top of the epoxy while curing. This causes trapping of gases
from the uncured epoxy ultimately leading to splattering of the epoxy: Alternative
methods for curing are the use of IR and microwaves.
(c) SQUASHING OF
BOND PAD OF THE DIE THE BALL FOR
BOND
FORMATION
o c
~ CONDUCTOR TRACK
(a) FORMATION OF THE LOOP
(d) CAPILLARY RAISES
TO THE lOOP HEIGHT
Fig. II. Graphic illustration of the bonding cycle of the ball bonding
(Wire) (MIs Kulicke & SoCfa Ltd. Inc., USA).
Materials and Processes in MICs Fabrication 25
potential and the time. Optimum diameter of the ball is about 1.5 times the
wire diameter.
In thermocompression bonding both the bonding tool as well as the substrate
are kept at the desired elevated temperature. The bonding tool moves down and
the annular rim of the tool squashes the ball against the bonding pad for the
preset time leading to bond formation. As already mentioned, the temperature,
the bond force (pressure) and the duration of the bonding decide the quality of
bond. Excessive force squeezes the material of the wire from underneath the
tool leading to weakening of the wire itself. Optimum size of the squashed ball
is about 2 to 2.5 times the diameter of the wire. After the bond formation, the
tool is withdrawn to a preset height and the substrate is moved to bring the
second bond pad into position beneath the capillary tool. The tool is lowered
to make the second bond. It may be noted that the second bond cycle does not
involve the formation of ball. The wire is squashed by the rim of the capillary
to establish the bond. The process of tool lifting after the first bond, translation
of the substrate to the second bond position and lowering of the tool for the
second bond formation have to be precisely controlled to enable proper 'looping'
of the wire bond. This is essential not only to avoid shorting of the wire to the
sides of die or chip but also to maintain and control the impedance offered by
the bonding wire in the circuit which is impOrtant in the microwave integrated
circuits. Because of the circular symmetry of the first bond (ball bond) the tool
can be moved in any direction to carry out the second bond. The wire is held
by a clamp as the tool is moved upto a preset height after the second bond
thereby snapping the wire. The wire is cut at the place where it is squashed
most.
through the bonding tool. The high frequency scrubbing in addition to providing
localised heating causes plastic flow of the wire and the contact pad leading to
solid state interdiffusion. It also helps in breaking down the surface contaminants
if any, in particular the oxide layer on aluminium, helping in intimate contact
between the metal surfaces. This is a convenient method where the components
cannot be raised to the temperature needed for thermocompression bonding.
But it is not useful in bonding highly brittle dies such as GaAs chips.
been considered as alternatives but have not replaced gold and aluminium. The
dimensions of the wire and the ribbon commonly employed are indicated in
Table 11. One of the important properties of the wire/ribbon that is significant
for the wire bonding is ductility. Higher. the ductility more plastic flow will
occur for any given applied pressure resulting in more intimate interface contact.
Oxidation is less important in case of noble metals in determining the bond
stability. Normally successful bonding is achieved between metals of similar
crystalline structures perhaps due to better mutual solubility in compression
bonding. For better bondability therefore most of the metalli7.8tion structures
are given a final layer of gold plating. However, gold wire bonding on aluminium
alloy metallization on silicon chip is a common feature. But a potential failure
mechanism in such configuration is the formation of brittle intermetallic phases
at the interface normally known as the purple plague. This is controlled to
some extent though not completely eliminated by alloying small percent of
palladium in the gold wire.
Elongation of the wire (the amount the wire stretches before it breaks expressed
in %) is very important since it decides the formation of good and stable bond
wire loop. Too much elongation results in the sagging of the loop leading to
bond failures. Too little elongation would make the formation of loop altogether
difficult. Typical values are given in Table 11.
5 CONCLUSION
The area of the materials used in the fabrication of Microwave Integrated
Circuits is very wide involving materials ranging from polymers, ceramics to
special high purity metals and alloys. Each of these serves a specific purpose
and possesses special characteristics. In this chapter it was only possible to
give an overall picture of the various processes involved in the fabrication of
MICs and the materials used therein. No attempt has been made to go into the
details of the preparation and characterisation of materials themselves. For
more detailed account the reader should consult the books and articles cited
under references. Secondly, as regards the characteristics of various materials
listed in the tables it should be emphasised that these are meant to be only
indicative of their typical values and cannot be used for any design calculations.
By the very nature of these materials there is bound to be a variation in these
characteristics depending on the detailed composition and the method of
preparation. It is therefore advised to use the values specified by the manufacturers
of the materials and if necessary and possible carry out inhouse characterisation
to confirm the listed specifications.
Another area which needs special attention is the defence and space electronics
wherein microwave circuits and systems find wide ranging applications. These
applications demand high reliability under adverse environmental conditions.
This implies that the system should have the ability to perform over a wide
temperature range and under conditions of high humidity, large vibration, high
acceleration, great impact etc. Detailed specifications of these and test methods
are given in US Military standards 883B and recently introduced standards
1772 or other similar standards. The need for the final subsystem to meet
28 MICROWAVE MATERIALS
stringent military and space standards implies that the materials used therein
have to perform well and meet the stipulated standards. One therefore has to
ensure that the materials used for the fabrication of microwave systems for
defence or space applications meet the stipulated standards by thorough screening
and characterisation as per the methods specified therein.
~EFERENCES
1. Berry RW, Hall PM and Harris MT (1968) 'Thin Film Technology' (Princeton,
D. Van Nostrand Co. Inc.).
2. Bhat Band Koul SK (1989) 'Stripline-like Transmission Lines for Microwave
Integrated Circuits' (New Delhi: Wiley Eastern Ltd).
3. Blum JB and Anzai K (1989) 'Aluminium Nitride Substrates for Hybrid
Microelectronics Application' Hybrid Circuit Technology, 6 No.8, p. 7-14.
4. Chopra KL and Kaur I (1983) 'Thin Film Device Applications' (New York:
Plenum Press).
5. Corkhill JR (1976) 'Thick Films at High Frequencies' in 'Hand Book of Thick
Film Technology' Eds. Holmes PJ and Loasby RG (Ayr, Scotland:
Electrochemical Publications Ltd.).
6. Edwards PR (1991) 'Manufacturing Technology in the Electronics Industry-
An introduction' (London: Chapman & Hall).
7. Estes RH and Pernice RF (1989) "Die Attach Adhesives-Evaluation of VceSAT
and 9jc Performance in Power Devices" Proceedings of ISHM International
Symposium on Microelectronics, Verginia, USA, p. 664-669.
8. Estes RH (1986) 'Adhesives for Military Hybrids' Hybrid Circuit Technology,
3 No.7, p. 21-24.
9. Estes RH, Kulesza FW and Banfield CE (1985) 'Recent Advances made in
Die-Attach Adhesives for Microelectronic Applications' Proceedings of ISHM
International Symposium on Microelectronics, Anaheim, USA. p. 391-401.
10. Estes RH (1984) 'The Effect of Porosity on Mechanical, Electrical and Thermal
Characteristics of Conductive Die-Attach Adhesives' Solid State Technology,
August p. 191-197.
11. Grovenor CRM (1989) 'Microelectronic Materials' (Bristol: Adam Hilger).
12. Haskard MR (1988) 'Thick Film Hybrids-Manufacture and Design' (Sydney:
Prentice-Hall of Australia Pty Ltd.).
13. Hernandez L (1974) 'Epoxy Techniques for Hybrid Microwave Integrated Circuits'
Proceedings of ISHM International Microelectronics Symposium, Boston, USA.
p.272-5.
14. Holland L (1965) 'Thin Film Microelectronics-The Preparation and Properties
of Components and Circuit Arrays' (London: Chapman and Hall Ltd.).
15. Holmes PJ and Loasl,>y RG (1976) 'Hand Book of Thick Film Technology'
(Ayr. Scotland: Electrochemical Publications Ltd.).
16. Hughes JE (1987, 'A Review of Thin Film Resistors and their Assembly Problems'
Hybrid Circuits, May.
17. Jowett CE (1982) 'Materials and Processes in Electronics' (London: Hutchinson
& Co (Publishers) Ltd.).
18. Kugler TR and Culkin TJ (1989) 'Ceramic Processing with Lasers' Hybrid
Circuit Technology, 6 No.8. p. 45-48.
19. Licari 11 and Enlow LR (1988) 'Hybrid Microcircuit Technology Hand Book:
Materials and Processes in MICs Fabrication 29
Materials, Processes, Design, Testing and Production' (park Ridge, New Jersey:
Noyes Publications).
20. Maissel U and GIang R (1970) 'Hand Book of Thin Film Technology' (New
York: McGraw-Hill).
21. Pitt KEG (1981) 'An Introduction to Thick Film Component Technology' (Luton,
England: Mackintosh Publications Ltd.).
22. Prasad SD and Vijayaraghavan MS (1987) 'Fabricating Hybrid MICs on J71'FE
based Boards' Hybrid Circuit Technology 4 No.3, p. 19-21.
23. Reddy TRs (1988) 'MMICs in Hybrids' Proceedings of ISHM (India) '88 Third
Annual Conference of International Society for Hybrid Microelectronics (India
Chapter), Hyderabad, INDIA p. 31-45.
24. Siddall G (1965) 'The Properties of Passive Circuit Elements' in 'Thin Film
Microelectronics-The Preparation and Properties of Components and Circuit
Arrays' Ed. Holland L (London: Chapman and Hall Ltd.).
25. Soane DS and Martynenko Z (1989) 'Polymers in Microelectronics: F\Dldamentals
and Application' (Amsterdam: Elsevier Science Publishers B.V.).
26. Stuart RV (1983) 'Vacuum Technology, Thin Film and Sputtering: An
introduction' (Orlando, USA: Academic Press Inc.).
27. Sunahara K and Takabatake M (1990) 'Low-Temperature Fired Multilayer
Circuit Board for High Frequency Application' Hybrid Circuit Technology, 7
No.2, p. 35-41.
28. Taconic Tech Topic 'Processing of J71'FFJWoven Glass Laminates' ¥icrowave
Dielectrics Division (Petersberg, USA: MIs Taconic Plastics Ltd).
29. Van Nie AG, Goedbloed W and.Kersuzan G (1981) 'Relaibility and Degradation
of Microwave Integrated Circuits' in 'Reliability and Degradation' Eds. Howes
MJ & Morgan DV (New York: John Wiley & Sons Ltd) p. 363-439.
2
Materials and Technology for Microwave
Integrated Circuits
1. INTRODUCTION
Advances over the past two decades in the planar techniques and technology
and also in the miniature microwave solid state devices compatible with this
technology have led to the realization of compact microwave integrated circuits
(MICs). These circuits are built on planar transmission lines such as the stripline.
microstrip line. suspended stripline. suspended microstrip. inverted microstrip.
slot line. coplanar waveguide and coplanar strips. The basic geometries of
these lines are shown in Fig. 1. For MICs. these planar transmission lines are
formed on substrates made of low loss dielectrics. ferrimagnetics and
semiconductors. A typical MIC consistS of one or more of the following parts:
(a) distributed elements (b) lumped elements in planar/discrete form.
(c) semiconductor devices and (d) special elements such as dielectric resonators
and ferrite discs. Two different technologies; viz. hybrid and monolithic are well
accepted for the fabrication of MICs.
In the hybrid technology. the passive circuit which consists of distributed
and/or planar lumped elements is realized as a conductor pattern on the substrate.
This is a single level process and involves metallization of the substrate through
vacuum evaporation/RF sputtering and defining the desired pattern through
acc~te photolithographic techniques. Resistors. if required. can be incorporated
by depositing resistive films at appropriate places. Semiconductor devices and
other disc:rete passive chip devices (capacitors and resistors) if any, are bonded
or soldered to the circuit pattern. Typical operating range of hybrid MICs is 1
to 30 GHz and with the adoption of more sophisticated photolithographic
techniques. their operation can be extended into the millimetre wave range up
to about 120 GHz. Nearly all coaxial and waveguide components. particularly
for operation at low power levels can now be realized in hybrid MIC form. The
advent of this t.echnology has resulted in considerable reduction in size and
weight. ease of mass production with improved reproducibility and potential
low cost of functional circuits. The technology offers the advantage of combining
Materials and Technology for Microwave Integrated Circuits 31
.. Ground
planes
Ground
plane
J
dL (.,. . -. .---~..:.,..-~ ---:f- ·-;5\··.· :.... .,
10·. ·.·0:·;
f~~t-::~
~ -IWI- ' -
Air gap
~~~.,.......~.
.,.-
,. . . . ,. . .r./
.....,........,.....:....:...,.:..:.......:..~...:..:.....:..JI
~~----______J
Ground
plane
Ground
plane
(eJInverted microstrip (quasi-TEM model
Fig. 1 (Contd.)
32 MICROWAVE MATERIALS
Conductors
(non-TEM mode)
Conductors
*~
T~
(g)Coplanar waveguide (quasi - TEM mode)
Fig. 1. Planar transmission lines for MICs and typical fields in their
cross-sectional planes, E field lines.- - - -H field lines.
Z= za/..[i; (1)
(2)
34 MICROWAVE MATERIALS
where Er is the relative dielectric constant of the dielectric filling. The following
closed from expressions reported in the literature [8] are known to yield virtually
exact results for the characteristic impedance:
For w/b ~ O.S
.r;;-
ZvEr =29.979 In[ 2 (1(1 +_ f]
k) (3)
(7)
\. C- - -----I
(a) Stripline
Metallic
Air ~shie ld
Gasket
Metall ic
Air ' sh ield
f---- c - -----lld--
(e) Suspended stripline
Fig. 2. Examples of shielded planar transmission lines.
above. Larger the value of Er of the substrate. the greater is the relative concen-
tration of energy inside the substrate and lesser is the radiation. The characteristic
impedance and guide wavelength of a microstrip can be related to Z· and AO
in the form [11]
Z = Z'f..JEerr (8)
A = Aof..JEerr (9)
where Eeff is the effective dielectric constant (relative) of the microstrip medium.
It is defined as the relative dielectric constant of an equivalent homogeneous
microstrip which has the same phase velocity as the original (inhomogeneous)
microstrip. The value of Eeff lies in the range
36 MICROWAVE MATERIALS
(10)
depending on the value of w/h. For small strip widths (w/h « I), the fields are
distributed nearly equally in the substrate and air regions and hence Ecff approaches
the lower limit (1 + Er )/2. For large strip widths (w/h » I), the electric field
is confined mostly between the strip conductor and the ground plane. The
microstrip then resembles a parallel-plate capacitor with Ecrr approaching Er•
(13)
where h is in cm and fd is in GHz. From (13), it can be seen that the upper
frequency limit for quasi-static operation can be extended by choosing substrates
of lower thickness and lower dielectric constant.
Effect of Dispersion
At higher frequencies, the fields tend to concentrate more within the dielectric
substrate. Consequently, Eerr increases with an increase in frequency, with the
value approaching the substrate permittivity Er asymptotically in the limit
frequency tends to infinity [16]. The following closed form dispersion formula
Materials and Technology for Microwave Integrated Circuits 37
can be used to compute the frequency dependent £CIT (denoted as £CIT (j) in the
range 2 ~ Er ~ 16, 0.06 ~ w/h ~ 16 andf~ 100• GHz [17]:
E
efT
(f) = [Fr -..re;; re-]
1 + 4F-LS
+ "Ie-efT
2
(14a)
where
and EefTis the quasi-static value given by (12). Similarly, the effect of dispersion
on Z can be obtained from the closed form expression given by [14]:
Losses
The propagation loss (neglecting radiation) in a practical microstrip is primarily
due to two types of dissipative losses; conductor loss due to the finite resistivity
of the conductor and dielectric loss due to the fmite loss tangent of the dielectric
substrate. Microstrip losses have been studied by several investigators [18-20].
If we denote ae as the attenuation constant due to the conductor loss and ad
as the attenuation constant due to the dielectric loss, both expressed in dB/unit
length, then the total attenuation constant a is given by
The following closed form expressions due to Pucel et al [18] can be used to
compute ae in dB/unit length:
{ R; [32 -
(W'/h)']
a _ 1.38 hZ 32 + (w'/h}2 A w/h ~ 1
(17a)
c - 61 x 10-5 Z E~ [w' +R: 0ft67w'/h JA w/h ~ 1
f
. h h (w'/h) + l444
Rs = ..j(CtJJl.o/2u) (18d)
6 =(1/Rs(1) (18e)
In these formulas, R. is the surface resistivity of the conductor, 6 is the skin
depth, (1 is the conductivity of the metal, Li is the rms surface roughness and
t is the thickness of the strip conductor.
The expression for l1ct in dB/unit length is given by [20]
Q-factor
The Q-factor of a microstrip corresponding to the conductor and dielectric
losses can be obtained from [15]
Q _ 11:..g;iiU} (20)
- ).,0 a
(21)
an inhomogeneous strip line in which the substrate carrying the strip conductor
is placed symmetrically between the two ground planes thereby creating an air
gap on either side of the substrate. The dominant mode of propagation is quasi-
TEM. The introduction of air gap results in the reduction of the effective
dielectric constant of the propagating medium. This configuration, therefore,
permits larger circuit dimensions leading to relaxed dimensional tolerances and
increased accuracy of circuit fabrication as compared with the microstrip. The
presence of the air gap also reduces the conductor loss in the ground plane,
because most of the electromagnetic energy gets concentrated in the dielectric
substrate. By choosing the substrate sufficiently thin, the effective dielectric
constant can be made close to that of air, thereby extending the frequency
range of operation in the dominant mode, which reduces to nearly TEM [22].
Because of the above advantages, the suspended stripline is ideally suited for
operation in the millimetre wave range. Practical suspended striplines require
some provision for supporting the dielectric substrate and also for electromagnetic
shielding. Fig. 2c shows the cross-section of a shielded structure with grooves
on the side walls to suspend the substrate.
where
E =0.2077 + 1.2177 (d/b) - 0.08364(c/b)
F = 0.03451 - ();1031 (d/b) + 0.01742(c/b)
v = - 1.7866 - 0.2035 (d/b) + 0,4750(c/b)
R = 1.0835 + 0.1007 (d/b) - 0.09457(c/b) (22d)
For c/2 < w < c
(23a)
where
..Jeerr = [1 + (E - Fin (w/b)) In (1I..je;)]-1 (23b)
and
Z = 1207t[V + R(w/b) + 1.393 + 0.667 In «w/b) + 1.444))-1] (23c)
40 MICROWAVE MATERIALS
where
E = 0.464 + 0.9467 (d/b) - 0.2063 (c/b)
F = 0.1424 + 0.3017 (d/b) - 0.02411 (e/b)
V =- 0.6301 - 0.07082 (d/b) + 0.247 (c/b)
R = 1.9492 + 0.1553 (d/b) - 0.5123 (e/b) (23d)
These expressions are valid for 1 S e/b S 2.5, I < Er < 4,0.1 < d/b < 0.5.
The accuracy of these expressions is within ± 2% for 0 < w < e/2 and ± 3%
for e/2 < w < e compared to rigorous methods.
In practice, the dimensions of the housing and grooves must be carefully
chosen so as to avoid propagation of undesired waveguide modes. The first
waveguide mode to appear can be either the TEIO-type or the distorted TEoI
mode depending on the dielectric constant and the dimensions of the enclosure.
For the TE IO type of mode, the cut-off frequency can be obtained from the
following relation [23] (refer Fig. 2c):
(25)
where COe is the cut-off angular frequency and Vo is the free space velocity.
(33)
The slotline is a convenient medium for shunt mounting of discrete devices.
It is particularly suitable for ferrite components that require regions of circularly
polarized magnetic field. One major disadvantage of the slotline is that its Q-
factor is low (=100) as compared with other transmission lines.
2.6 Coplanar Waveguide and Coplanar Strips (Fig. Ig and Ih) [3, 32-34]
The coplanar waveguide is basically a coupled slotline (Fig. Ig) in which the
signal is applied to the centre conductor with respect to the two ground conductors
on the two sides. The configuration of coplanar strips (Fig. Ih) is complementary
to the coplanar waveguide. Unlike the slotline, which is non-TEM in nature,
both the coplanar waveguide and coplanar strips propagate quasi-TEM mode.
At higher microwave frequencies, however, the contribution due to the longitudinal
magnetic field is sufficiently large resulting in non-TEM mode of propagation.
Both coplanar waveguide and coplanar strips have been analytically studied
by several authors [3,32-34]. The expressions for the characteristic impedance
Z and effective dielectric constant £elY of both these structures are given below
[34]:
Materials and Technology for Microwave Integrated Circuits 43
z = 30 te K(k')
(34)
..Jed K(k)
where
Ie::; (sl(s + 2w») (36a)
kl = ({sinh (m-/4h»/(sinh (te (s + 2w)/4h»)) (36b)
In (35), K(k) represents a complete elliptic function of the first kind and K(k')
=
with k' ...J(1 - k 2 ) is its complementary function. An approximate expression
for K(k)/K(It) which is accurate to 8 ppm is given by
General Requirements
The dielectric substrate for hybrid MICs must have the following general properties:
1. Low dielectric loss: The dielectric loss in a cirqJit is directly proportional
to the loss tangent (tan 6) of the substrate material at the operating frequency.
Typically values of the order of 5 x 10-4 or less would be desirable.
2. Fine surface finish: The conductor loss due to the metal mm at microwave
frequencies depends on the degree of surface finish of the substrate (in addition
to the resistivity of the metal), with the requirement on fineness of polish
becoming increasingly stringent with increasing frequency. Smooth surface is
also important for achieving fine line definition of the conducting pattern on
the substrate. The surface finish must be at least of the order of one skin depth
(typically 1 JIID or better at X-band).
Ceramic Substrates
Ceramic substrates, in general, are hard and can be produced with good surface
polish. These substrates, however, cannot be easily cut or drilled.
Material £, tan & x 10" Surface Thermal Thermal Dieleclric Special features
(approx.) at 10 GHz roughness conductivity expansion strength
ijun). (W/cm. K) (ppm/K) (KV/cm.)
and thennal properties. It has very low loss, negligible dispersion between
batches but is slightly anisotropic. Alumina substrates for MIC applications are
available in standard thicknesses 0.1, 0.254, 0.635, 1.27 and 2.54 mm with
dimensions in multiples of one inch (1" x 1" to 4" X 4"'). Because of its high
dielectric constant, alumina substrates are used extensively at lower microwave
frequencies.
Fused quartz has a lower dielectric constant than alumina and is available in
substrates with thickness as low as 0.05 mm and with a high degree of surface
finish (=0.006 J.llI1). With these features and its low loss property, fused quartz
offers an excellent medium for use at millimetre wave frequencies. The undesirable
features of fused quartz are, its high cost and highly brittle nature leading to
easy breakage during machining.
Plastic Substrates
Unlike the ceramic substrates, plastic substrates can be easily machined and
drilled. The most commonly used plastic substrate is the glass-fibre reinforced
polytetrafluoroethylene (PTFE) trade named as RT-Duroid 5880. It has a lower
=
dielectric constant (Er 2.2-2.3) than fused quartz and hence can be used at
millimetre wave frequencies. The loss tangent of this material is three to four
times higher than that of fused quartz, but this would have negligible effect on
circuit perfonnance since the overall loss is governed primarily by the conductor
loss (which is nearly ten times more than the dielectric loss). The thennal
expansion coefficient (: 10 ppmf'C) ofRT-duroid is compatible with the metal
compounds which are used for conductor patterns (: 10-30 ppmf'C for Cu,
Au) whereas that of fused quartz is much smaller (:0.5 ppmf'C). Duroid is
also mechanically stable up to temperatures as high as 350°C. It is a low cost
Materials and Technology for Microwave Integrated Circuits 47
Ferrimagnetic Substrates
Ferrites and garnets have relative dielectric constants in the range 9 to 16 and
dielectric loss tangent of the order of 10-3 at 10 GHz. These materials are hard
and brittle. Substrates are normally cut from a bar and ground to the required
thickness and surface finish depending on the device application. In the presence
of a d.c biasing magnetic field, they exhibit gyromagnetic anisotropy thereby
permitting the realization of non-reciprocal microstrip devices.
~
~
~
Material t;.
(approx.)
tan I) x 104
at 10 GHz
Surface
roughness
Thennal
conductivity K
Resistivity
(a-em)
Electron
mobility
Thennal
expansion
Dielectric
strength
i
(,urn) (W/cmf'C) (em2/V-sec) (ppm/K) (KV/em)
a given application. one must choose a substrate which offers the best compromise
between the desirable properties.
For hybrid MICs at microwave frequencies. microstrip on alumina substrate
is the most extensively used planar transmission line. Alumina. with its high
dielectric constant keeps the circuit size small and its low loss tangent keeps
the losses low. The choice of substrate thickness depends on the desired impedance
level and the operating frequency. For operation up to about 20 GHz. substrates
of standard thickness 0.635 mm are employed. Typical characteristics of a
microstrip on alumina substrate are discussed in Sec. 3.4. It may be noted from
(21) that as the frequency of operation increases. microstrip circuits must adopt
progressively thinner substrates preferably with a lower dielectric constant.
Another factor which assumes importance as the frequency increases. is the
surface roughness of the substrate. As can be seen from (17) the conductor loss
increases considerably as the skin depth in the metal reduces to the order of
rms surface roughness and lower. Using alumina substrates of smaller thicknesses
0.2 to 0.3 mm a variety of integrated circuit components and subsystems upto
about 50 GHz have been reported [35-36].
=
Fused quartz. with its lower dielectric constant (t;. 3.8) and extremely smooth
surface finish (~0.006 mm which is nearly 50 times smoother than alumina).
and availability in sufficiently small thicknesses offers a superior alternative to
alumina at frequencies above 20 GHz. By using 0.12 mm thick Z-cut quartz
substrates. several microstrip components such as the up-converter and balanced
mixer. have been fabricated and integrated into hermetically sealed receivers
for operation in the W-band (75-100 GHz) [37]. Fused quartz also has the
advantage that it is compatible with most ferrite materials. This property allows
insertion of ferrite discs into a quartz substrate thereby enabling complete
integration of circulators with other components on a single substrate. Fused
quartz substrates. however are very expensive. They are difficult to machine
and drill.
An inexpensive alternative to fused quartz at millimetre wave frequencies is
= =
the copperclad RT-duroid 5880 (Er 2.22) or Cu-flon (t;. 2.1). Unlike fused
quartz. these substrates are flexible. and easy to machine and drill. Using these
substrates in shielded microstrip configuration. compact receivers have been
reported for operation in the V-band (50-75 GHz) [38. 39]. By using 0.127 mm
thick RT-duroid substrate in suspended stripline configuration. integrated circuit
mixers have been realized at W-band (75-110 GHz) [40] and even at D-band
(110-170 GHz) [41].
Among the dielectrically anisotropic materials. sappbfre is the most useful
because of its well defined and repeatable electrical characteristics. availability
in small thickness and optical grade finish. The anisotropic property can be
advantageously utilized for equalizing the even-and odd-mode phase velocities
in microstrip and suspended stripline coupled lines to achieve high directivity
in directional couplers [42]. Microstrip-like transmission lines and coplanar
lines with anisotropic substrates also find applications in electro-optic modulators
and surface-acoustic wave (SAW) applications [43].
Ferrites exhibit magnetic anisotropy under d.c magnetic bias. Planar
50 MICROWAVE MATERIALS
Stripline 20-120 high negligible high Substrates--RT duroid/for passive components, incon- ~
(- 500) venient for mounting discrete devices .,~
Microstrip line 20-120 medium small high Substrates-illurnina, fused quartz, RT-duroid for iS o
0:;--
(-:: 250) hybrid MICs; GaAs for MMICs, and ferrites for tl
non-reciprocal devices/most widely used transmission ::s
tl.
line at microwave frequencies
,..,~
Suspended stripline 40-150 high small high Substrates--fused quartz, RT-duroid/well suited for ;:so
millimetre wave components, inconvenient for shunt ::s
<:l
mounting of active devices C-
O<:>
Suspended microstrip 40-150 high small high Features similar to suspended stripline '<
Inverted micros trip high medium ~
.,
25-130 small Substrates--alumina, fused quartz, RT -duroid/suit-
able for higher microwave frequencies, inconvenient ~
rio
for mounting active devices
~
Slot line 50-200 low large low Normally used in conjunction with microstrip, suitable ~
tl
(- 100) for shunt mounting of chip deviceso Produces elliptically <:
~
polarized RF magnetic field, useful for non-reciprocal ;;-
devices on ferrite substrates ~
0<:>
Coplanar 40-150 low medium medium Easy connection of series and shunt elements, useful ~
waveguide for MMICs on GaAs and non-reciprocal components ~
tl.
on ferrite C)
~o
Coplanar Strips 40-250 low medium medium Easy connection of series and shunt elements, useful ....,
for MMICs on GaAs ;::
a"
VI
......
52 MICROWAVE MATERIALS
Er
L 0.8
2.22 - - _
---------
---- ---~ ---
~-----
-
3.18
6
9.6 -- ---... -. 0.6
-. --- -----
-----
IU 9·6
4
----- -- ..... -.-~ 0.4
3.78
2 0.2
212
-twl-
HiC..'.·.~ . ).:1
o 0.0
0.01 0.05 10
W/h
Fig. 3. Effective dielectric constant EeJf and nonnalized guide wavelength A. / Ao of micro-
strip versus w/h with t;. as parameter. t;. = 9.6 (alwnina), 3.78 (fused quartz),
2.22 (RT-duroid).
=
Er 9.6, the coupling of quasi-TEM mode to the spurious higher order mode
=
occurs at!c,TM 53.2 GHz, thereby ensuring operation only in the dominant
mode in the microwave band. The main factor which sets the limit on the
highest frequency of operation is the attenuation in the line which increases
rather rapidly with an increase in frequency.
From Fig. 5, which illustrates the attenuation versus the height of the substrate
in a 50 n microstrip, we note that the attenuation is much less with fused
quartz and RT-duroid substrates, than with alumina. However, even with these
substrates there is a limit on the frequency upto which microstrip geometry can
be used since the requirement on making the substrates thinner (for ensuring
operation only in the dominant mode) poses problems due to increased conductor
loss and critical dimensional tolerances.
The preblems of high conductor loss and critical dimensions encountered in
microstrips in the millimetre wave range are to some extent circumvented in the
suspended substrate configurations (Fig. 1(c)-(e». As discussed in Sec. 2.3,
introducing an air gap between the substrate and the ground plane reduces the
effective dielectric constant and consequently, the strip dimensions are nearly two
to three times larger than in a microstrip for the same characteristic impedance.
Fig. 6 which shows a typical comparison of the impedance characteristics of a
Materials and Technology for Microwave Integrated Circuits 53
250~----------~----------~----------~
Er = 2.22 -jWr- h
,······Ir:.:.:.;.·.;.; .j.1
200~----------~----------4-----------~
3.78
1~~--------~~~~----~----------~
.,.
e
.c
9.6
-
o
N 100~-----------+~~----~~~----------~
50~----------+---------~~--~~----~
O~ __________ ~ ____________ - L_ _ _ _ _ _ _ _ _ _~
0·01 0·1 1 10
W/h
Fig. 4. Characteristic impedance Z versus wlh for microstrip with Er as parameter.
, - - 10GHz
- -- -- 20GHz
1· 0
--=...,e
'0
a
0· 1
0·01 L..-.-,-L,------~------_f_---~
0·01 0·1 5
h{m m)
Fig. S. Theoretical attenuation constant a ( = ex..: + ad) for a 50 n micros trip line
as a function of substrate height h with £,. as parameter:
I-alumina: E., = 9.6, tan ~ = 10-4, .d = 0.05 J.l1I1
2-fused quartz: E., =3.78, tan ~ = 10-4, .d =O.ot5 Jlm
3--RT-duroid: E., =2.22, tan ~ =5 X 10-4, .d =0.09 J.l1I1
substrates. Both these structures permit mounting of devices in series as well
as shunt configurations. The loss in these structures, however, is higher than
that in a microstrip. The microstrip is therefore preferred over these trans-
mission lines for MMICs and hence is more frequently used than the coplanar
structures.
120
Suspended microstrip (a/d=1)
Inverted microstrip (a/d=1)
Microstrip (d =h)
VI 80
e
.c.
o
N
40
OL-______~--------~~-----LI----~--J--
0 6 8
W/d
Fig. 6. Comparison of impedance characteristics of microstrip (Fig. I b), suspended
microstrip (Fig. ld) and inverted micros trip (Fig. Ie), Er = 3.78.
4.1 Discontinuities
Discontinuities in MICs commonly involve a change in the strip conductor
width or slot width. Figure 8 shows some of the frequently encountered
discontinuities in circuits fabricated using the stripline, microstrip and their
variants and Fig. 9 shows the discontinuities encountered in slotlines. Two
types of effects may be identified in these discontinuities. One is the generation
of fringing electric fields at and in the vicinity of a discontinuity which can be
represented in terms of an equivalent capacitance. The second effect is the
change in the normal flow of current which can be represented in terms of an
equivalent inductance.
Open-end
Open-end and short circuit terminations are invariably required in any circuit.
In a microstrip an open circuit can be easily realized by abruptly terminating
a strip conductor whereas a short circuit requires drilling a hole through the
substrate and making a connection to the ground plane. Fig. lOa shows a open-
ended microstrip and the nature of fringing electric fields at the termination. At
lower microwave frequencies, these fringing fields and the resulting increase
in the electrostatic energy in the region of the open end may be modeled as a
capacitor C1 as shown in Fig. lOb. The capacitance, in tum, is equivalent to
extending the microstrip line by a length fll such that the input impedance of
this extended line section is equal to the capacitive reactance at the operating
frequency.
56 MICROWAve MATERIALS
0.25
0.20
Microstrip
-
- 0.15
eu
a:l
0·10
Inverted mlcrostrsp
0.05 -
'~ I aft! = 1) _---
---- .------.
----Z-.-
...
,,-' ~.---
....;:::... ___ . Suspended microstrip
......... la/d=1)
'-
10 20 30 40
Frl!q IGHz)
FIg. 7. Comparison of attenuation constant a (= ex" + ad) versus frequency of 50 n
line in microslrip (Fig. Ib), suspended microslrip (Fig. Id) and inverted microslrip
(Fig. Ie)
Series-gap
A narrow series gap in a microstrip acts as an open circuit for de but presents
a finite impedance at microwave frequencies. The gap can therefore be used as
a dc block in active device circuits and as a RF coupling element between two
strip conductors. As illustrated in Fig. 8b, the series gap may be represented
as a x-network of capacitors. The shunt capacitors account for the fringing
Materials and Technology for Microwave Integrated Circuits 57
"l
~~ z
~
TCl
~ 'p
la I Open end
(g
~III
~~ I
P P
I
z +Cp +Cp
I
,
z
P P
Ibl Series gap
Ls
111"'1-
~
z,
, T~s Z2
p:
Icl Step change in vidth P "
Lt
,
~
Z Z
I
I
p p
iP
Idl Transverse sUt
,
p
61 I I 61 I
~--P Z
,
I
I
I
'r
-reb
~.
I
: Z
I
~
t
I
P p'
leI Chamfered bend
If) T- junction :
"2
Fig. 8. Examples of discontinuities in the strip conductors of planar transmission
lines shown in Fig.l(a)-{e) and their equivalent circuits.
electric fields from the open end to the ground plane and the series capacitor
accounts for the fringing fields between the two open-ends (see Fig. 11). If the
line widths are different, then the two shunt capacitances would have different
values. For very large gaps, Cg tends to zero and Cp approaches the end-
capacitance of a open-circuited line.
58
a
MICROWAVE MATERIALS
p
=:JL. I
P
la I Shor ted slot
= ,
Zz
I
, 0 I
I
~ IPZ ~
Ibl Inductive strip
z~C: ! 1:n:
p p
P
lei StlP thang. in slot
width
~: :P2 CS
~~ II
,
•
Z Z Z Z
~ I
T I
r'mI
Ls
Z
C
p
I
o
,
r I
<
P2
Cp
z
P,
Ibllnduttive notch
It I Capacitive strip
~ MetaUization
Fig. 9. Examples of slotline discontinuities.
Materials and Technology for Microwave Integrated Circuits 59
Z,p Z,(1
I Ideal open
~circuit
I
i l
p
p p'
Ground plane
lb)
10)
Fig. 10. (a) Microstrip with an open end showing fringing electric field and
(b) Equivalent end capacitance C, and end correction <1/.
PI IP
I I
E-liIes
Ground plone
Grou nd pi ane
(oJ (bJ
Fig. 11. (a) Microstrip with a series gap and (b) Cross-section showing fringing
E-field lines.
Chamfered Bend
Bends in the strip conductor are generally required in order to accommodate
the circuit optimally in a given substrate area. A sharp bend in the strip gives
60 MICROWAWMATERIALS
Current flow
lines
Ground plane
Fig. 12. SymmetrlC:'microstrip step discontinuity showing current flow lines on the
strip (:Onductor and fringing E-field lines at the step.
rise to excess capacitance resulting in poor VSWR. In practice, the effect of the
discontinuity reactance is minimized by chamfering the bend as shown in
Fig. Se. The equivalent circuit for the bend section between the planes P and
P' can be modeled as a shunt capacitance with transmission line sections of
length .11 on both sides.
T-junction
T-junctions are required in most MICs, such as power dividers, filters, couplers
and amplifiers. At the T-junction, two different transmission lines meet at right
angles giving rise to fringing electric fields with respect to ground and also
distortion in current flow. The junction can therefore be modeled as a three-
port network with shunt capacitance and series inductances as shown in Fig. Sf.
Metalization
Current
flow lines
~lS
OR
'p
~ ,,
p p'
(a) (bl
Fig. 13. (a) Slotline with a shorted end showing current flow lines around the
short and (b) Equivalent end inductance L. and end correction til.
Planar Inductors
Figure 14 illustrates some typical layouts of planar inductors. The simple form
of planar inductor is a short section (I « 1../4) of very high impedance line
terminated in very low impedance lines as shown in Fig. 14a. A simple relationship
between the length I of the section and its inductance L can be obtained from
the expression for the input impedance of a section of short-circuited transmission
line. It is given by
PI = sin-1 (mLrz) (41)
~22222222~
t-t«~
(a) (b)
(c) (d)
L R
Oo---'lW ''/1lIII0----0
O~-----------O
A thin strip conductor on a dielectric substrate without the ground plane (or
with no influence of the ground plane) also acts as an inductor. Single turn
loop inductors of the form shown in Fig. 14b can be used for realizing lower
inductance values in the range 0.5 nH to about 3 nH. Spiral (Fig. 14c) and
meanderline (Fig. 14d) inductors depend on the mutual coupling between the
adjacent line segments to achieve higher inductance values upto about 50 nH
in a small area. Values higher than this are difficult to achieve in lumped form
because of the inter-element fringing capacitance. The Q-factor for a spiral is
typically 100 which is higher than that for a straight ribbon.
Planar Capacitors
A lumped capacitor can be realized as a smaUlength (I « i./4) oflow impedance
line (conductor patch) terminated in very high impedance lines as shown in
Fig. 15a. If Z and fJ denote the characteristic impedance and propagation constant,
Materials and Technology for Microwave Integrated Circuits 63
Ibl
lei Idl
Dielee trie
~tilm
lei
~, If I film
~ Metallization
Fig. 15. Configurations of planar capacitors: (a) Short length of low impedance line
in microstrip; (b) Small gap in a micros trip conductor; (c), (d) Interdigital
line and (e), (f) Dielectric film overlay.
respectively, of the line, the length I of the·line can be obtained from the expression
for the input impedance of a section of open-circuited transmission line. That
is,
PI = sin-1 (roCZ) (42)
Planar Resistors
Planar resistors are used in attenuators, as terminations in directional couplers,
power dividers/combiners and circulators and also as isolation resistors in power
dividers. Fig. 16 shows typical configurations of a series resistor in a microstrip,
terminating resistor for a microstrip and an implanted resistor in MMIC. These
resistors are made of high resistivity metal films or cermet films on a dielectric
R
-c::::::J---
Ground
Z Z
plane
la)
~Cr
Ib)
Hltal Hltal
RlSistor film
Ie)
Flg.I6. Configurations of planar resistors: (a) Series ~istor in amicrostrip;
(b) Microstrip tenninated in a resistor and (c) Implanted resistor
film for MMIC.
R =p.l/wd (43)
where Ps is the specific resistivity (O-cm) of the resistor film, and the dimensions
I, w, d, which denote the length, width, thickness, respectively of the film are
expressed in cm.
4.3 Resonators
Resonators for MICs can be classified into the following: lumped element
resonators, transmission line resonators and dielectric resonators.
Materials and Technology for Microwave Integrated Circuits 65
la) Ib)
Fig. 17. Examples of lumped resonant circuits: (a) Series resonant circuit and
(b) Parallel resonant circuiL
la) Ib)
Slat
Ie) Id)
Fig. 18. Examples of transmission line resonators: (a) Half-wavelength micros trip
resonator; (b) Microstrip ring resonator; (c) Half-wavelength slot resonator
and (d) Slot-ring resonator.
66 MICROWAVE MATERIALS
where I is the physical length of the resonator, AI is the end correction due to
the fringing fields at the termination and It is the guide wavelength in the
transmission line.
Unlike the rectangular resonators, the ring resonators do not need any end
correction. The resonance condition for the ring resonator is given by
n(2a + w) =nit (45)
where a is the radius of the inner ring, w is the width of the strip/slot and n
is an integer indicating the number of azimuthal full-wave variations of the
field. Ring resonators are useful in measurement techniques, particularly for
measuring the effective dielectric constant of planar transmission lines [53, 54].
Dielectric Resonators
Dielectric resonators for MIC application are made of low loss, high dielectric
constant (Er :-30-100) ceramic mixtures such as the titanates and zirconates
(e.g. Ba2Ti9020, (Zr-Sn) Ti04). Resonators made of these materials have two
important advantages over the lumped and transmission line resonators; viz-
very high Q-factors in the range 3000-10000 and excellent temperature stability.
They are widely used in low loss, narrow band filters and temperature stabilized
oscillators [55, 56].
For most applications, resonators are fabricated in the form of a cylinder,
although othor shapes such as the ring and rectangle are also used. Figure 19a
shows the geometry of an isolated cylindrical resonator. The commonly used
resonant mode is the lowest order circular symmetric mode and is denoted as
TEol6- The electric field lines form concentric circles around the z-axis and the
magnetic field lines lie in the meridian plane as shown in Fig. 19b. The resonant
frequency of a resonator is determined by its dimensions, relative dielectric
constant Er and the surrounding medium. For an isolated resonator, the resonant
frequency for the TEo16 mode is given approximately by [56]
where a and d are radius and height, respectively of the resonator. This relation
is reported to be accurate within about 2% in the range 0.5 < aid < 2; 30 < Er
< 50. As an example, typical dimensions of a cylindrical TEo16 mode resonator
having Er = 38 and resonating at 10 GHz are a = d = 2.45 mm.
Figure 19c shows the arrangement of a dielectric resonator coupled to a
microstrip. The TEo16 mode is easily excited because of the magnetic coupling
between the strip conductor and the dielectric resonator. The amount of coupling
can be adjusted by varying the lateral distance between the strip conductor and
the resonator. It may be noted that the presence of the microstrip alters the
resonant frequency of the resonator and also lowers its Q-factor [56].
~-linIS
"
,,-,~
',' "
... -,
\
: /~ 1 ,-\ \H-lines
f ttl Ert i 1 \!
\ \ •• I' ' \ _/ '
\ ....... ,'1 \
_; "'-- /'
I
lal Ibl
ii=-lines Stri
con~uctor
,..!~-,
, .... -', '. Dielectric
r-T.."........,.,="'~.!..!3;.~'1"'!.,.:,'.,t.,_'_~ substrate
Icl
typical examples. The low pass filter shown in Fig. 20a is made up of series
inductors and shunt capacitors cascaded in an alternate fashion. The series
inductor is realized as a short section of high impedance line (narrow strip
width) and the shunt capacitor is realized as a short section of low impedance
line (wide strip). Figure 20b shows a four-port circuit incorporating a ring
having a circumference of 3)"/2. This circuit is popularly known as the rat-race
hybrid. Ports 1 and 3 are mutually isolated and so are ports 2 and 4. For a
signal fed to port I, equal power division takes place between ports 2 and 4
with signals differing in phase by 180°. For a signal fed to port 3 also, equal
power division takes place between ports 2 and 4 but the two signals remain
in phase. When two different signals (VI and V3) are fed to ports 1 and 3, the
sum signal appears at port 2 and the difference signal appears at port 4. These
properties are used in the design of balanced mixers, p-i-n diode phase shifters,
and comparator networks.
Figure 20c shows a 3 dB-power division network illustrating the use of a thin
film resistor for achieving good isolation between the two output ports (marked
2 and 3). Figure 20d is an example of a directional coupler circuit employing
coupling between a microstrip and a slotline to achieve broadband coupling
performance. The solid lines indicate the micros trip conductor pattern and the
68 MICROWAVE MATERIALS
10 I
~
-jv/If
Ie I Idl
Fig. 20. Examples of MIC components: (a) Low-pass filter. (b) Rat-race hybrid.
(c) 3 dB power divider. (d) Microstrip-slot direction81 coupler.
dotted lines represent the slot pattern etched from the ground plane side of the
microstrip. The slot line is parallel to the micros trip with its two ends terminated
in open circuits (indicated by dotted circles). Power fed to port 1 is equally divided
between ports 2 and 4 but the two signals differ in phase by 900 • Port 3 forms an
isolated port.
Figure 21 shows a typical microstrip layout of a two-stage FET amplifier
which includes in it step junctions. parallel-coupled line (which also serves as
a d.c block) and bias lines. The circuit incorporates d.c. block chip capacitors
at the microstrip gaps marked CI. Figure 22 shows the photograph of the
assembled microstrip amplifier.
5. FABRICATION TECHNOLOGY
Two different technologies; hybrid and monolithic have proved important for
the fabrication of MICs. Hybrid MICs permit the use of a wide variety of
planar transmission lines described in Sec. 2, whereas for MMICs, the
configurations are rather restricted to the microstrip and coplanar structures by
virtue of the process technology. The substrate materials appropriate for use in
the two technologies are already covered in Sec. 3. In this section, we provide
a brief review of the choice of other materials and some key features of the two
fabrication technologies [57-59].
Materials and Technology for Microwave Integrated Circuits 69
Ground
Grou nd
5.1 Materials
Conductor materials
Conductor materials for the MICs must have the following desirable properties:
• high conductivity or low RF resistivity so that the ohmic loss is minimized.
70 MICROWAVE MATERIALS
Substrates for MICs are metallized in two-or three-layers. The metal systems
commonly employed are, Cr-Au, Cr-Cu-Au, Ta-Au or Pd-Au for hybrid MICs
on ceramic substrates and Cr-Au, Ti-Pt-Au and Ti-Pd-Au for MMICs. These
materials are commonly deposited using evaporation or RF sputtering. For
MMICs, materials such as Ta, Mo and Pt are also deposited using the electron
beam evaporation.
Materials and Technology for Microwave Integrated Circuits 71
Dielectric Films
Dielectric films are used in capacitors as overlays, in passive components such
as couplers and protective layers for active devices. The properties of commonly
used capacitances in the range 0.2 pF-lOO pF are required in MICs. Thin-film
dielectrics in MICs are listed in Table 5. The desirable properties for these
dielectrics are, reproducible dielectric constant, low loss tangent, sufficient break-
down voltage and low probability of developing pin holes. The quality factor
of silicon monoxide (SiO) is about 50 whereas values higher than 100 are
achievable in silicon-dioxide (SiOV, tantalum pentoxide (Ta20S) and silicon
nitride (Si3N4). These materials can be deposited using the techniques mentioned
in Table 5. For higher power MICs, breakdown voltages in excess of about
200 V are required and these are generally obtained with larger film thicknesses
in the range 0.5 to 1 J.LrD.
Table 5. Dielectric film materials for MICs [7]
Resistive films
Examples of planar resistors for hybrid MICs and MMICs are illustrated in
Fig. 16. The desirable properties for the resistive films are, good stability, low
temperature coefficient of resistance and good heat dissipation capability. The
layer thickness is generally less than one skin depth so that the resistance value
is independent of frequency. Table 6 lists the properties of important resistive
materials. Sheet resistivities in the range 5 to 1000 O/square are achievable with
these materials. Of the various materials listed, nickel-chrome (NiCr) and tantalum
(Ta) are preferred because of their high resilience against environment, heat
and aging.
Table 6. Resistor film materials for MICs [7, 58]
Metallization
The substrate is first chemically cleaned in acetone and sulphuric acid. The
metal combination commonly adopted for alumina is Cr-Cu-Au. In order to
achieve good adhesion a seed layer of Cr of about 150A is first deposited
followed by a thin conducting layer (0.1 JlI11) on the substrate using either simple
evaporation or RF sputtering. The high conductivity Cu-Iayer is built up to
about 10 JlI11 either in the same vacuum run or by electroplating. Finally a flash
A. Metallization
k, :, 1. Uncoated alumina substrate, Clean
2. RF sputter both sides
Cr (-= 150A)-Cu (-= 10Mm)-Au (.:- 150A)
OR
RF sputter Cr (-= 150A-Cu (-= 0.1Mm)
i
Electroplate Cu (.::: 10Mm)-Au (-= 150A)
Photoruist 8. Etching the pattern
. ss s." '."'''''' . l - Cr -(U- Au 3. Apply (-ve) photoresist, spin, dry cure at
~
_ .' ... .. ., ' :...:. high temperature
E == = = : : : J l - cr-Cu- Au
....----- Ph ot ortsist
[",E;,~
Apply protective lacquer on lower surface,
Etch Au, Cu, Cr from top in sequence
P t ' 6.
~ ro tchvt
:E[
lac quer
St,i P
I '. '
1 0 . ,_ _ _. . . . .
..
."~
_~;...
.;
..,'.;.,
'
_ .' . .
. .
conductor 7.
(C r -eu-AU) Remove photoresist and lacquer
Ground plant
(Cr- Cu-AU)
Fig. 23. Typical hybrid MIe process for realizing a micros trip.
Materials and Technology for Microwave Integrated Circuits 73
,------'----------;;..z;;f-,_
- layer
I,Attive
'-r-_--_-_-_se_-~_i~_i~_;U_-I~_t_i~9_--_G_~_S--------' 1. Active layer formation
s 0
(--- -----?::\ 3. Ohmic contacts: Source (S) and
drain (D)
Au-Ge/Ni evaporation or alloying
S G 0
(n~_
0""""
n-\L._ _ _ _ _--, 4. Schottky-gate (G) formation (Ti-Pt-
Au)
[------:::6,
""i'!eno~
rzzza
J I
== 6. Resistor (R) formation
~ 7. Dielectric film/passivation
Mesa Etch
Mesa etching is a process by which active device areas are isolated so that
current flow is restricted to the desired portions. This is achieved by etching
away the surface leaving mesas of active layer at the desired locations. The
thickness of the material removed is on the order of 0.8 p.m.
Ohmic Contact
Ohmic contacts are formed on the active n-Iayer by sequential evaporation of
Au, Ge and Ni followed by lift-off and alloying in H2 ambient at around 450°C.
The total layer thickness is approximately 20ooA.
Schottky-gate Formation
The gate material must possess properties of good adhesion to GaAs, good
electrical conductivity and thermal stability. The metal system that is commonly
used for gate formation in GaAs MMICs is Ti-Pt-Au. Gates are normally
defined by contact photolithography, and submicron gates by electron beam
lithography.
First-level Metallization
This is a overlay metallization which forms inductors, lower plates of MIM
(metal-insulator-metal) capacitors, transmission line sections and provides overlays
for ohmic contacts. The preferred metal systems are Ti-Pt-Au, Mo-Au, Cr-Pt-
Au. For example, sequential layers of Ti, Pt and Au are deposited and patterned
by lift-off. The pattern can also be formed by ion-milling through a photo-
resist mask to remove the unwanted metal. The thickness of this layer is typically
6OOOA.
Resistor Formation
Resistors are formed by using GaAs material or resistive films such as Ni, Cr,
Ti, NiCr and TaN. GaAs resistors are formed between two ohmic pads by
using the existing isolation and ohmic contact masks. Thin film resistors made
of materials such as Ni, Cr, TaN etc are realized by sputtering.
REFERENCES
using alumina substrates, Fujitsu Sci and Tech. I., Vol. 14, No.4, pp. 33-43,
Dec. 1978.
37. P.L. Lowbridge, C. Burnett and B. Prime, W-band high reliability hennetically
sealed microstrip receiver, Military Microwave Conf., London, Conf. Digest,
pp. 502-511, Oct. 1984.
38. M. Dydyk and B.D. Moore, Shielded microstrip aids V-band receiver designs,
Microwaves, Vol. 2, pp. 77-82, March 1982.
39. K. Chang et al, V-band low-noise integrated circuit receiver, IEEE Trans.
Microwave Theory Tech., Vol. MTT-31, pp. 146-154, Feb. 1983.
40. R.S. Tahim, G.M. Hayashibara and K. Chang, Design and performance of W-
band broadband integrated circuit mixers, IEEE Trans. Microwave Theory Tech.,
Vol. MIT-31, pp. 277-283, March 1983.
41. L.Q. Bui, N. Ton and D. Ball, A D-band millimetre-wave cross-bar mixer,
IEEE MIT-S Int. Microwave Symp.l>igest, pp. 55S-556, 1984.
42. N.G. Alexopoulos and S.A. Maas, Characteristics of microstrip directional couplers
in anisotropic substrates, IEEE Trans. Microwave Theory Tech., Vol. MIT-30,
pp. 1267-1270, Aug. 1982.
43. S.K. Koul and B. Bhat, Generalized analysis of microstrip-like transmission
lines and coplanar lines with anisotropic substrates for MIC, electro-optic
modulator and SAW applications, IEEE Trans. Microwave Theory Tech., Vol.
MIT-31 , p. 1051-1059, Dec. 1983.
44. S.K. Koul and B. Bhat, Microwave and Millimetre Wave Phase Shifters, Volume
I on D~lectric and Ferrite Phase Shifters, Artech House, MA, 1991.
. 45. A.I. Baden Fullce, Ferrites at Microwave FreqUD/C~s, lEE Electromagnetic Wave
Series 23, Peter Peregrinus Ltd, 1987.
46. R. Garg and I.I. BahI, Microstrip discontinuities, Int. 1. Electronics, Vol. 45,
pp. 81-87, 1978.
47. R.K. Hoffman, Handbook of Microwave Integrated Circuits, Artech House, MA,
1987.
48. M. Caulton, Lumped elements in microwave integrated circuits, in Advances in
Microwaves, Vol. 8, by L. Young and H. Sobol (Eds.), Academic Press, NY,
1974.
49. D.A. Daly et al, Lumped elements in microwave integrated circuits, IEEE Trans.
Microwave Theory Tech., Vol. MTT-15, pp. 713-721,1967.
SO. F.E. Terman, Radio Engineering Handbook, McGraw-Hill, NY, 1943.
51. E. Pettenpaul et al, CAD models of lumped elements on GaAs upto 18 GHz,
IEEE Trans. Microwave Theory Tech., Vol. MTT-36, pp. 294-304, 1988.
52. R.S. Pengelly and D. Richard, Design, measurement and application of lumped
elements up to I-band, Proc. 7th Eur. Microw. Conf., pp. 461-464, 1977.
53. I. Wolff and N. Knoppik, The micros trip ring resonator and dispersion
measurements on micros trip lines, Electron. Lett, Vol. 7, pp. 779-781, 1971.
54. K. Kawano and H. Tomimuro, Slot-ring resonator and dispersion measurement
on slot line, Electron Lett, Vol. 17, No. 24, pp. 916-917, 1981.
55. I.K. Plourde and C.L. Ren, Applications of dielectric resonators in microwave
components, IEEE Trans. Microwave Theory Tech., Vol. 29, No.8, pp. 754-
770,1981.
56. D. Kajfez and P. Guillon (Eds.), D~lectric Resonators, Artech House, MA, 1986.
57. H. Sobol, Application of integrated circuit technology to microwave frequencies,
Proc. IEEE, Vol. 59, pp. 1200-1211, 1971.
58. R.W.Bery,P.M.HallandM.T.H8rris,Thin-FiImTechnology,VanNostrand,1968.
59. R.A. PuccI (Ed.), MontJlithic Microwave Integrated Circuits, (A reprint volume),
IEEE Press, NI, 1985.
3
Metallization of Plastics by
Electroless Plating
B. Viswanathan
Department of Chemistry
Indian Institute of Technology, Madras, India
PI asticsl ceramics
moulded ,formed or
machined
Clean and
condition
the redox reaction taking place between Pd(ll) ions in the solution as well as
tin ions adsorbed on the substrate. This means one should achieve good adsorption
of sensitizers. Schlesinger and Kisel [70] have examined the adsorption properties
of acidified SnCl2 solution with additives like hydroquinene, triton x-loo, thiourea
and showed a non-linear relationship between the amount of sensitizer adsorbed
and the number of metal islands deposited from electroless nickel bath (citrate
bath) per unit area of the substrate. The effectiveness of commercially available
sensitizing solutions for electroless copper deposition on hydrophobic substrates
has been gauged by the measurement of the contact angles. Feldstein and
Weiner [71] have demonstrated that controlled additions of stannic ions with
or without sodium chloride especially with aging could yield superior wetting
and thus can yield uniform plating of hydrophobic substrates [72-74]. The
aging process in the stannic halide solutions probably favors the transformation
of an a-stannic acid to a p-stannic acid form. The colloidal nature of fj-stannic
acid is consistent with the view that the sensitizers together with the activators
form only colloids and not solution complexes [75]. Cohen and West [76-78]
postulate that a complex between Sn(II) and Pd(II) is first formed in which the
reduction of Pd(ll) to Pd(O) occurs subsequently forming a nucleus for the
growth of the colloid. The core of the colloid is a metallic alloy of Pd and
tin surrounded by stabilizing layers of SnCl2 and Sn (OHh. According to this
model, one should expect the deposition of metallic tin on Pd and the cyclic
voltammetric study [79] by Jean Horkans aimed at identifying the chemical
state of the catalyst on the activated surface showed that in addition to the
stabilizing stannous layer produced by the reduction of Sn(lV) metallic tin
also constitutes to the core of the active colloid. The catalytic activity of Pd(O)
that are formed seems to be prone to UV irradiation and irradiated Pd(O)
species appear to be incapable of becoming catalytically active in the metal
plating bath [80, 81].
The structural and composition of the colloidal catalyst particles have been
investigated by a variety of techniques like electron diffraction, Mossbauer
spectroscopy, Rutherford backscattering and photoelectron spectroscopy [82].
Though there is some convergence on the fcc structure of the active catalyst,
there still seems to be some uncertainty regarding the composition of
Pd-Sn alloy. It is certain that Pd/Sn ratio is greater than I, [83, 84]. The
various values of the ratio reported in literature could have arisen because the
analysis of the data have been performed in the different regions of the active
catalyst from the core to the outer layer depending upon the type of technique
employed.
In the sensitizing and activating step, certain accelerators like NaOH, EDTA
are added which are effective in removing the tin species from the surface and
increasing the initial rate of metal deposition. The uniform distribution of the
metal deposit is also dependent on the nature of the accelerator used, for example
NaOH and EDTA are favorable for uniform deposition of copper [85].
In the sensitization step as stated earlier, various types of tin compounds
including tin oxide (Sn02) and ~tannous and stannic chlorohydroxides,
oxyhydroxides and hydrated oxides have been identified. The formation of
Metallization ofPlastics by Electroless Plating 85
these compounds and hence the extent of sensitization are dependent on the pH
of the solution [86]. The process sequence involves a rinsing step after the
activation and sensitization. There seems to be some difference of opinion on
the rinse water pH for the activation of plastics, Cohen and Meek [87] propose
that acidic solution rinse provides a cleaner, more catalytic surface while Ghorashi
=
[86] claim that a rinse water with pH 9 provides optimum conditions for
obtaining a uniformly activated surface. It is to be remarked that the final rinse
with appropriate pH provides the necessary type of species, hydroxide or chloride
species on the outer layer of the activator-sensitizer combination which favors
the catalytic reduction and deposition of the metal from the solution.
A new concept of the activation can be introduced based on the anchoring
the functional groups or ions on the polymer surfaces. For example Pd2+ can
be exchanged with polymer substrates with functional groups especially caIboxylic
groups which will avoid the formation of tin chloride shell over the activator
and thus promote in a facile manner electroless deposition [87a].
--- --
(+)
'"'(l-ttt})
'l9'- ....... _ -
EMF'
Eeq
Ale
c-)
- ....... ~
.... ,~!!.f)J
I.Q.....
........ .......
+
log i log i dep
Fig. 2. Current-Potential curves for the system with two different simultaneous
electrochemical reactions, Kinetic scheme.
Wherein it is seen that the potential of the redox couple is raised from its
reversible value E~ and the potential of the metal electrode is depressed
cathodically from its reversible value EAlso as to reach the mixed potential
EMP value. With the overall reaction at the electrode is represented as
Mn+ + Red -+ M + Ox (8)
In essence, the mixed potential can be considered to be the intersection
points of iM and i R• This implieSt at the steady state mixed potential, the rate
of reduction of the metal is equal to the rate of oxidation of the reducing agent
or
+
(+)
Eeq
M
eq
ERed
(-)
+~--------------------~~~~~
logi 1dep logi2deplogi3dep
logi
Fig. 3. Variation of the rate of electroless deposition and the mixed
potential with the exchange current density.
as well as ideposilion. Another aspect that has been investigated is to account why
certain metals with negative free energy of adsorption of hydrogen can be
deposited using a specific reducing agent like formaldehyde [92, 93].
The solution chemistry of electroless copper bath has been probed by a
variety of electrochemical techniques. Using cyclic voltammetry technique below
the mixed potential value (- 0.7 V) Tam [94] has identified that methylene
glycolate (CH20 2H) and its copper (11) complex are the electroactive species.
in solution. The methleneglycolate anion is adsorbed on the copper sites with
the C-H bonds adjacent to the copper surface which then undergoes electro-
dehydrogenation to give rise to formate anion as well as molecular hydrogen
evolution [95]. As seen from the data in Table 1 only a limited variety of
reductants are used in electroless process namely hypophosphite, formaldehyde,
borohydride, dialkylamine borane and hydrazine. Normally electroless plating
is accompanied by hydrogen evolution though it is not directly related to metal
deposition. Van der Meeraker [96] proposed a universal mechanism for electroless
deposition which involves the dehydrogenation of the reductant as the first
step.
RH ~ R + H(10)
R + OW ~ ROH + e- (11)
H+H ~H2 (12)
H+OH ~ H20 + e- (13)
Mn+ + ne~ M (14)
88 MICROWAVE MATERIALS
where RH represents the reductant It is seen from this mechanism that hydrogen
atom combination step (12) indicates that metals with dehydrogenation-
hydrogenation catalytic activity can promote this reaction step favorably.
Extending this proposal Ohno et al [97] propose that the oxidation of the
reductants proceeds mainly along with hydrogen evolution step on copper,
silver and gold while hydrogen ionization mechanism predominates on Co, Ni,
Pd and Pt. The catalytic activity series of the metals for anodic oxidation of
reductants does not coincide with that for hydrogen electrode reaction.
Electroless copper obtained using hypophosphite as reductant is supposed to
proceed through the following steps
H 2 P02 ~ HP0 2 + H
Cu 2+ + 2H 2 P02 + 20H- catalyst surface ) CUO + 2H 2 PO :i + H2 (15)
when complexing agents like EDT A are used octahedral complexes are formed
while with ligands like oxalate, glycine square planar or square pyramidal type
complexes are proposed. Multinuclear (usually dimeric) complexes are reported
with citrate, tartrate, malate which did not show any ESR signal indicating
strong anti ferromagnetic coupling, and in the presence of these ligands significant
plating rates were observed [98, 99]. Eventhough complexation is one of the
essential steps in the electro less plating no definite relationship could be estab-
lished between the plating rate and the stability constant of the possible complexes
that are formed. However ligands which can form dimeric copper species exhibit
higher plating rates (Refer to the data assembled in Table 3 [100]).
The mixed potential theory proposed for electroless deposition does not
seem to predict correctly the experimentally obtained mixed potential and the
current potential (i IV) curve is not a simple sum of the half cell i IV responses
in the case of copper electroless deposition by formaldehyde in presence of
EDTA. When the two half cell reactions are
Cu (EDT A)2- + 2e- ~ Cu (metal) + EDTA4- (16)
Table 3. Plating rates and stability constants with copper (II) and nickel (ll) Ions
= =
for various complexlng agents (M metal Ion and L ligand; K value
will change with pH and Ionic strength of the medium)
of low solubility of cuprous oxide the following reactions may also take place
in the bath
CU20 + H20 -+ Cuo + Cu2+ + 20H- (21)
2Cu+ -+ Cu2+ + Cuo (22)
These reactions result in fine particles of copper dispersed randomly in the
solution. Since cuprous ions are not easily reduced by formaldehyde the bath
instability also occurs. There are various ways one can avoid the formation of
cuprous oxide. They are: (1) agitation or aeration of the bath, (2) use of low
concentration of the constituents, (3) employing polyelectrolytes like cellulose,
ether, polyvinyl pyrolidine, polyvinyl alcohol, gelatin peptone polyamides etc
to cover the cuprous oxide to prevent the catalytic effect, (4) Decreasing the
free concentration of cupric ions by using suitable complexing agents and
(5) removing the nucleating impurities in the materials used especially in the
Rochelle salt.
been found applicable when EDTA is used as complexing agent and HeHO as
the reducing agent [109]. Donahue et aI [110] have deduced the relationship
iELP =K/Rp
where K is a constant and Rp is the polarization resistance. The deposition
rate decreases with aging of the bath while the proportionality constant K
(= 27.3 mV) is independent of the substrate used as well as aging of the bath.
It is therefore obvious that the kinetics of electroless plating though amenable
to various kinds of measurements is complicated and only empirical kinetic
laws can be generated on them which depend on a number of process parameters
like substrate used, additives added, aging of the bath and the nature of reducing
agent used. There is possibly a correlation between the rate of dissociation
of the complex (when the ligands like tartrate, EDTA, Quadrol, 2-diamine
N, N, N', N'-tetraacetic acid, triethanolamine [113] are used) and deposition
rate [114] and the hydro~yl concentration depenndence on the deposition
rate depends on the nature of the ligand used [115]. But for these few
generalizations the kinetics of electroless deposition still appears to be grossly
empirical.
or the free fonnaldehyde concentration) with HeHO have nearly equal elongation
values and greater tensile strength than electrolytic copper from acid sulphate
solutions containing no additives. The mechanical properties have a direct
correlation with the deposition rate. The internal stress in ~e electroless copper
is attributed to (a) entrapped hydrogen resulting from the plating process and
(b) fine particles of copper obtained from bath decomposition occluded in the
deposit [119].
Plating temp. °C 38 49
Plating rate m/hr 1.9 ·2.82 3.43 3.45 4.32 5.69
mil/hr 0.073 0.111 0.135 0.14 0.170 0.224
strip lines have also been designed by electroless copper plating [124]. The
usefulness of this technique as compared to copper clad PTFE is demonstrated
by the data given in Tables 7 and 8.
The Ni-P or cobalt deposits should have a high polish and uniformity, otherwise
the pits and non-uniformity will lead to loss of information and make the disc
scratchy and noisy.
10. CONCLUSION
Electroless plating has thus been receiving considerable attention in recent
times with respect to new bath formulations with improved features like long
term stability, increased plating rate, and increased throwing power from which
purer deposits or deposits with consistent composition and quality can be obtained.
Non-conventional methods like electroless gold plating on superconducting
YDa2Cu3O,.x ceramic oxides from non-aqueous baths are also attempted for
specific applications [126]. Plastics with thin uniformly metallized coatings is
used for various electronic and machinery applications and the need in this
sector is increasing more than what is expected. Structural studies of the deposits
still seem to interest scientists [127]. On the whole as expected, electroless
deposition appears to have a challenging future.
REFERENCES
13. K.S. Rajam and S.R. Rajagopalan, Technical Memorandwn, MT-TM-8601 (1986);
MT-TM-8801 (1988) NAL, gangalore, India.
14. K.S. Rajam, S.R. Rajagopalan, M.S. Hegdc and B. Viswanathan, Materials
Chemistry and Physics, 27, 141 {1991).
15. M. Papini and F. Papini, Thin Solid Films, 115, 1 (1984).
16. M. Schlesinger and J. Kisel, 1. Electrochem. Soc., 136, 1658 (1989).
17. S.L. Chow, N.E. Hedgecock, M. Schlesinger and 1. Rezek, J. Electrochem.
Soc., 119, 1614 (1972).
18. DJ. Levy, Electrochem. Tech., 1, 38 (1963).
19. J.W. Dini and P.R. Coronado, Plating, 54, 385 (1967). Deutsches Aulegeschrift
(DAS) 1, 137,918 (1958).
20. M. Gulla, US Patent, 3764, 352 (1973); 3, 832, 168 (1974).
21. M. Matsuoka and T. Hayashi, Plating and Surace Finishing, 68, 66 (July 1981).
22. A. Sergienko, US Patent, 3,418, 143 (1968).
23. H. Narcus, Met. Finish., 45, 64 (sep 1947).
24. M. Paunovic and R. Zeblisky, Plating and.Metal Finishing, 72, 52 (Feb. 1982).
25. K.F. Blurton, Plat. Met. Finishing, 52 (Jan, 1986).
26. S. Mizumoto, H. Nawafune, M. Kawasaki, A. Kinoshita and K. Araki, ibid., 48
(Dec, 1986).
27. R. Junginger, J. Electrochem. Soc., 135,2299 (1988).
28. C.I. Courduvelis and G. Sutcliffe, plating 67, 71 (Sep, 1980).
29. Y. Okinaka and H.K. Straschil, J. Electrochem. Soc., 133,2608 (1986).
30. S. Nakahara, Y. Okinaka and H.K. Sttaschil, J. Electrochem. Soc., 136, 1120 (1989).
"31. C.E. Baumgartner, Plating and Surface Finishing, 53 (Dec, 1989).
32. K. Kondo, J. Ishikawa, O. Takenaka, T. Matsubara and M. Irie, 1. Electrochem.
Soc., 137, 1859 (1990).
33. F. Pearlstein and R.F. Weightman, Plating, 474 (1972).
34. Aina Hung, Plating and Surface. Finishing, 62, (Jan, 1988); 74 (April, 1988).
35. Aina Hung, Ken-Ming Chen, J. Electrochem. Soc., 136, 72 (1989).
36. Aina Hung, and Izumi Ohno, J. Electrochem Soc., 137,918 (1990); Plating and
Surface Finishing, 54 (March, 1990).
37. F. Pearlstein and R.F. Weightman, Plating, 56, 158 (1969).
38. R.N. Rhoda, 1. Electrochem. Soc., 108, 707 (1961).
39. W.V. Hough, 1.L. Little and K.E. Warheit, US Patent, 4, 255, 194 (1981).
40. Y. Okinaka, Plating, 57, 914 (1970).
41. J.F. McCormack, US Patent, 3, 589, 916 (1971).
42. M.F. EI-Shazly and K.D. Baker, US Patent, 4, 337, 091 (1982).
43. A. Molenaar, 1. Electrochem, Soc., 129, 1917 (1982).
44. F. Pearlstein and R.F. Weightmen, Plating, 61, 154 (1974).
45. M.E. Warwick and B.J. Shirley, Trans, Inst. Met. Finish., 58, 9 (1980).
46. G.O. Mallory, US Patent, 4, 019, 910 (1977). G.O. Mallory and T.R. Horhn,
Plal Slu'. Finis., 66, 40 (April 1979). G.O. Mallory, Plating and Surface Finishing,
63, 34 (June 1976).
47. F. Pearlstein and R.F. Weightman, Electrochem Technol., 6, 427 (1965).
48. K. Baker, Plating, 61, 834 (1970).
49. A.E. Cahill, AES Proc., 44, 130 (1957).
50. F. Pearlstein US Patent 3, 222, 195 (1965).
51. M. Saito, Prod. Finish., 31, 7, 57 (1967).
52. R.1. Zeblisky, J.F. McCormack, J.D. Williamson and F.W. Schneble, US Patent,
3,095,309 (1963).
53. F.W. Schneble, R.J. Zeblisky, J.F. McCormack and J.D. Williamson, US Patent,
3,361,580 (1968).
98 MICROWAVE MATERIALS
V.R.K. Murthy
Department of Physics
Indian Institute of Technology, Madras, India
In the recent years, there has been considerable interest in the microwave
properties of dielectric and magnetic materials usually termed as microwave
materials. Every cost effective microwave device is a success story in coping
with the limitations of the materials.
The measurements in microwave frequency region may be made purely for
scientific purposes for e.g., in connection with the investigation of relaxation
phenomena. However, due to the increasing importance of the microwave
materials in telecommunications, in the design of microwave circuit components
and quasi-optical components such as substrates, dielectric wave guides, radiation
absorbing materials (RAM), one needs high precision in measurements and in
some cases, the dielectric loss should be critically measured.
In this chapter, various methods are discussed to measure the dielectric
constant, loss, complex magnetic susceptibility, microwave conductivity on
powders and single crystals. These methods can also be used to study the
microwave characteristics of thin films. All these methods have been verified
on standard samples and found agreeable.
C _ (eoal)
y - b (1)
L _ JJ. oN 2 al (2)
xz - (a2 + 12)
Where 1= P A,J2 for TE lOp mode and N has usual meaning similar to the number
of turns in a solenoid. If N is replaced by l/rc, the above equations result to
10= 1 (3)
2tr.JLxz Cy
Where 10 is the frequency of the cavity.
en= ~[/~
4V. if at
(..!. __Qo1)] (5)
J.I.' =1 +.1 Yc
K V.
(/011-11) (6)
where
K = 2a 2 (8)
a 2 + 12
The details of the experimental arrangement used in this type of measurement
is given in [3].
where fo is the centre frequency of the cavity, .1 is the change in the half power
bandwidth of the cavity with sample and without, .1fis the change in the centre
frequency of the cavity with and without. For a cylindrical cavity operating in
=
TEall mode, die filling factor a 2.1 (volume of the sample/volume of the
cavity). The depolarization factor n is evaluated for (a) long cylindrical sample
(L » d) as
(11)
(13)
(14)
(15)
(16)
these Tcs obtained by direct current (dc) and microwave frequency (ac) and
also due to the effect of thermally excited quasi particles.
The method of microwave conductivity measurement is described [7] using
a rectangular cavity.
In this study, the change in Q (quality factor) values were measured using
a rectangular cavity in frequency modulation mode. The value of Q for empty
cavity is of the order of 103 at room temperature.
Figure 2 shows the flow chart of the microwave conductivity measuring
system employed. A rectangular cavity of TEJ()6 mode with resonant frequency
at 9 GHz (X-band) was used. The cavity was coupled to the system and evacuated
I FM
MODULATION
MW SOURCE UL TRA- FAST
HY BRIO INTERFACER
INTEL'S
ANALOG ~
ISOLATOR 8255
TO DIGITAL \r-V'
1 CONVERTER
I ~~
FR EQUE NC Y ATTENUATOR HAS 1002
COUNTER
J.
CIRCULATOR
T
ULTRA HIGH
I SPEED HYBRID MIC R 0-
TRACK & HOLD PRO C ESSOR
r - --
I
----,
I
CRY STAL
DETECTOR
1
1- AMPLIFI E R
HTS 0025
SYSTEM
INTEL'S
8085
I I
I
I CAVITY
I
OSCILLOSCOPE T
I LOW NOISE
rt
I CURRENT - ........, LOW ORIFT
I I PRECISION
VOLTAGE
L
I ______ .JI CONVERTER IE- FET 52 J
AMPLIFIER
TEMPERATURE
& VACUUM l INTERFACER
CONTROLER DIGITAL TO
x-v INTEL'S
~
ANA LOG
SVSTEM ""- CONVERTER
RECORDER 8255
DAC 0080
to about 0.13Pa. The sample is kept at the maximum magnetic field in the
cavity, so that maximum current density can be achieved in the sample. The
frequency modulated power is fed to the cavity and the response of the cavity
is plotted using XY recorder. The microwave conductivity is calculated from
change in Q values
where Ql and Q2 are the quality factors of the cavity with and without the
sample, Po is Joule loss due to sample, ~ = 2tclo, 10 being the resonance
frequency of the empty cavity and W is the power stored in the cavity. The W
arid Po are calculated using the relations
- 0Os
W- e E2 abd (18)
106 MICROWAVB MATERIALS
(19)
where Eo is the maximum value of the electric field, a, b, d are the dimensions
=
of the cavity along breadth, width and length respectively, Rs (O'c5t 1 is the
surface resistivity of the sample and c5 is the skin depth at the frequency of
=
operation (2/.aJoJJoO')lfl asb. is the total surface area of the sample, Eo, JJo are
the pennittivity and penneability of vacuum. From the above relations, the
conductivity is given by
The dielectric constant t' and loss tangent (tan 8 =e"/e') are given by the
following relations
E'=tE[I+~I- ~] (21)
tl/=12 -II
11 = (I - R IT} I) (23)
(R - IT} I)
Thus from three experimental quantities, viz, the sample length, the frequency
difference between two extremes and the amplitudes of maxima, one can evaluate
e' and tan 8. This method can also help one to decide whether or not there are
any inhomogenities present in the sample such as large voids and cracks.
3.1 Ferroelectrics
Lanagan et al [12] have described this method for measuring on high permittivity
materials. This method can be essentially used on ferroelectrics and is based
upon S-parameters measurement using microwave network analyzer.
The specimen is a discontinuity for travelling waves and generally the incident
wave incidents at an angle on the air/dielectric boundary as shown in Fig. 3.
Since the incident wave has a reflection coefficient equal to unity and the
reflected wave can be described as complex quantity given by
(25)
INCIDENT WAVE
.
--------
(1 - f 2 ) e(-r I )
1'(1- f'2) e(-2rl)
S,1 5 21
p2(1_ p 2)e(-3rl)
p3(1_ p 2)e(-4rl)
Fig. 3. Plane wave incident to the interface of two different dielectric media.
21re'
p=;:;- (27)
where tan ~ = e" Ie'; ~ is free space wavelength and J,t is complex permeability
which is unity in case of nonmagnetic materials.
The sum of the reflected and transmitted waves can be expressed in terms
of the scattering parameters S11 and S21 which characterize two port device
such as a waveguide connected on both ends. The scattering parameters are
usually taken as complex quantities in terms of magnitude and phase given by
S21 = 1S211 e''9 (28)
The internal reflections shown in figure are accounted for by an infinite
geometric series and relations for S11 and S21 are given by
In order to minimize the complication to solve for e from the above equation,
an approximation is made in the above equation which requires S21 measurement
at several frequencies. For high dielectric constant and high loss materials,
{i'- exp (- 2rl) can be assumed to be less than unity. The above equation is
simplified to the following equation S21 = (1 - (i'-) exp (- 2r/). A plot of
as
log S21 vs frequency is linear per the above equation. The dielectric constant
and loss interms of S21 phase and magnitude are given by
(33)
110 MICROWAVE MATERIALS
I I
I
I
I
I 1 I
I
I i
I
where Jo(a) and J 1(a) are two Bessel functions of the first kind of the orders
zero and one respectively; Ko(/3) and K1(/3) are the modified Bessel functions
of the second kind of orders zero and one respectively; f3 is the radial wave
number outside the dielectric resonator and a is the radial wave number inside
the dielectric resonator. The values of a and f3 are given by
2 ]1/2
f3 = 1~ [(~) -.1 . (34)
2]112
a= j~ [ E'- (~) (35)
",=--
1 i1f
fo i1T
(36)
T
Fig. 5. Dielectric resonator in a cylindrical cavity.
Thus, in this chapter, emphasis was given to describe the various reliable
experimental methods to measure the dielectric constant, loss and conductivity
in the microwave frequency region. The materials include polymers, ceramic
oxides such as ferrites, titanates, dielectric resonators and high Tc superconductors.
REFERENCES
1. 1.S. Artman and T.E. Tamrnelwald,l. AppJ. Phys., 26, 1124, 1955.
2. B. Lax and K.I. Button, Microwave Ferrites and Ferrimagnetics, McGraw-Hill,
New York, 1962.
3. V.R.K. Murthy and R. Raman, Solid Stale Commn., 70, No.8, 847, 1989.
4. L.T. Buranov and I.F. Shchegoler, Translated from Pribory i Tekimilon
Eksperiments, No.2, 171, March-April, 1971.
5. Iroshi Kobayashi, lap. 11. Appl. Physics, 10, No.3, 345, 1971.
6. H. Zijlstra, Experimental methods in magnetism. 2 (North Holland), Ch. 2, p.70,
1967.
7. R. Pragasam, N.S. Raman, V.R.K. Murthy and B. Viswanathan, Physica Status
Solidi, Vol (a), 125, 583, 1991.
8. W.R. Tinga and E.M. Edwards, 11. Microwave Power, 3 (3), 112, 1968.
9. S. Roberts and A. Von Hipple, 11. Appl. Phys., 17,610, 1946.
10. W.H. Surber Ir. 11. Appl. Phys., 19,514, 1948.
11. C.O. Montgomery, Techniques o/microwave measurements, (McGraw-Hill Book
Co. Inc, New York), Ch. 10, 1947.
12. M.T. Lanagan, 1.H. Kim, D.C. Dube, S.1. lang and R.E. Newnham, Ferroelectrics,
82,91, 1988.
13. B.W. Hakki and P.D. Coleman, IRE Transactions on Microwave Theory and
Techniques, Vol MTT-8, pp. 401-410, 1960.
14. William E. Courtney. IEEE Transactions on Microwave Theory and Techniques,
Vol MTT-S, pp. 476-485, 1973.
15. D. Kaifez and E.I. Hwan, IEEE Trans. on Microwave Theory and Techniques,
Vol. MTT-32, pp. 666-670, July 1984.
5
Microwave Ferrites
G.P. Srivastava
Department of Electronic Science
South Campus, Benito luraz Road, New Delhi, India
Bijoy K. Kuanr
Zakir Husain College
lawaharlal Nehru Marg, New Delhi, India
1. INTRODUCTION
Emergence of ferrites arises due to the search for ferromagnetic materials with
low eddy current losses. The high resistivity of these materials is the primary
factor for controlling the eddy current losses, which is useful as cores for
transformers and inductors. The present status is that ferrites have been established
as materials of immense industrial use and ferrite devices find numerous applica-
tions in entire frequency range. At higb frequencies, as in the communication
field, the advantage of the ferrites become more pronounced specially at
microwave levels. Great bulk of the microwave applications will be quite
impossible without the assessment of ferrite and garnet materials.
The foundation of modem interest in ferrites was laid by Snoek [1] in 1946,
thereafter, the basic theory of magnetism developed by Neel [2] in 1948 was
the starting point for the rapid expansion of research and development activities
in this field of materials. The importance of ferrites is due to the fact that they
possess the combined properties of a magnetic material and an electric insulator
[3]. As a results. a high frequency electromagnetic wave can be propagated
through ferrites with very low attenuation. The work of Gorter [4], Goodenough
[5] and Blasse [6] showed that it is possible to make ferrites with different
substitution having a very wide range of saturation magnetisation and Neel
temperature values. These materials are also important from the point of view
of theoretical investigation because of their different type of spin arrangements
and exchange interactions.
Because of the large application of ferrites in microwave frequency range,
a designer of the ferrite devices has to know the detailed characteristics of the
material. Important parameters needed to characterise the ferrite material at
high frequencies are the resonance line-width (&I) and spin-wave line-width
(&I,~). &It is a measure of the power handling capability of the material.
Microwave Ferrites 113
There has been steady interest in developing new or improved latching type
high power ferrite phase shifters for use in phased array scanning antenna. The
device performance of phase shifter is Iimi~ by the ferrite material parameters
mentioned above. Inadequacies in currently available commercial ferrite and
garnet for use at high power levels has prompted the need for further material
development with improvement in power-handling capability as well as hysteresis-
loop properties. In addition, to the requirement for suitable hysteresis-loop
properties, materials for microwave latching phase shifters should have low
dielectric losses.
Lithium ferrite with chemical formula LiO.5F~s04 is an inverse spinel [7]
having a wide range of device applications. Several research programs have
been undertaken on this series of material to study its fundamental properties
and especially to develop high-power microwave materials from it. The utility
of Lithium ferrite and its substituted compositions as a class of materials for
application in microwave components and memory devices is due to the following
characteristics of the materials [8, 9].
1. Lithium ferrite can be prepared with a low value of tAH, with proper
substitutions of non-magnetic materials of the order of 50 oersted. This
is an extremely useful parameter for use in microwave devices.
2. Lithium ferrite can be used in high-power microwave devices. The
power-handling capability can be raised with appropriate non-magnetic
substitutions (like relaxing impurities) in its composition. Hence lithium
ferrite have come up as a low cost substitution for expensive garnets.
The unique properties of lithium ferrites which render them invaluable in
microwave applications is the employment of appropriate chemical substitution
in the basic formula unit. Although a wide range of substituted lithium ferrites
are available commercially, those in general used at microwave frequencies
include Ni, Zn, Mg, AI, Co, Ti etc.
The proper doping level and amount of dopants leads to material with high
Curie temperature, good density, low microwave dielectric losses, high hysteresis
loop squareness, cover a wide range of saturation magnetization values, low
stress sensitivity, high resistivity, high permeability and above all improved
microwave power handling capability.
by Griffithis [11] in 1946. Until today a lot of experiments have been made by
various workers for the complete understanding of relaxation processes in
ferromagnetic insulators. In a typical FMR experiment a sample is placed in a
uniform magnetic field large enough to magnetize it parallel to the field direction.
The absorption of rf power from the sinusoidally varying rf signal is a function
of Happ for fixed frequency. A resonance peak is obtained if the absorption is
plotted as a function of H app' The full width, in field units, at half maximum
absorption point is designated as the resonance line-width tJI. This simple
description of FMR contains the three basic ingredients common to resonance
phenomena are precession, resonant response and relaxation. The understanding
ofFMR was advanced considerably by Kittel [12] when he pointed out the role
of demagnetizing fields in determining the resonance conditions. The usual
resonance condition with r(gyromagnetic ratio) is satisfied for most materials
when demagnetizing [13, 14, 15] field are taken into accounL A phenomenological
description of the FMR absorption was given by Van Vleck [15]. He discussed
the observed line-width and various possible sources for line broadening.
Microwave phenomena have further expanded with discovery of YIG [16].
Sparkes [18] has made a detailed study of FMR in YIG and pointed out the
important role played by spin-waves. Kittel's theory was modified [19] for the
ferrimagnetic material which can be described by two sub-lattice systems of
oppositely directed magnetization. Further Brown and Park [20] had shown
that there were two types of responces, one in which the two sublattice magnetiza-
tions precesses about the applied field direction out of phase i.e. the exchange
resonance and the other when they precess in phase, which is the ferromagnetic
case. The size effect of FMR in ferrites was observed by Beljers and Polder
[21]; the resonance field was found to be a function of the diameter of the
ferrite sphere.
Yager et al [22] have obtained the linewidth of single crystal nickel ferrite.
It is 70 oersteds. Extensive studies were made on the variation of LlH with frequ-
ency [23], temperature [24], and ferrite composition [25]. The behaviour of
LlH with temperature could be attributed to the cation distribution [26] and the
valence state of the iron ion [27], in the ferrite. Lecraw and Spencer [28] had
shown that the linewidth in pure YIG was of the order of few millioersteds.
=
is characterised by a wave vector k whose magnitude is I k I 21ft)., where
). is the spin wave wavelength.
=
For the uniform mode k O. The relaxation process assumed that energy is
scattered from the uniform precessional mode into higher order modes [29].
But Clogston et al [30] provided a clear picture for the understanding of the
exact mechanism of the energy transfer by taking into account the effect of the
dipole-dipole interaction. The dipole-dipole interactions broadens the spin wave
dispersion relation into a band, which was named as spin wave manifold. The
spinwave manifold may be defined as that region of the dispersion relation
=
where spin wave analysis is valid. In this manifold k 0 spin waves also exist,
which are degenerate with the uniform precession.
The relaxation process assumes that energy is scattered from the uniform
precessional mode into degenerate spin wave modes. The analysis of this scattering
process depends upon the knowledge of the relationship between wavelength
and resonant frequency of such modes. According to the theory of Clogston
[30] the relaxation process can be visualized as follows. In a resonance experiment
the rf field puts its energy into the uniform precession. Thus the system has an
= =
excess of uniform precession magnons (k 0). The k 0 magnon can relax to
the lattice through three channels as shown in Fig. 1. In the first process a
k = 0 magnon can be annihilated and a k = 0 degenerate magnon can be created
=
in a two magnon process, with the k 0 magnon eventually relaxing to the
lattice through processes involving magnons and phonons. Secondly a k 0 =
magnon can relax to the lattice via interactions with magnons other than the
degenerate magnons. In the third process, a k = 0 magnon can directly relax
to the lattice through processes not involving other magnons. The two magnon
process [31] has the dominant mechanism for relaxation in polycrystalline ferrites.
lengths these fields must be taken into account. Walker [32] solved the problem
by including these surface demagnetization fields and the resulting modes are
=
called the magnetostatic modes. The uniform mode has k 0 and therefore is
a magnetostatic mode. Walker's calculations showed that the magnetostatic
modes has a spread wider than the spinwave manifold i.e. the upper limit for
the Walker modes does not correspond to an extension of the upper limit of the
spinwave manifold. The bottom limits however, do coincide.
The spinwave manifold shown in Fig. 2 can be divided into two parts. A
very flat region where the exchange interaction plays no part is the first region
and the second is a curved region where the exchange effect is appreciable.
o K - -.......
Fig. 1. The spin wave spectrum.
Geschwind and Clogston [33] and Schlomann [34] have explained linewidths
in polycrystalline materials by calculating the coupling of the uniform precession
with degenerate spinwaves of medium k values (i.e. in the no exhange region).
They have neglected the effect of spinwave with high k values, where the exchange
effects are appreciable. In spinel ferrites the scattering arises from a distribution
of the magnetic ion on the octahedral sites. The coupling between the uniform
precession and the high k-spin waves is thought to be stronger in the spinel
than in the garnet. So the spinels have greater line width as compared to those
of garnets.
Subsidiary Main
resonance resonance
c
I
o
...o
CII
.J:l
a
....
.Q
CII
a:
The presence of these nonlinear effects can seriously interfere with the
performance of microwave devices such as isolator, circulator and phase shifter.
The reduction of main resonance can impare the performance of resonance
isolators. The subsidiary resonance which appeared at low dc field cause serious
deterioration in the high power performance of phase shifter and circulators.
So it is important to understand the cause and cure of these nonlinearity.
Suhl [37] has explained these nonlinearities theoretically. Both the above
mentioned effects arise from power dependent coupling between the so-called
uniform mode of magnetic precession which is driven by the rf field and
certain spinwaves which become excited if the applied microwave field exceeds
a critical value. The spin waves which have the same frequency as that of the
applied field are responsible for the saturation of the main resonance and the
spin waves having the frequency one half of the signal frequency causes the
subsidiary absorption peak. The threshold value required for these non Ii neari ties
differ for the two types, but, both threshold (hcrj.) depend upon the linewidth,
the saturation magnetization, the geometry of the sample and the operating
frequency. In some cases the subsidiary absorption peak coincides with the
main resonance, this happens when threshold field are low.
Suhl [38, 40] presented a theoretical investigation on the behaviour of ferrites
at high microwave signal levels and showed that the nonlincariLies were connected
with two kinds of instability [39] of the uniform precessional motion of the
total magnetization against certain spinwave disturbances. And these disturbances
grow exponentially when the signal level exceed a certain threshold value.
118 MICROWAVE MATERIALS
threshold. The first order spinwave instability threshold has also been measured
[SO] as a function of sample shape (sphere, rod and thin disk), sample orientation,
pump configuration and magnetization state. The effect of sample shape and
pumping configuration on the threshold field for saturation was compared with
the theory. They have observed a consistent correlations between the data and
the theory which provided that domain shape plays the same role in determining
the threshold for partially magnetized samples that sample shape does for
saturated material.
Spinwave linewidth on polycrystalline YIG observed as a function of porosity
[51] pump configuration [52] and grain size [53, 60, 63] provides a clear
picture for the understanding of threshold mechanism. A spin wave transit time
model {55, 61] was given to explain the experimental data. Effect of nonmagnetic
inclusions on the spinwave linewidth in polycrystalline YIG was observed by
Schotter [57]. The threshold field for nonlinearity for first order processes on
the various configuration of static field angles were studied [54] on single
crystal YIG. Schouer [57] has studied the effect of rare-earth doped YIG
on spinwave linewidth and showed that the high power capability of ferrites
(,1HIc~ was increased with rare-earth ooping. Parallel pump [58] and subsidering
absorption [59] spinwave linewidth have been studied in porous polycrystalline
YIG (as a function of temperature) and single crystal YIG respectively. The
effect of crystalline anisbOphy for any arbitrary microwave pumping configuration
on spinwave instability theory [60] of single crystal YIG [62] provided a good
agreement with experimental data. Spin wave linewidth in polycrystalline YIG
[63] was compared to the theory of Sawado [62] for spinwave scattering by
nonmagnetic pores.
I. SUBSIDIARY ABSORPl10N
Suhl [37] proposed a mechanism for the high power effect which is bound on
the interaction of the uniform mode with spin waves of short wavelengths. In
"first-order Suhl process", where there is an appearance of a subsidiary peak,
=
energy from a single k 0 magnon is transferred to and creates two magnon,
having wave vector, k and - k respectively. This is shown is Fig. 4a.
Due to the conservation of energy principle these magnons must have one-
half the frequency of the k= 0 magnon. One particular pair, of mag non, among
many pairs with Wk = 0J/2 and with equal and opposite k, will be strongly couple
to the k = 0 mode and consequently lead to a nonlinearity in the absorption.
For a ellipsoid the critical field derived by Suh} [37] can be written as
/
-
K
- ./ /
-
q"'
K=O
I.
~
1'=0
i!".O ./_
/-i!" -K
(a) ( b) (c)
Case 1
This corresponds to the experimental observations when rok = fJJ/2 but ror not
close to ro, the subsidiary absorption occurs at an applied field less than that
required for main resonance. The threshold for this case can be written as [37]
Case 2
Merging of the subsidiary absorption with the main resonance occur for
rok = ro/2 = ror. This condition occurs provided
NtroM > ro/2 (4)
Here the final result for threshold is
h '1 = 2ro 71k 7]0 (5)
en roM(ro/2 + ro - NtroM) sin 8k cos 8 k
122 MICROWAVE MATERIALS
(10)
From standard microwave theory the threshold field, hc' incident on the sample
is given by the relation [37, 38]
Peak power = 70 kW
r Mo;it~ri;;g - , - --l Ql=600
Pulse width = 1 }J sec arm
Prec
P.R.F = 120 Hz Attn
,I
,Frequ-
Isolator ency
~ Imeter
I
,I ~
Calib rated ~.
I
crystal
I ~
~
l,ood CaUb rated
crystal
To osc.illoscope , ~
L ________ J To oscilloscope
...i·
Fig. 6. X-Band high power bench: hc:ril measurement in reflection mode. ~
-
126 MICROWAVE MATFJUALS
(ii) Pulse repetition frequency should be chosen in such a way that the duty
cycle should be as low as possible i.e. of the' order of 10-5, to avoid sample
heating.
(iii) Pulse width should be larger than the response time of the cavity.
(iv) The leading and the trailing edges of the magnetron pulses should be
avoided.
A pulse width of 1 J.JS and PRF of 50 or 100 Hz has been found suitable for
all requirements.
A TEI02 rectangular microwave cavity of a low Q, should be used so that
a slight detuning caused by the insertion of the ferrite sample could not change
the reactance' of the cavity.
The RF power provided by the magnetron operating in the pulsed mode,
passes through a high power ferrite isolater into a 10 dB directional coupler.
The unused power of the main arm of the directional coupler is terminated in
a high power load in order to minimize frequency pulling effect due to mismatch.
The desired RF signal is incident on the cavity through a circulator and a
shorting switch, which preceed the cavity. The shorting switch helps to measure
the incident power as well as the reflected power from the cavity which is
monitered with calibrated diode detector connected to a CRO. The precession
variable attenuator which precede the detector is kept at a constant level such
that the crystal output is constant. This ensured that the deviation of crystal
behaviour from ideal square law does not affect the reading. The power absorbed
by the sample as a function of increasing input power level is measured at a
fixed biasing field HIpp. From the graph of the return loss versus input power
level the sharp increase in the cavity reflected power gives the onset of instability.
This procedure is repeated for various values of the applied dc field. The
threshold field for non-linearity (hJ was calculated using the standard relation
given in Eq. 11. These values of he was plotted as a function of Happ and the
curve obtained is usually called as "Butterfly curve". Spin wave line-width
&It is calculated from the ~ (minimum) value USing the relation in Eq. 10.
The crystal IN21 with mount and the isolator gives an output of 200 mV
on the CRO when the power incident is 200 mW. All measurements are
obtained with spherical samples of 2 to 3 mm diameter to permit the applica-
tion of perturbation technique. The sample is placed in a region of minimum
electric field and maximum magnetic field, by a teflon rod sample holder
inside the cavity. Such placement insured small dielectric losses and nearly
uniform microwave magnetic field throughout the sample. The cavity is
continuously tuned to the magnetron frequency at each biasing field by a
tuning screw.
4 MICROWA VE STUDIES
levels on Gd3+ substituted YIG and C02+ and AI3+ substituted UTi ferrites are
given. The microwave field is applied parallel to the static field. The method
of measurements is described in section 3.2.
Figure 7 shows the variation of critical fields, hcrit as a function of the static
applied field for some specimen of garnet and ferrites respectively. These
curves are called the "Butterfly Curves". Here the angle (yt) between the pump
field and the static field is zero degree. The well known butterfly shape of the
curves are apparent for all these samples. It is evident from the figure that the
heri! decrease to a minimum. In this field range, the instability corresponds to
Ok = n/2 spinwaves with k values which are gradually decreases to zero at the
minimum, this is the one with lowest relaxation rate. The applied static field
at which the wave number decreases to zero and the butterfly curve has a
minimum for a isotropic material is given in Eq. (14) [42],
2,
Co F.U
90 I- • •
x x
0.000
0.005 •
• fI 0.01
80 I- • •
•• 0.02
0.04
70 fo-
t 60 r-
•
8
QI
••
u
• • o
•
J:.
50 fo-
•
40fo-
•
301-
1 1 1 • 1
1 1 10
1 G
,
1
0 <:)
201- <:)
<:)
<:) <:)
101- x x
x x
<:)
.- •
• • • • • •x 1
x
I
o
-
1000 2000 3000
Happ
Fig. 7 (ConJd.)
128 MICRowAVB MATERIALS
'IO~------------------------------------------------------~
GJ+/F.U 411'I0Il5
X 0.0 1800
150
•
t:.
0.1
1.6
1120
860
• 2.2 530
f
~ 10
50
; ;; ;:)
500 1000 1500 Happ (0.) _ 2000 2500
where
(15)
and
H.w =(Hullania + H.) - 41fM.Nz
Using Eq. (16) the theoretical butterfly minimum position is calculated and
observed are nearly the experimental value.
Above this minimum position threshold field increases rapidly with the
increase of static field for all the three series of samples [68]. The low level
substituted ferrites or garnets show smaller tendency for dipping at butterfly
minimum before the steep rise. This is in agreement with other published data
[31-33]. The experimental parallel pump data in these figures indicate that
IlHk is indeed Ie dependent. Moreover. increase of relaxing ions (like C02+ or
Gd~ below butterfly curve minima. makes IlHk a strong Ie dependent. Since
co the operating ffequency is fixed. the threshold (hmJ at each value of Happ
corresponds to a different Ie. These data clearly show that the threshold increases
substantially as the C02+ or Gd3+ content increases. The hen.. for maximum C02+
content i.e. 0.04 Co2+ ionS/F.U. is over ten times greater than the threshold for
the zero C02+ content sample. Gd3+ also increase lam, substantially. But the
increase of hen, by AI3+ is the least. Borghese [39] observed the variation of
IlHk for Mg-Mn ferrites with 2% cobalt with grain size. His results show that
IlHk is virtually independent of grain size. In the present investigation the
saturation magnetization is kept constant and the' average grain size is also
fixed for Co and AI ferrites. So the increase of lam, is only due to C02+ or AI3+
in addition to the LiTi ferrites. These results suggest that the relaxation mechanism
of low field loss contains no two magnon contribution. which is the major
effect of the ferromagnetic resonance r~iaxation.
In this calculation 8k is taken as 1f(1. which minimizes the critical field (hJ.
and for a isotropic material for parallel pumping he is given by
(17)
(18)
The square bracket term (SBT) represents the effect of anisotropy of the parallel
pump coupling. Eq. (17) is applicable to the isotropic materials like Co ferrites
and Gd YIG. but in case of AI ferrites where the crystalline anisotropy has a
large effect Eq. (17) does not hold good. So for these samples he is obtained by
130 MICRowAVE MATERIALS
Eq. (18). The experimental butterfly curves for AI ferrites do not show any
double minima. Sethares et al [10] observed double minima butterfly curves
for single YIG at 9.55 GHz. This double minima may be due to the spin-
=
wave switching phenomena. Setheres et al·ensure that only tPk 0 or 1r/2 are to
be selected.
In case of AI ferrites absence of any low field butterfly minimum ensures
=
the instability of spin wave with tPk 1r/2. The coupling of energy between fast
relaxers like Co or Gd through long range 4ipolar interaction is very strong.
Thus a large increase of instability is observed in case of Co ferrites and Qd
YIG. But in case of AI ferrites the coupling due to anisotropic field is not very
strong, thus a moderate increase of he occur.
For high static field, i.e. above butterfly curve minima the range of available
8k values becomes more restricted. At these external fields 8k starts decreasing
from 1r/2 to zero and k remains nearly zero.
The theoretical verification of the experimental data [68] are made by the
following models.
MODEL I
These parallel pump butterfly curves, for samples having large grain size (ao)
and small porosity (P), can be reproduced theoretically by considering the mean-
free-path or the transist-time model given by Vrehen et al [65] and Patton [63].
=
According to this model a generated spin wave having frequency COk coI2 travels
a distance 1 at a group velocity va before being destroyed. l is the mean-free-
path and is related to the grain size ao. It gives a life time for the spinwave,
l' = z/v, (19)
and the mean-free-path related spinwave Iinewidth can be expressed as
I
Nlk =-Y1'1 =-IylVal =-2Dk
l
(20)
where
=2yDk k + y4lrM.
A A
MODEL II
Scotter [57] has provided another model, which is a refinement of the transit-
time model. According to this model the spinwave linewidth is affected by the
size of the nonmagnetic pores, rather than the grain boundaries. Here the relaxation
has the form
1'- 4R (22)
- 3pvt>
where R is radius of the pore and p the porosity. The basic aim of Schotter's
model is that the pores in ferrites act as the scattering center for the travelling
spinwaves.
MODEL III
Sawado [62] has improved the pore scattering model by applying the screening
effects to the pore dipole potential. This method is used explicitly to explain
the experiment data here. The mean-free-path 1 as obtained by Sawado [62] for
a spinwave at k and 6" is given by
1 =f3!pa(6,,) (23)
where Pis the effective pore volume and is written as
P= 21l~+ 1 Po (24)
where
1(60 = f sin 8" d8" dtP" f 1P2 (cos 8)12 sin 8" (26)
1(6,,) is an integral which sums over all the angles into which the spinwave
may be scattered, 6" is the polar angle of the wave vector k. The spinwave
linewidth is then given by
132 MICROWAVE MATERIALS
(27)
As the experimental data given here shows a strong k dependence, the scattering
cross section cannot be obtained by integrating overall allowed values of Bt.
Because an integration overall spinwave angles provide a wave vector-
independent linewidth. So the suggestions made by Silber and Patton [64]
seems to be true for the samples investigated under present study. In this work
tJlk is calculated by using Eq. (27) instead of Eq. (28).
Theoretical butterfly curves for parallel pumping conditions are obtained by
including the wave-vector k dependence of the Iinewidth, which can be expressed
as
(29)
where A and C are two constants. The value of these constants are calculated
in the following way. The values of A are calculated from the he value at the
=
butterfly minimum of the experimental data with 0... 90°, k 0 and at Haw =
around the butterfly curve minimum position, by using Eq. (10). The values of
constant C are obtained from low field side experimental data of the butterfly
curves, where 0 ... corresponds to tr/2 and for nonzero k values.
The most striking feature of the present investigation is the rapid increase
of A values with the addi"tion of Co2+ and Gd3+ contents except AI3+ content
samples. In addition, the parameter C reflects the degree of k dependence of
l1Hk • From the calculated C parameters it is clear that the increase of the relaxing
ions (Co+2 or Gd+3) l1Hk are more and more k-dependent.
The theoretical fitting of the low field experimental data are quite good for
the threshold data below butterfly minimum.
But for higher static field the constant mean-free-path model does not fit the
experimental data. So, the scattering of spinwave at grain boundaries cannot be
the only mechanism which limits the spinwave life time in polycrystalline
ferrites. In this investigation an attempt is made to fit the data with pore
scattering approach given by Silber and Patton [64]. For the external static
field beyond butterfly curve minima l1Hk may be expressed in the form of
(30)
where l1H...{p) is given in Eq. (28). The parameter B is calculated by setting
he equal to the experimental.
The agreement between the high field theoretical and experimental data,
though not quantitatively perfect, are still good. The trend of both the curves
are same. Only the difference is that the theoretical curves diverge more rapidly
than the experimental curves. This may be due to the fact that the onset of
absorption is not sharp for the static fields beyond 2000 Oe.
Microwave Ferrites 133
The results obtained for the samples under present investigations having
large average grain size and porosity> 3% suggest that pore scattering contributes
a large part to the spin wave threshold.
Thus the pore scattering theory originally given by Sawado [62J and latter
on modification by Silber and Patton [64J presents a good theoretical fit to our
experimental data. The present results show that the threshold minimum, he (min)
=
occurs only at 8 k 1C/2 and not at some value of 8 k less than 90°, as given
by scotter [57J. The integral 1(80 appearing in the expression for scattering
cross section 0'(80 shows the 8k dependence of linewidth at higher static field
i.e. above butterfly curve minimum. This integral is not only dependent on the
porosity alone it depends on the size of the pore present in polycrystalline
ferrite. Scanning Electron Microscope photrographs of these samples show that
the inclusion of C02+ ion is in the composition increases the collective presence
of smaller pores. The collective present of smaller pores increase the cross-
sectional area R/r times than a single larger pore, where Rand r are the radius
of the larger and small pores respectively. The increase of cross-section area
has a marked affect on the spin-wave line width.
.. 30
8
'"
:l:
<l 20
• •
10
. . -
•
o~______~~:=====c==~:==~~==~~~:~=:·=-j
1.0. 2.0 3.0 4.0
5
5.ox10
K-
The results obtained here for the k dependence of spinwave linewidth is due
to a transist-time phenomena. Such dependence leads to the high power capability
of ferrites, since relaxing ions are more effective at increasing the L1Hk -+o values.
4.1.3 Spinwave Linewidth L111" with the Variation of Co2+ and AI3+
Ferrite and Gd3+ YIG
=
Room temperature X-band spinwave linewidth, for k 0 spinwaves calculated
from parallel pump butterfly by curves data, are shown in Fig. 9. Using standard
20r------------------------,
t
.......
III
0 15
~:.c
X
<I
.&;
~ 10
~
III
-=
III
>
0
~
c:
'Q.
1Il
o 0.1 0.2
Al (Conc.)-
Fig. 9. Room temperature X-band spinwave linewidth, for k = 0 spin waves
calculated from parallel pump butterfly curves data [68].
136 MICROWAVB MATERIALS
theories of Suhl [40] and Schlomann [41] the heri' data obtained from parallel
pumping experiment is used to calculate the value of LlHt for k = 0 (8 t = Tr/2)
magnons. The standard relation between the critical microwave field amplitude
for spinwave threshold heri' and spinwave linewidth LlHt, for parallel pumping
is given by
he'nt -- (..!!!....)
(Om
(~)
sin 8f min
(38)
where (0 is the pump frequency, (Om is r4TrMs with rthe gyromagnetic ratio.
Fig'. 9 dipicts that, for C02+ addition from zero to 0.04 ionslF.U. the X-band
spin wave linewidth increases by more than an order of magnitude. LlHt increases
approximately linearly with increase of Gd3+ in YIG. But in case of AI3+ the
increase of LlHk though linear but increase is very slow and also at higher
concenttation of A13+, LlHt appears to attain a saturation value. The sharp increase
in the value of LlHk arises due to the fast relaxation effect of C02+ ions in
octahedral sites, which is based on their crystal field stabilization energy. The
higher charge Ti4+ ions on neighboring octahedral sites and low charge U 1+
ions on adjacent tetrahedral sites help, in the stabilization of C02+ in octahedral
sites. The clustering effect of Ti4+ ions around octahedral sites, if any, is expected
even in the absence of C02+ ions and is not going to affect the material behaviour
on addition of the fast relaxing C02+ ions. The observed data can be explained
by considering the strong relaxation the effect of C02+ on the anisotropy of the
material and the enhancement of spin-lattice relaxation rates. The anisotrophy
cancellation effects attributed to C02+ ions do not appear where Ti 4+ ions are
used as the dilutant in the basic composition of lithium ferrites. C02+ ions in
octahedral sites. provides a large positive contributions to the negative anisotrophy
of the iron sub lattices. Through magnetic superexchange interactions, the C02+
anisotrophy is communicated to the iron sublattices. This caused rotation of the
Fe 3+ spins in the adjacent tetrahedral and octahedral sites. If the C02+ spins are
decoupled from the Fe3+ by the presence of Li 1+ in tetrahedral and Ti4+ in
octahedral sites, then the isolated C02+ anisotropy effects is undetected at these
small concentrations. This give rise to the fact that C02+ now behaves as a
paramagnetic ion, and this coupled to the Fe3+ ions only through dipolar fields.
The exchange isolation cannot prevent the occurrence of increased spin-lattice
relaxation rates, due to the cross relaxation between paramagnetic ions, which
can transfer energy to fast relaxers like C02+ by means of longer range dipolar
interactions. This leads to a sharp increase of spin wave linewidth.
In case of Al ferrite the increase of M1'r. is very small but still appreciable
to use this material in medium power microwave devices. This slow increase
of LlH'r. may be attributed to the coupling of energy to Fe3+ ions via crystalline
anisotropy. The strong point of Al addition over Co in UTi ferrite is that AI3+
does not raise the magnetic losses unlike C02+. So a fine control of aluminium
can make this group of ferrite to best use for medium power microwave devices.
The large increase of LlHt in Gd-YIG over the concentration range studied
may be attributed [68] in the following way. Substitution of Gd3+ in YIG
Microwave Ferrites 137
occupies the sites reserved for nonmagnetic yttrium. For garnets the principal
relaxation mechanism is provided by the rare-earth ions. Gadolinium like other
rare-earth ions relax the magnetisation in a two stage process. In the first stage
energy is coupled from the ferric ion system into the spin system formed by
Gd3+ ions. This energy is then dissipated to the crystal lattice in a second stage.
The exchange interaction provides the energy required for coupling between
the ferric ions and Gd3+ ions. This exchange interaction is an order of magnitude
weaker than the interaction between ferric ions. Gd3+ will behave as a para-
magnetic ion. The cross relaxation between paramagnetic ions channel energy
to fast relaxer through the fluctuating field it produces on the ferric lattice.
Hence there is an increase of tJ.Ht •
500
,....
II
9
:x: 300
<I
200
100.lt-----~
OL-__________- L____________L -_ _ _ _ _ _ _ _ _ _ ~
400
t
CII
2 350
:I:
<I
300
400
.x
f
.
.....
CD
:I:
<1
300
200~-----4------1-------~-----4--~
0.0 0.05 0.10 0.15 0.20
A\3+/Formula unit - -
Fig. 10. The variation of X-band resonance Iinewidth (LlH) with Gd-YIG
and Co and Al ferrites at room temperatures [68].
combine according to Hund's rule in such a way that the ion has no orbital
angular momentum. The spin orbit interaction is therefore very small and cannot
lead to a rapid relaxation as in the case of the other rare earth ions.
In case of C02+ ferrite the relaxation effect vary according to (4nMsrl. The
slope of the .1H vs C02+ content reflect the lower magnetisation of the samples
and the small increase of .1H with cobalt content is caused by the fast relaxation
mechanism of C02+ ions. The increase of .1/l with AI3+ may be due to poor
microstructure, increasing anisotropic field and also by increasing porosity.
The large value of .111 can be understood in terms of spin wave scattering. Due
to crystalline anisotropy the distribution of resonance field for the randomly
oriented crystallites induces the broadening of linewidth.
Microwave Ferrites 139
REFERENCES
42. E. Schlomann, 1.1. Green and U. Milano, J. Appl. Phys. 31 Suppl. (1960)
No. 5 p. 386S.
43. R.C. Lecraw, E.O. Spencer and C.S. Porter, J. Appl. Phys., 29 (3) (1958)
p.326.
44. J.J. Green and E. SchIomann, J. Appl. Phys., 33 (S) No.3 (1962) p. 1358.
45. 1.H. Saunders and J.J. Green, J. Appl. Phys. Suppl., 33 (3), (1963) p. 1372.
46. E. Schlomann, 1.1. Green, J.H. Saunders, IEEE Trans. on Magnetics, MAO-l
(1965) p. 168.
47. 1.R. Samuel Dixon, J. Appl. Phys., 38 (1967) No.3 p. 1417.
48. J.J. Green and C.E. Patton, 1. Appl. Phys., 40 (i) (1969) p. 172.
49. C.E. Patton, 1. Appl. Phys., 40 (7) (1969) p. 2837.
50. C.E. Patton and J.J. Green, IEEE Trans. Mag., MAO-5 (3) (1969) p. 626.
51. C.E. Patton, Proceedings of the ICF, (1970) p. 524.
52. C.E. Patton, 1. Appl. Phys., 41 (1) (1970), p. 431.
53. C.E. Patton, J Appl Phys., 41 (4) (1970) p. 1637.
54. D.O. Scatter, 1. Appl. Phys., 32 (10) 1971) p. 4088.
55. Yu. M. Yakovlev, Yu N. Burdin, Yu R. Shilnikov and T.N. Bushueva, Soviet
Phys-Solid State, 12 (10) (1971) p. 247S).
56. C.E. Patton, IEEE Transactions on magnetics (1972) p. 433.
57. D.O. Scatter, J. Appl. Phys. 43 (11) (1972) p. 4813.
58. 0.0. White, C.E. Patton and C.A. Edmendson, J. Appl, Phys. 50 (3) (1979)
p.2118.
59. C.E. Patton and Wolfgang Jantz, J. Appl., Phys., 50 (11) (1979) p. 7082.
60. C.E. Patton, Phys, Stat. Sol. (b) 92 (1979) p. 171 and 93 (1979) p. 7082.
61. Om Prakash and C.M. Srivastava, Bull. Mater. Sci., 2 (3) (1980) p. 181.
62. Eikichi Sawado, Proceedings of ICF (1980) p. 818.
63. C.E. Patton, Proceeding of ICF (1980) p. 807.
64. L.M. Silber and C.E. Patton, IEEE Trans. Mag., MAO-18 (6) (1982) p. 1630.
65. Q.H.F. Vrehen, H.O. Beljers and 1.0.M. del au, IEEE Trans. Magn. MAO-5
(1969) p. 617.
66. J.J. Green and T. Kohane, SCP and Solid St. Tech. 7 (1964) p. 46.
67. Isidore Baby and Ernst Schlomann, J. Appl. Phy. Suppl. 33 (1962) p. 1377.
68. Bijoy Kumar Kuanr; Ph.D. Thesis, University of Delhi, 1992.
6
Microwave Lithium Ferrites
Pran Kishan
Solid State Physics Laboratory, Delhi, India
1. INTRODUCTION
Among the various magnetic oxide materials used in devices operating at micro-
wave frequency ranges lithium ferrite is presently occupying a prominent position.
Although its potential as rectangular loop material was being utilised for long
in memory devices the exploitation of its attractive feature as a microwave
material was much delayed due to excessive losses observed in early samples.
Many researchers working in the field put up a good deal of effort in the early
70s to obtain lithium ferrites with improved dielectric properties. Preparation
of low loss lithium ferrite was first reported in 1971 by Collins and Brown [1].
Considerable interest has persisted in lithium ferrites since then. With the
establishment of reproducible procedures for the preparation of lithium ferrites,
there has been no looking back and at this juncture lithium ferrites are among
the most wanted materials for the microwave frequency ranges. The family of
lithium ferrites has expanded to such an extent that it now covers a very wide
spectrum of properties for utilisation in microwave devices. The frequency
range of its use extends even to millimeter wave bands.
Braun [2] was first to show that lithium ferrite with chemical formula
Lio.sFe2.S04 is an inverse spinel. The divalent ion in this case being a composite
ion (Li ~~s Fe~:S). The compositional variations made possible by incorporation
of a variety of other metal ions in its formula unit have given rise to lithium
ferrite family as a class of material with many special features [3, 4]. These
features are:
1. Unsubstituted lithium ferrite (Lio.sF~.s04) has the highest Curie tempe-
rature (Tc • 640 0c) among the ferrimagnetic oxide materials. High Tc
signifies temperature stability of its magnetic properties. The substituted
compositions of lithium ferrites also inherit this property from the parent
material. A case of materials belonging to different ferrite families
and a comparison of Tc values for a typical value of magnetisation
(4nMs = 1000 Gauss) is illustrated in Fig. 1.
2. The lithium ferrites possess excellent rectangular loop characteristics.
From its earlier use in memory core industry the present application in
latching microwave devices is a natural extension.
142 MICRowAVE MATERIALS
1 UTi fERRITES
2 li TiZn fERR1TES
3 YN. GARNfTS
" Hg Hn Al fERRITES
I
3ID.
-
VI
VI
:::J
rg naa
l!J
VI
l:
5- 1aaa
,'1.,
I
I
lh
• '2ID laD It.. saa nD
CURIE TEMPERATURE (oC) ..
FIg. 1. Saturation magnetisation (4nMs) vs Curie temperature (Tc)
for different microwave ferrites.
NiZn ferrites 9 to 12). High e' values are significant from the view-
point of size and weight considerations of the device.
6. The dielectric loss tangents of lithium ferrites presently available are
comparable with other microwave ferrite series (tan c\ < 0.0005). It has
become possible with the advancements made in the processing methods
and from the compositional considerations.
The above features have contributed in the establishment of lithium ferrites
to their present status in microwave magnetics.
2. MATERIAL PROPERTIES
The choice of the ferrite for a microwave device is decided by the working
frequency, power level of operation and whether it works at resonance, far off
resonance or at remanence. The properties of the ferrite optimised in various
aspects determine the feasibility of the device and its level of performance. In
this connection the following parameters of the material are of technical
importance from the viewpoint of its utilisation in devices.
tan c\ =e"/e'
has values less than 0.001. For lithium ferrites e' has a high value in the range
14 to 20 and typical dielectric loss factors of 0.00025 are obtained.
The dielectric loss occurs primarily due to electrical conduction in the material.
The conduction by hopping mechanism takes place between Fe2+ and Fe3+ ions
present on equivalent crystallographic sites in the structure of the ferrite. The
desired values of resistivity of ferrite material for low dielectric loss at microwave
frequencies is more than 107 ohm cm. In lithium ferrite, represented as
Li 1+ 3+ 0 2 -
o.s Fe 2.S 4
there are no Fe2+ ions and a low loss factor is expected for it. However the
preparation of the ferrite requires high temperature ftring at 1150-1250 °C for
obtaining dense material. At these temperatures oxygen dissociation and lithia
volatility occurs resulting in formation of non-stoichiometric composition. The
consequence is reduction of Fe3+ ions into Fe2+ ions and high dielectric losses.
In addition the control of impurity ions of higher and lower valence in the
structure and reduction of macroscopic and microscopic heterogeneities (e.g.,
pores, non-magnetic inclusions etc.) are also very essential. Suitable techniques
have been developed to overcome it, namely sintering at lower temperatures
144 MICRoWAVE MATERIALS
2.2 Magnetisation
The magnetisation of ferrites arises from the antiparallel alignments of the
magnetisation of the two sublattices. The magnetic moments on each sublattice
are arranged parallel to each other and the difference between the magnetisation
of the two sublattices results in a net magnetic moment. The saturation
magnetisation (4nMs) is defined as the magnetic moment per unit volume when
all its individual megnetic domains are aligned by the application of an external
magnetic field. However the magnetic ordering is disturbed as the temperature
of the material is raised. Magnetisation decreases and ultimately disappears at a
characteristic temperature of the material called its Curie temperature (Tc).
It is the specific chemical formulation of the ferrite which primarily controls
its saturation magnetisation. The process parameters involved in the preparation
of the material also play an important role and for some cases the distribution
of ions on the two sublattices is affected by the firing schedule of the material.
The 4nMs of Lio.5F~504 which is - 3750 Gauss at room temperature can be
varied by substituting appropriate other metal ions in the crystal lattice. It has
become possible to prepare substituted lithium ferrite compositions with 4nMs
value covering a wide range from low value of a few hundreds to 5000 Gauss.
The Curie temperature, 640°C for the un substituted lithium ferrite, however
decreases with the increasing substitution levels.
Several series of lithium ferrites for pticrowave applications are available
with Tc varying from 80 to 6200C depending upon the 4nMs and other JrOperties.
The temperature variation of the magnetic properties of lithium ferrites are
superior to other ferrites due to their inherent property of high Tc. Only some
grades of garnets possess better temperature characteristics but their high cost
and limited range of magnetisation restrict their utility.
resonance ("") peak, and it includes all magnetic Joss processes. The contributions
to tJl come from spin-lattice relaxation and magnetocrystalline anisotropy.
Presence of non-uniformities in the ferrite medium such as pores, non-magnetic
inclusions, cracks, surface roughness and variation in volume density of magnetic
ions, all tend to increase the tJl value. Suitable substitution of several ions like
ZnZ+ in the chemical formulation of lithium ferrite is also quite effective in
adjusting the tJl of the material. The presence of relaxing ions like eo2+ tend
to increase it Lithium ferrites of low linewidth values have been developed by
the chemical formulation techniques. This has led to the development of lithium
ferrites as low cost substitutes of garnets in several devices.
A number of microwave devices operate at fields away from the resonance
e.g. a latched phase shifter at remanent magnetisation. For such devices off
resonance linewidth is considered as the relevant loss parameter. The linewidth
measured as a function of external magnetic field is expressed as effective
linewidth (tlHea). The measurement of tlHeCf with external magnetic field for
lithium ferrite was first reported by Koelberger et al [6].
=
where (J) is the incident frequency and co... r4nMs. The factor C has value
of the order of unity. The spinwave resonance linewidth tlHk is a material
parameter and is considered to be a measure of the critical field. For normal
microwave ferrites tlHk is 1 to 2 Oe. Higher values of tlHk for ferrites are obtained
by incorporation of fast relaxing ions in the ferrite composition. However some
increase in low-power magnetic loss accompanies it. Fine grained materials
also exhibit improved spinwave linewidths and better peak power handling
capability without any significant increase in low power loss.
sample this is done by driving a pulsed current through a threading wire wound
on the toroid which can produce a field H» He. Latched remanent positions
at any in-between values can be reached by partially switching. the toroid.
Several types of phase shifters and switches are based on the latched magnetisation
operation. The shape of the hysteresis loop plays an important role for such
devices.
Ferrite materials with rectangular loop characteristics (high remanence ratio
and low coercive force) are needed for this type of devices. The lithium ferrite
materials employed in the fabrication of latching devices have R > 0.85 and
He - 1 Oe. The switching coefficient and switching energy are two other
important parameters for such a device and are governed by the hysteresis loop
parameters of the material and the external circuit used in'the device.
Stresses produced in the ferrite during shaping, machining processes and
fabrication, affect the shape of the hysteresis loop and reduce the remanence
ratio through magnetostriction effect as shown in Fig. 2 [5]. Ferrites with low
stress sensitivity of remanence are essential for the microwave latching purposes.
41TMr
R= 417Mr
47TMs
-------------r~~~----------~H
He
-NORMAL
-WITH STRESS
are: saturation magnetization, Curie temperature, loss factors and the rectangularity
of the hysteresiS" loop.
The several series of lithium ferrites that have emerged out of the parent
composition have been prepared by substituting a number of other metal ions
in the ferrite composition. For microwave application the compositions that are
prepared are represented by quite complicaled chemical fonnulae. A typical
composition includes several cationic constituents which can be divalent, trivalent
and tetravalent ions, each included for one or more specific purposes. The
beneficial and deleterious effects of some of these ions has been discussed by
Baba et al [3]. Each ion has a different role to play in controlling the properties
of the material. The resulting composition is derived keeping in view the desired
properties of the product. This molecular engineering for lithium ferrites and
its bearing on the properties is discussed briefly below.
Zn,Fel-l lLio.5-I/lFe1.S+IIiIO"
For higher z values (> 0.4) this substitution weakens the exchange interaction
and does not result in any further increase in 4trMs, on the other hand a fall
in magnetisation is observed. Similar behaviour of magnetisation is observed
in all spinel ferrites on zinc substitution.
Zn substitution is also very effective in controlling several other properties.
It promotes grain growth and densification during sintering and lowers the
anisotropy. All this results in decrease in resonance linewidth and coercive
force. Lower remanence ratio values are also obtained simultaneously [10, 11].
Resonance line widths of around 25 Oe have been achieved [12].
Lio.5+I/2-c12Ti,zn,F~5-31~"
Studies on the effect of Zn and Ti substitutions on the static magnetic properties
in lithium ferrites have been carried out by several authors [5, 13-19-]. For a
typical LiZnTi ferrite composition the distribution of cations over the two
sublattices is represented as
forz>t
and
forz<t
Mn 3+ + Fe2+ -+ Fe3+ + Mn 2+
+-
The reaction is favoured in the forward direction.
Another notable effect of Mn ions is in lowering the stress sensitivity of the
material. The magnetostriction constant (l) for Lio.sF~s04 is - 8 x 10~ [20].
It was observed long back by Baltzer [21] that the system (1 -x) Lio.sF~s04·
xLio.sMn2.s04 is said to have its saturation magnetostriction approach zero
value at x =0.12. Higher value of remanence ratio was also observed in the
neighbourhood of this composition. Like other non-magnetic ions Mn also
decreases the Curie temperature.
The Mn substitution is necessary in lithium ferrites particularly for latching
applications where low magnetrostriction is needed. Material becomes less
sensitive to stresses, which are introduced in the machining process of ferrite
parts by mechanical pressure in device fabrication and by thermal effects, by
Mn substitution in the ferrite composition.
4. MATERIAL PREPARATION
Lithium ferrites were earlier finding application in memory cores due to its
rectangular hysteresis loop properties. Their wider use particularly for microwave
devices was restricted due to the difficulties experienced in sintering the material
at the high temperatures employed to achieve high densities in stoichiometric
form. The irreversible loss of lithia [25] and oxygen during sintering was the
main cause that made lithium ferrites technologically difficult to prepare. Low
resistivities of LiZn ferrites, sintered at 1 175°C, were observed even in the
case when firing was carried out in oxygen atmosphere [11]. This was attributed
to the loss of oxygen and lithia occurring at the high sintering temperatures
resulting in the reduction of Fe3+ to Fez+.
The above said hindrances in making lithium ferrites useful for microwave
frequencies were overcome by employing sintering aids like bismuth oxide,
vanadium pentoxide niobium oxide etc. [26]. The first two are low melting
materials and are effective by liquid phase sintering process. The addition of
NbzOs enhances the sintering by increasing bulk diffusion occurring due to
increased vacancy concentration caused by solubility of Nb5+ in the ferrites [27].
Bi z0 3 has been found to have an edge over others and has been adopted in
manufacturing of lithium ferrites for microwave applications. The addition of
Bi z0 3 in small amounts has been reported by several authors [28, 29, 2] for the
preparation of dense materials of both pure and substituted lithium ferrite
composition. This aspect of the lithium ferrite preparation, which has played
an important role in bringing up these materials to the present level, is discussed
below.
A lithium ferrite composition is prepared by the conventional ceramic
procedures. A small amount of Bi z0 3 is mixed either at the starting stage or
after the presintering. This makes the material sinterable at comparatively low
temperatutes (950-1050°C) where the loss of lithium and oxygen are minimal.
There have been speculations in the literature regarding exactly where and
in what form Biz~ locates in the polycrystalline ferrite bodies. Baba et al [2]
incorporated Bi3+ in the formula unit of the ferrite replacing Fe3+ ions. Similarly
Peshev and Pacheva [30, 31] included Bi3+ as a part of the formula unit although
they considered it merely illustrative of the composition. Simonet and Rermosin
[32] and Green et al [33] considered small quantities of Biz0 3 as a simple insoluble
additions segregating mainly at the ferrite grain boundaries. Microstructural
and thermal analyses carried out have confirmed this and have given a clear
picture of the role played by Biz0 3 [29, 30, 31].
In the chemical formula unit containing several substituents, like the one
given in Section 3, when a small amount of Biz0 3 is added, density upto 99%
of the X-ray density is achieved. Biz0 3 content of 0.25 to 1.0 % by weight has
been found to be most appropriate. Riger amount of Biz0 3 interferes with the
crystaUisation process and hampers grain growth. It leads to lowering of densities
and the material properties are adversely affected. Smaller amounts are quite
Microwave Lithium Ferrites 151
t
-..
Ct
Ct
99
c:a
!
.....
97
c:a
-
95
f!
.3-
""
:1 ~~b:
a:
(b)
~
I:J
:>
~
(el
...t
UI
31D
-
0
:z:: lID
<I 180
5 ld)
'-'I
I
It
t
-
III
g
3
1
...5
....
...
::c 1
a:
0 to 2.0
Bi20 3 as a sintering aid also improves the mechanical properties of the sintered
ferrite.
The thermal analysis of Bi2~ rich mixtures with lithium ferrite shows that
it melts eutectically at around 770°C while the melting point of Bi20 3 itself is
820°C. The microstructural studies by electron microprobe technique have
depicted the grain boundary composition to be rich in bismuth while it does not
appear in the grains. It is inferred that eutectically melting composition of
Bi2~ rich ferrite is responsible for lowering the sintering temperature and
promoting grain growth by the liquid phase sintering process.
Presently addition of a small amount of Bi20 3 at the starting stage of the
lithium ferrite preparation is being adopted on a routine basis. For certain cases
such as low linewidth ferrites the concentration of Bi2~ is kept at very low
levels as it also acts as a unwanted non-magnetic impurity and proves deleterious
for this property. All lithium ferrite compositions containing Bi20 3 are calcined
at temperatures not exceeding 800°C followed by comminution and pressing.
The material gets sintered to high densities in the temperature range 1000 to
lOSO°C with well developed grain structure.
The other aspect in the material preparation of the ferrites is the microstructure
control. Several properties of the ferrites namely coercive force, remanent ratio
and resonance linewidth depend to some extent on the grain structure of the
material. Grain size effects on microwave ferrite magnetic properties have
been described by Inui and Ogasawara [3S]. Several new techniques are now
being used in the ferrite preparation to achieve the desired control on the
microstructure dependent parameters. For powder preparation besides conventional
methods other processes like co-precipitation, cryochemical and freeze drying,
solution spray draying, fluid bed etc. are used in practice. The primary aim in
all these methods is to prepare thoroughly dispersed, uniform and homogeneous
powders for carrying out most complete reaction to form the ferrite.
The second basic step in the preparation of polycrystalline ferrites is
densification. The general approach is to compact the powder in the required
shapes and f1l'e at high temperatures in a suitable atmosphere. The firing schedule
is accordingly adjusted for achieving optimal material properties. For lithium
ferrites containing Bi2~ as a sintering aid the firing is generally carried out
in air. For some special purposes oxygen atmosphere is also used.
The techniques of isostatic pressing, hot pressing, isostatic hot pressing etc.
are used for preparation of some special grades of materials like high power
ferrites. These methods give a better control over density and size of the crystal
grains.
t
2000
1000
o
-50 50 150 250
TEMPERATURE (Oe)
---
Fig. 4. Temperature variation Qf saturation magnetisation (4nMs)
for various grades of type Ia and lb.
Type 4nMs Tc (0C) E' M-l (Oe) M-lk (Oe) tan eSc X 10-4 tan c5u. X 10-4 R He (Oe)
(Gauss)
LiTi 800-3500 3()()....{i20 15-19 350-500 2 <5 <5 > 0.9 1-2
LiTiZn 250-3000 120-500 16-20 100-300 2 <5 <5 > 0.85 0.6-1.5
4000-5000 520-400 15 200-400 2 < 10 > 0.9 2-4 ~
High Power 600--2000 200-450 17-19 300-700 S7 <5 <10 > 0.85 1-2 ~.
Low Linewidth 800-3000 150-350 15-19 < 100 2 <5 S 10
~
~
t"'"'
§:
~.
~
~.
...,
VI
VI
-
156 MICRowAVE MATERIALS
strong positive anisotropy. The spin wave resonance linewidth (t1Hk) of the
ferrite is found to increase by almost an order with extent of the substitution
of C02+ as small as 0.05 ions/formula unit (FU) in the chemical composition
(Fig. 5).
25
-..
I I I I
Cii
0
lITi FERRITE
:
<I
20
•
~
4 lr'Hs .22506 (38)
4rr,.... 125116 (39) )(
i5 +
sa 15 - •
~ + •
""~
:.
a;
a..
111 ..
5
,. • •
.."
It
i
.11 I I I I
Cos. IONS IF U _
Bannerjee et al [36], Brower and. Patton [37] and later Dionne [38] have
observed an apparent paradox in the properties of C02+ substituted lithium ferrites.
The presence of C02+ in the ferrite has simultaneously two types of effects
namely through anisotropy and relaxation. An anisotropy cancellation is expected
at a particular cobalt concentration, and a minimum in 1¥sonance linewidth
should be observed. The hysteresis loop properties are also supposed to reflect
this anisotropy effect. These authors have reported that such a situation is not
observed in titanium substituted lithium ferrites. A new model of cation clustering
by C02+ has been put forward for understanding the observed behaviour of
anisotropy effects [38].
Figure 5 shows that C02+ concentration of 0.01 ions per formula unit increases
t1Hk by more than two fold [38, 39]. A simultaneous increase of magnetic
losses also occurs. For devices working at moderate power levels, it would be
desirable to introduce less than 0.01 ions/FU (C02+) for synthesising the optimum
material. The control of cobalt content in these small concentrations on
reproducible basis in the preparation of ferrites is found to be rather difficult,
t1Hk values being extremely sensitive to C02+ concentration. In the recent work
[40,41] an alternate course of aluminium substitution in LiTi ferrites has been
suggested. AI3+ content upto 0.2 ions per formula unit have been used and
results obtained on several properties like spin wave resonance linewidth,
resonance linewidth, remanence ratio and coercive force are given. Fig. 6 depicts
Microwave Lithium Ferrites 157
4.. 0
o
I .,
2.0
1.0
D 0.1 0.2
All .. IONS / FU •
Fig. 6. Variation of spinwave resonance linewidth (tlHk ) with aluminium content.
the variation of ,1Hk with the AI concentration, the value increasing in a controlled
manner from 1.8 to 3.2 Oe for Al concentration varying from 0 to 0.2 ions/FU.
It is also noticed that there is a tendency of ,1Hk to attain a saturated value for
higher Al concentrations. In comparison the ferrite containing Co shows
monotonic rise in ,1H". The effect of aluminium concentrations on 41rMs and
Tc is rather large and has to be taken into consideration while arriving at the
appropriate composition by suitably adjusting the other cationic contents like
titanium.
The aluminium and cobalt substituted lithium ferrites have been evaluated
in reciprocal phase shifter configuration at moderately high peak power levels.
Fig. 7 shows the experimentally observed results [41]. For a composition free
of both A13+ and C02+ the onset of nonlinear effect occurs at around 100 Watt
peak power while it is higher than 300 W for aluminium containing ferrite
(0.1 ionslFU). The C02+ (0.004 ionslFU) is also effective in raising the threshold
power level but it is accompanied by some increase in insertion loss.
FREQ. 5·46Hz
2
r J
I
!iJ 0.2
&on
g
r
z
5 8.1
~
~
:>
------- -!.
~ 0 ----
:5
~ Rderente
ao::
magnetostatic wave and bubble memory devices. But here also it is the YIG
material films, grown by liquid phase epitaxy (LPE) methods, which have
dominated the scene. It has been established that thin film approaches are
highly attractive for microwave and millimeter wave devices but the problems
cOnnected with producing films of required thickness and quality have restricted
the desired advancement. The motivation for thin film ferrite devices is also
provided by cost, size and weight considerations. There are several thin ferrite
film microwave devices reported in literature having potential for competing
with single crystal devices [42, 43]. The different aspects of ferrite thin films
are described by_ Glass [44].
The growth of lithium ferrite and lithium ferrite-aluminate films by LPE has
been investigated by Glass et al [45] and Van der Straten et at [46] respectively.
Interest in ferrite films has also extended to polycrystalline materials. Thick
films deposited from pastes containing lithium ferrite have been evaluated in
microstrip edge guided isolators and circulators [47]. Other techniques attempted
include ferrite plating [48] and arc plasma spray. Millimeter wave ferrite phase
shifters have been demonstrated by employing the latter method [49]. Experiments
have been carried out on deposition of ferrite films on GaAs substrates [50].
The rapidly growing field of monolithic microwave integrated circuits
(MMICs) lias created renewed interests in development of ferrite film devices.
From the viewpoint of compatibility it is desired that both ferrite and
semiconductro devices are fabricated on the same chip for realizing monolithic
integration. In this connection the three possible approaches for deposition are-
ferrite film on semiconductor substrate, semiconductor film on ferrite substrate
or both semiconductor and ferrite films on a mutually compatible substrate. As
mentioned above attempts have been initiated for deposition of ferrite films on
GaAs substrates, but the results are not very satisfactory. Other approaches are
also in a stage of infancy.
For deposition of single crystal films lattice match between the substrate
and film material is a basic requirement. The lattice constant of ferrite spinels
is - 8.4 A and of III-V compounds is - 5.9 A. The mismatch of lattice is quite
obvious. Schloemann [50] has pointed out that the lattice can match along a
[100] interface with the two lattices rotated by 45 0 with respect to each other.
In such a case the ratio of the two lattices should be "2 for a perfect match.
This requirement is coincidentally met by lithium ferrite (8.33 A) and GaAs
(5.64 A)/lnP (5.87 A), the ratio being quite close to "2. It has been- further
suggested that any residual mis~h of a few percent between the two lattices
can be absorbed by the deposition of suitable buffer layers. This approach is
expected to provide some interesting results for MMIC compatible ferrite
components.
better temperature stability. Fa phase shifter with higher peak power specifications
lithium ferrites of type II are preferred. Based on the design--eonsideration in
a C-band phase-shifter lithium ferrite of 41t'Ms 1200 Gauss is used while an
X-band phase shifter employs material with 41t'Ms around 2000 Gauss. As a
thumb rule the magn~tisation of a material selected for the phasor is about
one-fifth of the centre frequency of the device consistant with the relation
4KMs/m« 1. In high frequency phase-shifters operating at 35 GHz and above
ferrites of 5000 Gauss are used. limited by the highest value of magnetisation
available among the ferrileS.
The shaping and machining of the ferrite in the various forms like toroids.
rods. yokes etc. for phase shifters is an important step in the use of ferrites for
this application. The production methods have been established for uniform
reproducibility alongwith good mechanical properties in the various configurations
of lithium ferrite materials.
The applications of both reciprocal and non-reciprocal phase shifters have
been extended as control elements in variable power dividers [57. 58]. Further
advancement of these devices fa antennas having polarization agility development
of a simultaneous dual polarization phase shifter has been reported [59].
The toroidal non-reciprocal and dual mode reciprocal~ largely based on
lithium ferrites. presently represent the major ferrite device market. A number
of phased array antenna programmes (e.g. PA1RIOT and AEGIS) have boosted
the production of ferrite phasors [60].
REFERENCES
17. M. Rosenberg, P. Deppey, S. Dey, U. Jansen, C.E. Patton and C.A. Edmondson,
Trans. IEEE, MAG-18, 1616, 1982.
18. Pran Kishan and K.K. Laroia, Adv. in Cer., 15,299, 1985.
19. S. Phanjoubam, D. Kothari, J.S. Baijal and Pran Kishan, Sol. State. Commn.,
68, 549, 1988.
20. J~ Smit and H.P. Wijn, Ferrites, Wiley NY, 1959.
21. P.K. Baltzer, US Patent 3034987, 1962.
22. R.G. West, J. App. Phys., 34, 1113, 1963.
23. M.P. Bunina, E.V. Lebodera, Al. Pilshchikov and I.I. Silvestrobich, Sov. Phys.-
Sol. State 12, 341, 1970.
24. H. Wang et al Acta Eleetronica Simica, No. I, 64, 1.979.
25. G. Bandopadhyaya and R.M. Fulrath, 1. Am. Cer. Soc., 57, 483,1974.
26. H.B. 1m, Proc. ICF-3 (Kyoto, Japan), 281, 1980.
27. H.T. Kim and H.B. 1m, Trans, IEEE, MAG-18, 1541, 1983.
28. V.G. Glotov, Porosh Met. 10,27, 1970.
29. K.D. Dugar Zabon, Porosh Met., 11, 60, 1971.
30. P. Peshev and H. Pacheva, Mat. Res. Bull., IS, 1055, 1980.
31. P. Peshev and H. Pacheva, Mat. Res. Bull., IS, 1199 1980.
32. J.J.Green and H.J. Van Hook, Trans. IEEE, MTT-25, 155, 1977.
33. W. Simonet and A. Hermosin, Trans. IEEE, MAG-14, 903, 1978.
34. Pran Kishan, D.R. Sagar, S.N. Chatterjee, L.K. Nagpaul, Nitendar Kumar and
K.K. Laroia, Adv. In Cer. 15,207,1985.
35. T. Inui and N. Ogasawara, Trans, IEEE, MAG-l3, 1729, 1977.
36. S.K. Bannerjee, P.D. Baba, B.1. Evans and S.S. Hafner, J. Phys. (Paris) Colloq.
C. 145, 1971.
37. C,J. Brower and C.E. Patton, 1. Appl. Phys., 53, 2104, 1982.
38. G.F. Dionne, J. Appl. Phys., 57,3727, 1985.
39. B.K. Kuanr, P.K. Singh, Pran Kishan And G.P. Srivastava, Proc. ICF-5 (Bombay,
India), 1005, 1989.
40. Pran Kishan, N. Kumar, B.S. Matheru, Chandra Prakash, K.K. Jain and G.P.
Sharma, Proc. ICF-5 (Bcmbay, India), 949, 1989.
41. Pran Kishan, G.P. Sharma, Nitendar Kumar, K.K. Jain and B.K. Kuanr, Proc.
Tenth Int. Con!. on Microwave Ferrites (Poland), Sept. 1990.
42. E. SchIoemann and R.E. Blight, Trans. IEEE, MTT-34, 1394, 1986.
43. D.C. Webb, Trans. IEEE, MAG-34, 2799, 1988.
44. H.L. Glass, Proc. IEEE, 86, 157, 1988.
45. H.L. Glass, F.S. Steams and L.R. Adkins, Proc. ICF-3 (Kyoto, Japan), 39,1980.
46. P.J.M. van der Straten and R. Metselaar, J. Cryst. Growth, 48, 114, 1980.
47. C.K. Maiti, D. Bhattacharya and N.B. Chakravarti, Trans. IEEE, CHMT-8, 221,
1985.
48. M. Abe, Y. Tamaura, Y. Goto, N. Kiramura and M. Gomi, J. App. Phy., 61,3211,
1987.
49. E.W. Babbit and R.A. Stem, Trans. IEEE, MAG-IS, 1744, 1979.
50. M. Abe, T. Itoh, Y. Tamaura, Y. Gotoh and M. Gomi, Tran. IEEE, MAG-23,
3736, 1987.
51. E.F. Schloemann, Proc. IEEE, 76, 188, 1988.
52. M.A. Truehaft and L.M. Silber, Proc. IRE, 48, 1538, 1958.
53. W.J.lnce and E. Stem, Trans. IEEE, MIT-IS, 87, 1967.
54. G. Cattarin, C.D. Gregorio, 'U. Pattrucci, F. Pucci and R. Roveda, Rev. Tee.
Selenia, 8, 29, 1982.
55. C.R. Boyd, Trans. IEEE, MTT-18, 1119, 1970.
Microwave Lithium Ferrites 163
T.R.N. Kutty
Materials Research Centre, Indian Institute of Science, Bangalore, India
S. Sundaram
Defence Electronics Research Laboratory, Hyderabad, India
1. INTRODUCTION
During the course of a wide search for the preparation of a magnetic material
of better performance than the conventional ferrites, Bertaut and Forrat [1]
found in 1956, that a mixed oxide of yttrium and ferric iron had peculiar
ferrimagnetic properties. It was found to have extremely low ferrimagnetic line
width and high saturation magnetization. In addition, it was found to be a good
insulator with comparatively very low electrical conductivity. This is an ideal
combination of properties indeed, which enables its application in magnetically
tuned devices useful throughout the microwave region.
It may be of interest to point out that such extraordinary and useful properties
were observed with the mixed oxides (Y203 and F~03) by Pauthenet (1956)
[2] while he was working for his doctorate dissertation. He found very low
magnetic line width (&I) of 5.7 Oe at 3.93 GHz for sintered mixed oxides of
iron and yttrium in the polycrystalline form. This unusual behaviour triggered
intense activity in this area during the last three decades [3-5].
On examinl;J.tion, the mixed oxide polycrystalline material was found to have
a structure identical with a garnet, in contrast to that of the spinel structure of
conventional ferrites. Garnets are a class of compounds with the general formula
X3Y2 (Z04h. In natural garnets, X will be a divalent element such as magnesium
Mg*), iron (Fe++), calcium (Ca++), manganese (Mn++), etc. Y will be invariably
aluminium (Al+++), iron (Fe+++) and chromium (Cr+++), Z is found to be silicon.
To represent the oxidation state of the component elements in such natural
garnets, they are called 2 : 3 : 4 garnets. In addition to such a combination as
is found in natural garnets, it is possible to have cations with different oxidation
states in synthetic garnets. One of the most important class of garnets containing
rare earth elements correspond to 3 : 3 : 3. All the three X, Y, Z components
will have the oxidation state of + 3 only.
Among the popular garnets, the following may be mentioned in connection
with the application to the fields of optics, radar and communication.
Single Crystal fIG and Allied Materials 165
X Y Z Formula Acronym
Y Fe+++ Fe+++ Y,Fez (Fe04h YIG
Y AI+++ AI+++ Y,All (AI04h YAG
Gd Fe+++ Fe+++ Gd,Fez (Fe04h GdIG
Gd AI+++ AI+++ Gd,AIl (AI04h GdAIG
Gd Ga+++ Ga+++ Gd,Gaz (Ga04), GOG
of magnetic memory domain devices. Such thin layer garnets have been extended
for the fabrication of a variety of surface devices.
In addition to the above practical applications, rare earth iron garnet crystals
provide basic parameters for theoretical predictions. It is possible to substitute
various metal ions (both magnetic and non-magnetic) at unambiguous sites in
the crystal and measure magnetic properties. These results could be verified
experimentally with the theoretically predicted values such as g-values, ferri-
magnetic resonance line widths and giant anisotropy. Thus, it is possible to
prepare tailor-made magnetic crystals of desired saturation magnetisation (41tMs),
compensation temperature and magnetic anisotropy.
Fig. 1. Portion of the garnet structure with cation and oxygen atoms.
There are 24 C sites in each unit cell of garnet and have the point group 222
(D~. A metal ion in a-site is surrounded by 6 oxygen ions which are at the
comers of an octahedron. There are sixteen a-sites in a unit cell which have the
local symmetry of point group 3(S6)' The 4-coordinated D ions have a distorted
tetrahedral symmetry and these (d) sites correspond to the point group 4 (S4)'
There are 24 d-sites in one unit cell. These, together with 96 h-sites occupied
by oxygen ions with triangular coordination, constitute 160 atoms of the garnet
Single Crystal fIG and Allied Materials 167
cell. We can take yttrium iron garnet as a typical example and we find individual
(Fe04) tetrahedra share comers with (Fe06) octahedra. Both these polyhedra
share edges with (YOs) dodecahedra.
This net magnetic moment of YIG shows typical Brillouin functional behaviour.
Substitution of paramagnetic or diamagnetic ions at different sites modifies the
magnetic properties of garnets. Any of the rare earth ions with an atomic number
above 61 (the rare-earth ions below samarium apparently have ionic radii too
large to fit into the garnet structure) can be substituted for yittrium. For instance,
if Gd3+ is substituted at c-sites, the term Me enters in Eq. (1). The magnetic
moment will be aligned antiparallel to the moment of the ions on the (d) sites.
It will diminish the net magnetic moment M. It is, therefore, reasonable to expect
that the saturation magnetisation 4teM. for gadolinium doped YIG will be lower
than that of pure YIG and it has been found to be so.
In addition, such doped YIG crystals are observed to show variation in the
saturation magnetisation (4teM.) with temperature. There is a temperature at
which M = 0 and this is called compensation temperature (Tcomp)' This Tcomp
shifts to higher values with increased substitution of Gd3+ for yttrium. Above
Tcomp' the contributions from c-sublattice diminishes.
Substitution of non-magnetic ions such as AI3+ at d-sites of YIG, provides a
means to regulate the shape of 4teMs vs T curves (Fig. 3).Thus, garnets with
.-..
HI
::J
to
~ 1700
VI
~
t; (a)
...
.8
to
...
N
C»
c:
f
-200 -40 120.
Temperature (e)
(b)
Tetnperatur1& (e)
•
Fig. 3. Saturation magnetization of substituted garnets: (a) Saturation magnetization
of yttrium gadolinium iron garnet (Y 3-3xGd3x) [F~] (Fe3) 0IZ; (b) Saturation
magnetization of yttrium gadolinium aluminium iron garnet (Yl.,Gdl.S) [Fez]
(F~5wAl,w) 0 12,
Single Crystal YIG and Allied Materials 169
minimum temperature coefficient for 4nMs values can be obtained by the combined
substitution at c and d-sites. It is also possible to substitute a-sites with metals
like gallium, indium and other trivalent elements. Such substitutions also will
modify the magnetic properties. With appropriate substitutions it is possible to
prepare a variety of garnet magnetic materials suitable for specific purposes. A
list of such materials reported in literature is given in Tables 1 and 2.
Material 4Me II. Ou Frequency of Minimum use- Temperatures depen- Curie temp.
(Gauss) (Oe) Ou measure- ful frequency dance of resonant ("C)
ment (GHz) (GHz) frequency (MHz/"C)
- .J
--
172 MICRowAVE MATERIALS
a b
t
Z
t4
Me!
y Y
x x
C d
Z zHa
Mo
t YIG Sphere
y y
It f
Fig. 4. Ferrimagnetic re.sonance (a) Randomly oriented magnetic dipoles in the
unmagnetized ferrite, (b) Magnetic dipoles aligned under the influence of a
magnetic field, (c) An equivalent representation of b showing the combined
effect of the aligned dipoles, (d) Precession of the net magnetization vector
due to RF magnetic excitation, (e) Equivalent representation of precessing
magnetization vector, and (f) Tuned bandpass filter consisting of YIO sphere
at center of two mutually orthogonal loops (extracted from 'Microwave Theory
and Application' Hewlett Packard Company, p. 163).
Fig. 5. Electron precession rate versus flux density (extracted from' APPLICA nON
Notes on YIO RF Components', YIO-TEK Corporation, p. 17).
Single Crystal YIG and Allied Materials 173
1640
Orthoferrite +
Liquid
1555 t 3·
iJ
~ 1520 Carnet
~ ~TPe+ U:uid
& 1480 Liquid 1469· ±2·
E 1t----~A~--------1 Ortho-
~ 1"0 I
Magnetite + Garnet
fer-ite
Garnet
20 30 40 50
V3FesO,2 VFe03
Mole .,. V203
5.1.1.1 PbO-PbFrB2~
The first flux material ever tried for growing single crystals of YIG happens
to be lead oxide, PbO. The phase diagram worked out by Nielsen and Dearborn
[5] showed that YIG is incongruently melting. The liquids region for crystal
growth tends towards the region rich in ferric oxide. It can be made out from
this that crystallization of YIG is possible only in the narrow region as shown
in" Fig. 7.
The solvent PbO has certain disadvantages because of its (a) high viscosity,
(b) high density and (c) high melting point Comparatively high temperatures
are required to dissolve the oxide, and at this temperature, lead oxide has a
tendency to decompose and get reduced to'metal and attacks platinum.
Attempts have been made to improve the perform8liCe of the above described
system by adding other compounds to the flux material, PbO. Addition of lead
fluoride (PbF~ brings down the temperature of fusion. The lowest eutectic is
found to be around 500°C. Lead fluoride will resist the reduction to give rise
to lead, and hence the flux becomes less corrosive to platinum. The density and
viscosity are also reduced considerably which improves the flow property of
Single Crystal YIG and Allied Materials 175
the molten mass. Crystals will sink to the bottom and it is possible to separate
flux more easily.
It may be pointed that lead fluoride is highly volatile under experimental
conditions. The loss due to evaporation has to be prevented to maintain the
composition and also protect the furnace from the fluoride attack. Addition of
boric oxide (or boric acid) will bring down the vapour pressure. The presence of
calcium oxide has been found to improve the size and quality of YIG crystals.
The solubility curve [15] for YIG in PbO-PbF2"B 20 3 is given in Fig. 8.
garnet+
fluxed melt
growing the crystals of YIG. Such a system has been found to be barium oxide-
boric oxide mixture. Another advantage of such a system is its comparatively
lower density. The stability region for such a system has been worked out by
previous investigators [16-18] and is shown in Fig. 9. The figure shows that
YIG has a narrow region of stability corresponding to the ratio of barium oxide
to boric oxide 3.6 to 1 (BaO : B20 3 :: 3.6 : I) and (4.55 : I).
SaO
1923'
From the study of solubilities, it has been found that the stability region for
YIG at high temperature is also narrow. YIG is stable between 1005 and
I 190°C. Above I 190°C the stable composition corresponds to YFe03 and below
l005°C, the composition corresponds to BaFe12C'19. From these considerations,
it becomes obvious, that the composition of the charge should be such that YIG
is stable over a convenient range of temperatures and the formation of other
phases is avoided.
(ii) Starting material for the preparation of lead fluoride (PhF:z) is either lead
acetate or lead nitrate (Ph (N03h> of analytically pure grade, via lead carbonate.
(iii) Boric oxide (B2~)' one of the ingredients added to improve the performance
of the flux, can be replaced by boric acid which is added to the charge and
heated slowly to the required temperature. (iv) Barium borate (BaOB 20 3)
corresponding to the composition BaO : B20 3 : : 1 : 0.6, employed as an alternate
flux material, is prepared by heating barium carbonate (BaC03) and boric acid
over a selected temperature range for several hours and cooling the molten
mass. It is also necessary to prepare barium carbonate starting from very
pure barium chloride and ammonium carbonate. (v) Calcium oxide, a minor
constituent, is obtained by heating calcium carbonate in a platinum dish to
900°C. (vi) Vanadium pentoxide, used as an oxidative additive, is prepared by
slow decomposition of ammonium vanadate. (vii) Lead peroxide is prepared
by the oxidation of Pb (II) salt, such as lead nitrate, with sodium hypochlorite
solution.
nucleation and growth at a faster rate. However, not all nuclei will grow at the
same rate. Therefore, initial rapid cooling will result in a large number of
crystals of varying dimensions of which a few will be bigger ones. After
lowering the temperature by 50°C, the furnace (Fig. 10) is reheated to near
soaking temperature (1270°C). This cycling in temperature enables the dissolution
Insulation·
Heating _-l,?-~-7''-1''''
elements
Platinum
vessel
Fluxed
melt
Crystal
Pedestal
Stand
Oxygen in
of smaller crystals leaving behind a few larger ones, which must have dissolved
only partially. The furnace is now cooled at a much slower rate (0.5-1 deg/hr).
The partially dissolved bigger crystals will now act as growth centres, thereby
restricting the development of newer nuclei. As the growth continues, the surface
area of the crystals increases. The larger amounts of constituents from the
Single Crystal YIG and Allied Materials 179
solution can get deposited on the growing crystal. This brings about a continuous
change in the supersaturation, which can be balanced by an increased cooling
rate towards the end of the processing. However, it has to be mentioned that
the optimum growth rate does not increase to high values so as to maintain
larger cooling rates. This means that the cooling rate, after the initial cycling
may be 0.5-1 deg/hr which can be increased to 3 deg/hr when the temperature
of the furnace goes down below 1100°C. However, cooling rate of 5 deg/hr or
above can still be deterrent to the quality of the crystals.
Faster cooling rates are always found to result in crystals with lot of flux
inclusion. This is due to the fact that the number of the growing nuclei will be
more at the beginning of the processing. The number keeps on increasing as
the temperature is lowered at a faster rate. These fast growing nuclei interfere
by coalescing and most probably will contain in themselves a part of the
growing medium. When the growth is complete, the crystals so produced will
have small pockets of solidified flux materials in them. Also, the fast growth
of nuclei encourages dendritic growth. When the dendrites join arms, small
amounts of flux materials get entrapped and the crystals acquire a defective
core. Therefore, slow cooling, especially at the early stages is essential.
( b)
are generally adopted. It has been mentioned in literature that the third method
results in development of strain in the crystal while being embedded in the
solidified matrix of the flux. Investigations have shown that there is no difference
Single Crystal YIG and Allied Materials 181
in the properties of crystals when method (ii) or (iii) is adopted, other parameters
being kept constant Since the third method is simpler for larger batch productions,
this procedure is generally followed.
The crystals have to be separated from the solidified flux. This is done by
leaching with dilute acids. Nitric acid is an ideal choice, since it dissolves the
solidified flux relatively faster and at the same time garnet crystals are not
attacked. The crucible is kept in boiling dilute nitric acid (3N). A charge of
about 500 g can be dissolved out by continuous boiling for two to thtee days.
In the case of procedure (i) and (ii), 2-3 hr of treatment with boiling nitric acid
(3N) removes the coating of the flux.
(3)
(1-3 mm size) even when given reasonable soaking periods (12-15 hr). Co-
precipitation of yttrium, ferric iron and lead from solutions as carbonate is
found to be an alternative method to attain easy homogeneity. Cooling rate
greatly influences crystal size as well as the number of inclusions they contain.
A continuously changing cooling rate, as shown in Fig. 12, is preferable to a
linear rate. Better crystals result by inducing nucleation at the bottom of the
crucible. This preferential nucleation can be effected by means of a stream of
oxygen projected to the bottom of the crucible. The crystals resulting from the
growth runs in which considerable PbF2 has evaporated are found to be smaller
in size with more inclusions. The size and yield of crystals have increased. The
inclusions also come down with the addition of PbF2 to PbO.
1200
r
T ·C ,..., 1.5"/hr
C;')
1100 ~.
1\"
(")
~
<oj
'""' 2.0·/hr
iii
-::s
C)
1000
~
~
End of the
growth rJ.? [
~
o 20 60 100 140 180 220 260 300 ~
TIME (Hours)- is'
t:;
Fig. 12. A typical cooling curve.
00
Vl
-
184 MICRowAVE MATERIALS
directly taken, the mole ratio of Y2~ and F~~ is kept close to 3:5. 75% of
the available volume inside the liner is filled 'with sodium hydroxide solution.
The seed crystals used are those obtained from the flux experiments. The baffle
opening is maintained around five percent. The space between the liner and the
autoclave is filled with distilled water (65-70% fill). Since sodium hydroxide
solution has lower pressure than that of pure water, lower percentage fill is
adequate to balance the pressure developed inside the liner.
The autoclave is assembled as shown in Fig. 13. It is closed with the cap,
followed by torquing the tightening screws. It is positioned in the furnace and
12
11
heated to 4000C. The temperature gradient is adjusted such that the bottom
temperature is 400°C, while the top thermocouple reads 380°C (temperature
gradient, liT - 20°C. The pressure within the liner is around 600 atm, while
outside the liner it is more then this value. The pressure vessel is maintained
for over 15 days, ltt the end of which the autoclave is cooled to room temperature
and the crystals mcovered. Growth of crystals is rather slow in the case of YIG
Single Crystal fIG and Allied Materials 185
from 20 wt % sodium hydroxide. The average growth rate is less than 5 mils
per day. The growth rate increases with larger temperature gradient, but coherent
and uniform growth is obtained with tJ.T - 20°C.
YIG crystals grown by the hydrothermal method have minimum Fe2+ iron
content (invariably less than 0.02 atoms per formula unit). However the greatest
drawback is the presence of (OH) groups incorporated in the crystal. Infrared
spectra of hydrothermally grown YIG crystals show a broad band in the region
of 2800--3650 cm- t • This broad absorption is invariably absent for the flux-
grown specimens. Presence of (OR) group broadens the ferrimagnetic resonance
Iinewidth of the material. Therefore, its reduction is of. considerable importance.
It has been suggested that potassium hydroxide, though more corrosive, is a
better mineraliser [20]. The addition of calcium is also said to reduce the (OH)
content.
density which for good quality GOO is less than 5 per cm-I . Film thickness can
be held within 10% across 90% of the substrate area, with no detectable
composition variations or second phases. Films can be grown at growth rates
of 0.1 pm/min to more than 3 pm/min and to thickness of greater than 100 pm.
Epitaxial films of YIG have been grown by Adam et al [22] on GGG by
L.P.E. from a Y2~ (1.4 g) - F~~ (11.82 g) - B20 3 (4.04 g)-PbO (182.74 g)
flux. The following details have been reported by them. The growth technique
used horizontal dipping with axial rotation. The 200 g melt was contained in a
platinum crucible, and has a saturation temperature of 920°C. The 1.5 cm diameter
substrate was held by a platinum vacuum chuck, and was rotated at 100 rev/min
during growth and at 1000 rev/min, immediately after removal from the melt.
Using this technique, films of up to 100 pm thickness were grown at a rate of
approximately 2 pm/min at 900°C. The versatility of the L.P.E. system allows
the addition of rare earth ions or diamagnetic ions such as Ga3+.
6.2 Density
The gross density of YIG crystals is used as a rough measure of the extent of
inclusions present. The measured density can be compared with X-ray density.
Gross difference between these values indicates the presence of other phases
e.g; orthoferrite (YF~). Density of the crystals is measured by the displacement
method using specific gravity botfle. This involves the determination of the
Single Crystal fIG and Allied Materials 187
12.39
.......
......
~
12.34
purity of them. The important absorption bands for YIG is around 600 and
380 cm-I . The band around 600 cm-I can be tentatively assigned to asymmetric
stretching modes of (Fe04) tetrahedra and has the first overtones around
1150 cm-I [27]. However, it is more complex in the sense that lattice modes also
influences these absorption bands. The important point to be mentioned is that
infrared spectrum serves to detect the silicon impurities. As mentioned earlier,
silicon impurity cannot be completely eliminated. Since rare earth iron garnets
and natural silicate garnets are isomorphous, the silicon will be incorporated in
iron garnets as Si04 tetrahedra. In Fig. 15, the characteristic absorption spectrum
of a silicate garnet is compared with those of two YIG samples: (1) containing
c21
~
..
Oil
c
~
~ ;!
"
.
==
Oil
c
!
....
;!
2N nitric acid and then evaporated to near dryness. The residue is boiled with
water when all the salts excepting PbS04 dissolve. PbS04 formed is estimated
gravimetrically. The amount of lead present is directly proportional to flux
inclusion. The lead content has been found to be minimum « 0.15%) in well-
grown crystals. However, the percentage of lead is higher in those crystals
grown with a faster cooling rate, reaching upto 1.3%.
From the filtrate of the above experiment, yttrium and iron are determined.
=
High quality crystals gave the analysis Y2~ 43.92 and F~~ 55.89% =
= =
(calculated values for YIG are YA 44.08 and F~~ 55.92%). The analytical
data, again, confIrm the phase identity.
Ferrous iron in YIG is estimated by the vanadate method. For this purpose,
the single crystals are crushed and powdered to - 400 mesh in an agate mortar
under acetone. This method is normally adopted to prevent oxidation during
grinding. A known weight of the dry powder is treated with 10 ml standard
ammonium vanadate solution and 5 ml concentrated sulphuric acid. The solution
is kept at near boiling point on a sand-bath with minimum evaporation. After
about 2 hr, the solution is cooled, diluted with 4N H2S04 and titrated against
standard ferrous ammonium sulphate solution. The difference between direct
and the test titration values is proportional to the reducing capacity-which is
due to Fe2+ content in the sample. The duration of the experiment can be
reduced using a pressure vessel at 150°C. The well grown crystals with low Si
content have FeO content < 0.28%. This value increases for products from
crystal growth runs where oxidizing additive has not been added. FeO content
increases to 1.5% in some cases. The lowest FeO content (0.025 atom per
formula unit of YIG) observed corresponds to experiments in which V20S is
added to the charge. It has been found that Fe2+ content increases when Si is
intentionally added. It may be mentioned that Si-doped YIG has giant anisotropic
properties.
(iv) various force methods and (v) microwave methods. The Curie temperature
can be determined from the plot of 41tM. vs temperature. There are three
practicable ways of estimating 4trM. by microwave technique. Measurement of
the shift in the ferrimagnetic resonance field for a non-spherical specimen [30],
observation of magnetostatic modes [31] which is applicable to narrow line
width single crystals and study of magnetostatic cavity modes in the bulk
materials.
Saturation magnetisation (4trM.) can also be determined by measuring the
mass susceptibility of powdered YIG crystal at a field strength of 10,000 Oe
(around 290 x 10-6 cgs units/g). At this field, magnetisation saturation is achieved
and the M values correspond to M.aturalion • The 4trM. is related to the mass
susceptibility in the following way.
B =H + 4trM. (4)
B =H + 4tr",d . H (5)
Therefore. 4trM. =4tr",d . H (6)
where '" = mass susceptibility, d = density, H = field strength and B = magnetic
permeability
The 41tM. calculated in this manner is around 1750 Oe [32].
Perspex
when emery paper of 1/0 and 2/0 grit size are used. Strict control of the
grinding time is necessary at this stage, to control the size. The size of the
sphere is checked at 1/2 hour intervals at 1/0 and 2/0 stages. With 3/0 and
4/0 emery, the surface acquires higher polish and air pressure is reduced to
5-10 psi. After the use of 4/0 emery, the spheres will be shining in reflected light.
The spheres are further polished with diamond paste of finer grit size in
steps of 2-4, 0-2 and 0-1/2 J.I.M grit. These abrasive compounds are first applied
to a soft carrier medium like wood, hard variety of paper or canvas cloth. The
diamond particles get embedded in the medium. The wall of the air cyclone
cavity is lined with this abrasive carrier.
Final polishing is carried out by a mechanochemical method using a suspension
of colloidal silica « 0.05 J.I.M grit) in 2 N KOH. This polishing mixture is
available in the trade name "Syton". The slurry is placed on a pelion polishing
pad and spheres are polished in it by simultaneous pressing and rolling for
6-10 hr. The finish of the surface is checked by viewing under reflecting
microscope (magnification, 50), whereby no scratches or pits should be seen.
6
10
Ds in mills
SPHERE DIA IN MILLS
Fig. 17. Carter's chart of Qc vs sphere dia for a spherical YIG resonator.
Thus, for a spherical resonator which is easier to prepare with precision, the
resonant frequency is independent of saturation magnetization and linearly
dependent only on biasing field Ho. In any other shape for the resonator, for
= = =
example, thin disc in the XY plane where NJ. Ny 0 and N z 1, the resonant
frequency
10 =2.8 (Ho - 4nM,) (10)
In this case, resonant frequency is influenced by saturation.
Non-uniform coupling between the rf field and the precessing magnetic dipoles
occur below this frequency, giving rise to non-linear behaviour and increases
in losses. At frequencies lower than (1/2)!c, resonance cannot occur as it is not
possible to achieve magnetic saturation in the YIG resonator.
Also, resonator operation at temperatures close to or above the Curie tempe-
rature Te, of the material is not possible as the 4nM. drops to zero at Te.
power level limitations, YIG tuned devices are restricted to low power
applications.
Ho =-2.8
10 - [2 - -5·
sm 8 - -15·
28M.
sm 2 8 ] -Kl (15)
where 8 is the angle between Ho and that 01(100) axis which becomes parallel
to Ho, as the sphare is rotated about the (110) axis. Thus, when the sphere is
oriented at the ± 270 points,
Ho = {~ MHz (16)
8.1 RF Tuners
A typical RF tunci comprises of a YIG tuned filter-oscillator combination driven
by suitable electronic drivers with associated isolators and a mixer preamplifier
IF filter combination. The operation is based on the 'superhet' principle wherein
the input RF signal selected by the YIG filters is down converted to an IF
signal for further processing. A signal command enables both the filter and
oscillator to be driven to appropriate frequencies, with a fixed IF frequency
off-set, throughout the tuning range of the tuner. An instantaneous bandwidth
of about 20 MHz over a large dynamic range and linear tunability over octaves
or multioctave frequencies has made these YIG tuners vital and critical
components for ECM receivers.
8.4 Staloc
To overcome mistracking problems due to frequency drift limitations. c1osed-
loop' operation of the octave and multioctave filters have been developed using
a unique tracking technique called "STALOC" (Self-tracking Automatic Lock-
on Circuit). These filters. automatically lock on and track a CW reference
frequency at a predetermined offset frequency. These filters find applications
in active ECM and jammer set-on receivers.
Magretic Field Ho
Dielectric
substrate
Ground Plane
l:' X
REFERENCES
1. F. Bertaut and F. Forrat, Compt. Rend. Acad. Sci., 242, 382 (1956).
2. G. Pauthenet, Doctorate Dissertation, University of Paris (1956).
3. S. Geller and M.A. Gilleo, Acta. Cryst., 10,239 (1951).
4. W.H. Grodkiewicz, E.F. Dearborn and L.G. Van Uitert, Cryst. Growth, Ed.
H.S. Peiser, Pergaman Press, N.Y., 1961, p. 441.
5. 1.W. Nielsen and E.F. Dearborn, 1. Phys. Chern. Solids,S, 202 (1958).
6. G.P. Rodrigue "Magnetic materials for millimeter wave applications" IEEE
Transactions on magnetics., Sept. 1963, pp. 351-356.
1. G. Winkler and H. Dotsch, 'Hexagonal Ferrites at Millimeter wave length'
Proceedings of the 9th European Microwave Conference, 1919, pp. 13-22.
8. P. Roschmann, M-Lernke, W. Tolksdorf and F. Welz 'Aristotropy field and
FMC linewidth in single crystal AI, Ga, and Sc substituted Hexagonal ferrites
with M structure. Materials Research Bulletin. 19, 1984, pp. 385-392.
9. W.H. Van Aulock, "Handbook of Microwave Ferrite Materials", Academic
Press, N.Y. (1965).
10. 1. Helszajn, "Principles of Microwave Ferrite Engineering", Wiley-Interscience,
N.Y. (1969).
11. E.A. Giess, B.E. Argyle, D.C. Cronemeyer; E. Klokholm, T.R. McGuire, D.F.
O'kane, T.S. Plasketl and V. Sadagopan, AlP Conference Proceedings Series
NO.5 (17th conference on Magnetism and Magnetic Materials, Chicago (1911).
12. S. Standley, "Oxide Magnetic Materials", Oxford University Press (1969).
13. F.F.Y. Wang in Treatise on Material Science and Technology, Vol. 2., Academic
Press, N.Y. (1973), pp. 213-387.
14. H.1. Van Hook, 1. Amer. Ceram. Soc., 44., 208 (1961).
15. W. Tolkdorf, Acta Electronica, 17,57 (1914).
16. R.A. Laudise, in 'Art and Science of Growing Crystals' Ed. J.J. Gilman, Wiley
Intcrscicnce, N.Y. (1963).
17. R.C. Linares, J. Applied Physics, j~, 433 (1964).
18. M.1. Kestigian, 1. Am. Cram. Soc., 50, 165 (1961).
19. R.A. Laudise and E.D. Kolb, J. Amer, Ceram. Soc., 45, 51 (1962).
20. E.D. Kolb, D.L. Wood, E.G. Spencer and R.A. Laudise, J. Appl. Phys., 38,
1021 (1961).
21. J.E. Pullian, G.R. Archer 1.L. and Besser P.1. 'Magnetic Oxide films' IEEE
Trans on Magnetics MAG-5, pp. 111-21, 1969.
22. 1.0. Adam, Prof. 1.H. Collins and J.M. Owens 'Microwave device application
of epitaxial magnetic garnets'. The Radio and Electronics Engineer Vol. 45,
No. 12, pp. 138-148, Dec. 1915.
23. A.B. Chase and J.A. Osmer, Jour. Cryst. Growth,S, 239 (1969).
24. V.N. Vertoprakhon, V.D. Zamozhskii and P.V. Klertosv, Sov. Phys. Crystalogr.,
13, 113 (1968).
25. S. Geller, G.P. Espinosa and P.B. Grandall, 1. Appl. Cryst., 2, 86 (1969).
26. W.1. Cruft, Amer. MinLTal, 50, 1634 (1965).
27. B. Cockayne, 1. Amer, Ceram. Soc., 49, 204 (1966).
28. K.A. Wickersheim, R.A. Lefever and B.M. Hanking, 1. Chcmp. Phys., 32, 211
(1960).
29. Measurement of the properties of ferrite materials Miss Sp. Maxwell. The Marconi
Review First Quarter 1910, pp. 2-11.
30. C. Kittel; Phys. Review 13, p. ISS, 1948.
31. M. Magid. IEEE Trans., IM-I3-p. 329, 1964.
Single Crystal fIG and Allied Materials 199
32. G.R. Harrison and L.R. Hodges (Jr.), J. Appl. Phys. 33, 1375 (1962).
33. W.L. Bond, Rev. Sci. Instr., 22, 344 (1951).
34. J.W. Jeffery, "Methods in X-ray crystallography", Academic Press (1971).
35. M. Sparks, "Ferromagnetic relaxation theory", McGraw-Hill, N.Y. (1964).
36. A.H. Harrish, "The physical principles in magnetism", Wiley, N.Y. (1965).
37. Lax and Hutton, Microwave Ferrite and Ferrimagnetics, N.Y., McGraw-Hill
1962.
38. Mathaii, Magnetically tunable band stop filters' IEEE transactions on Microwave
theory and Techniques. Vol. MTT-13, pp, 203-212, March 1965.
39. Hexagonal Ferrites for Millimeter Wave Application, D.B. Nicholson, Hewlett-
'Packard Journal, 41, Oct 1990, pp. 59-67.
40. Microwave Magnetics and SAW Devices RADC Electromagnetics Sciences
Division, Microwave Journal, Apri11979, pp. 20-21.
41. D.B. Nicholson, R.J. Matreci and M.J. Levernier, 26.5 to 75 GHz, Preselected
mixers based on magnetically tunable barium ferrite filters, Hewlett-Packard
Jour., 41, OcL 1990,49-58.
8
Radome Materials
a.s. Mani
Institute of Annament Technology
Defence Research and Development Organisation
Ministry of Defence. Pune. India
1. INTRODUCTION
1.1 Definition
According to IEEE radome is defined as "an enclosure for protecting an antenna
from normal effects of its physical environment, generally intended to leave
the electrical performance of the antenna unaffected" [1]. In simple terms, a
radome is a housing for an antenna. Because of the reason that radome is
essentially a protective device, it is required to provide necessary structural
strength, but yet, not deteriorate the electromagnetic performance of the antenna
under operational conditions.
I I
-II-
A/20
--\ t--
12
I
--+l f--
nA/2
m~ m
Fig. 1. Commonly used radome wall configurations.
rings or patches have been used to reduce abberations due to antenna scanning
within the radome [15].
Apart from the above wall configurations, which were essentially made of
dielectric materials, other wall configurations have also been reported. These
are the metal space frame radomes capable of quick assembly at site for ground
applications [16] and perforated metal radome for missile applications. The
latter is reported to have better rain erosion resistance, high strength to weight
ratio and low static charge build-up [17].
I
~ ~
SELECT
Primary materials. Relax
Wall struc. ture. specs
Fabrication techniques
STUDY
i) Better
IEvalUate structure I Relax
materials
fo- materials
ii)Wall
Not ok
I I
Over design
specs
structure
Ok
I
Evaluate
VARY Bectrical performance I
I
1 Materials
I-- 11 Wall shape
mAntenna Not ok
interaction Ok
I Manufacture prototype
I
!
I ~
Electrical
te~ts
lOther
tests
Not ok
I a< I Ok[ Not ok
!
Output
of different variables are then used to fabricate prototype which is then refined
for further optimisation.
Electrical performance of the radome largely depends on range of incident
angles, which the electromagnetic waves make with the radome wall. In addition,
polarization of the antenna enclosed in the radome and the electrical characteristics
namely dielectric constant and loss tangent of the material decide the electrical
performance of the radome.
Radome Materials 205
Radome shape and location of the antenna relative to the radome dictate the
range of incident angles. In the case of ground based or ship-borne radomes,
the shape can be chosen on the basis of optimum electrical performance. In
case of airborne radomes, it is generally optimised on the basis of aerodynamic
considerations. Since shape is an important electrical factor in radome design,
it has been found to be convenient to classify radomes on this basis. A normal-
incidence radome is identified as the one in which most of the area illuminated
by the antenna is approximately normal to the radiated beam of antenna. The
transmission properties in such case can be approximated by those exhibited by
plane dielectric sheets traversed by plane waves normal to the surface. A large
spherical radome, in which the antenna is located at the centre of the sphere
will yield performance of an ideal normal-incidence radome. Streamlined radomes,
as the name implies, have large fineness ratio (ratio of length to base). Some
of the practical shapes used for airborne radome designs are shown in Fig. 4 [3].
t----------A----------t
2. RADOME MATERIALS
8=4
12.5
FREQ 9375MHz I
I
: 120'10.1.
1
I
I
I I I
elO 20",.1.
I I
I
E ~----,/~--------~ 75 I
fJ)
fJ)
10",_ ~eI/ I
I
'"z 10',• .I.
I
I
I
'"
!.! I
...
:J:
I
I
I I ,
-' I I 1201•
-' I I lIel
; 7.5 I 10'101 \
I 5.0 lIell \
I 20'10.1.
I
I PARALLEL POLARISATION------
I PER P£NDICULAR
/10'" lI el
5.0·~--'-;;----TO---'-;;---T:"""--'
0' 2c1 40' O' 10' 20' 30' 4r! 5r! 6r! 7r! 80" 9
ANGLES OF INCIIENCE - ANGLES a= INCIDENCE-
(a) Monolithic AJ2 wall (b) A-Sandwich wall
snow and hails must also be considered. Shock, vibration and acceleration
levels may form some of the other considerations in selection of materials for
the radome.
Radomes are expected to have large electromagnetic transmission coefficient.
However, this performance may get drastically affected by any moisture absorbed
by the materials forming the radome wall. Dielectric properties of the water
vary in the region 80 to 40 over the frequency region of 1 to 20 GHz. The loss
tangent in the same frequency region vary from about 0.06 to 0.9. Hence, any
possibility of absorption of moisture in the radome wall structure must be
totally avoided. Apart from selecting the materials impervious to absorption of
moisture, it will be advisable to treat the surface of the radome so that rain
water does not stick to surface. If the thickness of water layer over the radome
is comparable to wavelength of electromagnetic radiation, the loss will no
more be negligible. From practical data collected on ground based radomes,
'?adome Materials 209
CORE THICKNESS
lmm / 2mm \
-4~4
//
CORE
/ / /
SKINS OF f=4
CORE OF E = 1.15
100
t 10",1
f 75
oil
~
-"
:5"
l"
o
u
50
Parallel polartsatoon
Pl!rpenchcular
I ! I I I I I
0' 10' 20' 30' 40' 50' &0' 70' 80' 90'
Angles of Incidence _
--
/ V V -/
d0Jr
400'c
~' I. ~ ~
.-
/ i11r- -
o 2 3
Free stream mach number_
2.2 Composites
Most of the materials used for radome fall under the category of composite
materials. A working definition of composite materials can be "a material
system composed of mixture of combination of two or more macro constituents
RadomeMaterials 211
differing in form and/or material composition and that are essentially insoluble
in each other" [19].
In principle, composites can be constructed of any combination of two or
more materials. But typical composites are those in which a structura1 constituent
called reinforcement is embedded in a matrix. Because the different constituents
are intermixed, there is always a contiguous region. It may simply be an interface
i.e., a common boundary of the constituents, or a distinct added phase called
an interphase. When such interphase is present, there are two interfaces, one
between each surface of the interphase and its adjoining constituent as shown
in Fig. 9. By suitable combination of the constituents, the composite material
can be designed to have the right combination of desired properties. These
properties may be related to structural strength, temperature characteristics or
the electrical parameters.
INTERPHASE
(BONDING AGENT
FIBER
~J~==+-INTERFACE
The high strength to weight ratio and the capability of tailoring the mechanical
and electrical properties of the composites m~e them very attractive for
fabrication of radomes. The constituents of the composites are selected based
on the required radome characteristics. Since the radome is required to be
electromagnetically transparent, the electrical conductivity of both the
reinforcement and the matrix selected for the composite have to be extremely
low. In addition they must provide the necessary stiffness to the final composite
structure.
considerably higher strength than same type of fiber that has been drawn as a
strand, sized, and woven on a reel and stored for some period. Also characteristics
such as resistivity may depend very much on extraneous factors such as water
content, surface treabnent etc. E-glass is a low alkali composition glass primarily
for electrical applications. It has 52-56% of Si02, 12-16% of Al20 3 and
16-25% ofCaO. MgO and B20 3 vary from 0-6% to 8-13%. S-Glass is a high
tensile strength glass which has significant strength to weight ratio, superior
strength retention at elevated temperature and high fatigue limit. Typical
composition of S-glass is 65% Si02 , 25~ Al20 3 and 10% MgO.
D-glass is an improved dielectric glass developed for high performance
radome application. The dielectric constant of D-glass is around 4.0, compared
to 6.11 for E-glass and 5.2 for S-glass. The loss tangent is also 0.003, compared
to 0.006 for E-glass and 0.007 for S-glass. However, it has lower strength and
substantially lower Young's modulus.
Basic raw material for glass fiber is pure molten glass which is extruded
through a bushing containing large number of holes. The emergent ends of
glass are drawn and sized. Sizing is a process wherein a material is applied on
its surface to fill pores and to modify the surface properties to improve adhesion.
The range of fiber diameter commonly produced vary from 0.003 to 0.02 mm.
Sometimes, conductive additives are added to the fiber to avoid electrostatic
charge build-up. Such additives will deteriorate the performance of radomes.
As reinforcements, glass fibers can be used in the form of rovings, chopped
strands, mats, fabrics and woven rovings.
Aramide fibers under the trade mark of Kevlar is marketed by E.I. Du Pont.
It is an organic compound of carbon, hydrogen, oxygen and nitrogen. The
relative mechanical properties of Kevlar and other reinforcements generally
used in composites is shown in Fig. 10. Kevlar 29 is a low density, high
strength aramide fiber useful for ballistic protection. Kevlar 49 is characterised
by low density, and high tensile strength and modulus. Kevlar 49 is useful in
fabrication of high performance composite applications where light weight,
high strength and stiffness are important. It can also resist shattering upon
impact and inhibit propagation of cracks. Its stress-strain behaviour is linear
upto ultimate failure in tension at 2344 MPa and 1.8% elongation. Its specific
Radome Materials 213
5 15
KEVLAR 29 KEVLAR49
• •
.6
"'0 10 :5
RESIN IMI'REGNATED STRANDS
20
•
S.GLASS
•
HTGRAPHITE
E
15 ",u
•
BORON ~
OTHER ORGANICS
HM GfW'Hrrl' 10
• E GLASS
• STEEL
5
• ALUMINUM
2 3 4 5 6 7
SPECf'lC TENSILE MODUWS.106 in
laminating upto 100 lb/sq in. requiring cure at 350 OF. The maximum usable
temperature can be upto 420 of under intermittent conditions. However, it is
felt that there is some degradation of properties after long time exposure to
humidity which limits the service temperature to about 275 of. Epoxy resins
are preferred in many applications due to versatility in terms of pot life, curing
conditions, viscosity etc. They are used in filament wound radomes and also
in sandwich constructions.
Polyimides and polybenzimidazoles are useful for high temperature
applications. They have excellent mechanical and electrical properties over
wide temperatures and can be used in applications requiring long term exposure
over elevated temperatures. For high temperature applications condensation-
type polyimides are useful. These resins are however difficult to process and
are also costlier than other types by about 5 to 20 times. Polyimide laminates
can become water absorbent unless properly sealed.
Generally, the fiber strength and stiffness greatly exceeds matrix strength
and stiffness. Hence, longitudinal mechanical properties are almost entirely
governed by the fibers. Compressive strength in the fiber direction is less than
the tensile strength, particularly if the fibers are thin or not very straight. For
glass reinforcements, the compressive strength may vary from 50 to 75% of the
tensile strength. For plastic reinforced with aromatic fibers, however, compressive
strength is generally 20 to 25% of tensile strength, due to low compressive
strength of the fiber itself.
As regards longitudinal thermal expansion coefficient, the phase with higher
modulus tends to impose its expansion coefficient on the final composite property.
It can be approximated as [22]
Strength changes due to causes such as water pick-up will also be governed by
similar equation.
The transverse properties are generally governed by the properties of the
matrix phase. The transverse strength is mostly lower than that of matrix, being
about 50%, but the nature of the fiber matrix interface is particularly important
here. Transverse Young's modulus, transverse conductivity and pennittivity
are also dependent on fiber-volume fraction. The transverse thennal expansion
can be approximated by
fibers, aspect ratio of fiber bundle is more important. Strength and stiffness of
such materials are generally not impressive.
I~ ~UNIDIRECTIONAl
IJIIII~
I~I~IL--- EHJ3
I I I1 I±lli
BI DIRECTIONAL
,~i~ ~ PSEUlXJ"'lllOPK:
For a balanced crossply wherein the two sets of fibers are orthogonal to
each other, the Young's mudulus in X and Y directions are equal and has
approximately the average value of the unidirectional composite in the two
directions. However, it has low Young's modulus in the + 45° and - 45°
directions. A laminate with plies in 0°, + 60° and - 60° has nearly the same
Young's modulus in every direction. Same is true for electrical characteristics
such as permittivity or conductivity in different directions of laminates.
A. Solid wall
1. Halfwave 1 2 3 3 4
2. Thin-wall 1 1 3 1 4
B. Multilayer
1. A-Sandwich 1 3 3 3 4 2
2. C-Sandwich 1 3 3 3 4 3
3. Multilayer 1 3 3 4 4 4
1: Most widely used; 2: Frequently used (dictated by type of materials); 3: Little used
(dictated by specialised requirements); 4: Not applicable.
Matched die moulding uses a pair of dies. Fabrication of these dies and their
alignment is an important step, since final dimension and finish depend on
these dies. Matched die moulding can give accurate and repeatable products of
high strength and electrical homogeneity. The technique involves high initial
cost outlay in terms of tools and dies. Modification of moulding tools to change
radome shape or thickness is difficult and expensive. Matched die moulding
technique is suitable for fabrication of radomes based on foam-in-place core or
sharply curved thick honeycomb.
In vacuum bag moulding process, dry glass fabric is wetted with resin and
laid on male mould. A plastic film bag is placed over the lay-up and after proper
sealing, the space between lay-up and plastic bag is evacuated by connecting
to a vacuum source. Atmospheric pressure is utilised in moulding the required
part. Generally the required thickness is built up by laying a number of layers
of reinforcing fabric. It is important to use resin with proper viscosity, so that
the resin and air can be easily squeezed from the lay up. This is a low cost
technique but getting uniform resin content over complete surface requires
skill and practice. This technique is useful only for radomes which are not
subjected to high stresses.
Principle used in autoclave technique is similar to vacuum bag moulding but
it uses much greater pressures. Also the moulding can be carried out under
elevated temperature condition depending on resin requirement. Special autoclave
equipment needs heavy capital investment. Preimpregnated cloth called prepregs
can be used in this technique and can give accurate, repeatable products with
consistent performance.
Sandwich C onstrucflon
from 3/16" to 1/2" with densities ranging from 2 to 10 lb/cft. The core to skin
adhesive rigidly joins the sandwich components and allows the complete unit
to act as single entity with high torsional rigidity. The rigidity obtained by the
sandwich construction can be understood by comparing it with an I-beam. The
facings of sandwich panel acts as flanges -and the core as the web of the 1-
beam. While loading on one of the facings is in th6 compression, the other is
in tension. The core resists the shear load and increases the stiffness of the
structure. In comparison to the web of I-beam, the honeycomb core gives
<;ontinuous support of the facings. Fig. 14 shows the comparison of sandwich
structures with normal monolithic structures.
.E
Monolithic Wall Sand wich Wa ll
1.
I 1+ 1 1 1 1 11 1111 1 1 1~t
1
Relative StiH ness(D) 100 700 3700
Relative Strength 100 350 '25
Relative Weight 100 103 10&
Glass fabrics, Nomex paper and Kevlar are some of the materials used for
honeycomb core in radome applications. Dielectric constant of different types
of honeycomb as a function of density is shown in Fig. 15. Apart from normal
standard hexagonal cells, over-expanded and flexible cell honeycombs shown
in Fig. 16 are useful in fabricating intricately shaped radome structures. The
220 MICROWAVE MATERIALS
- - Prirotlel polarization
- - - - Perpendicular polarizaf
c .........
.EVI .......... ... .....
u
6 1.12
... .....
-
.!rl
~
L..
Gi 1.08 .._..
0
t04
Hexagonal cor.. ""II Over Expandt!d cor.. c...11 FI ..xible cor ... ""II
.....~ 100
----.
" ~"
0
I-
Cl.I
a.~ 80
~ -
....... c
0
E .~ 60
o
....e
I::.
using honeycomb cores is the need to properly bond the core to the skins. In
order to achieve a good attachment, the adhesive must have the upique qualities
of surface wetting and controlled flow during early stages of cure. This controlled
flow prevents the adhesive from flowing down the cell wall and leaving a low
strength top skin attachment. Adequate attention must also be paid for closing
the sandwich structure at the edges, to avoid moisture pickup through these edges.
Transfer of heat through a sandwich panel is dependent upon the basic
principles of convection, conduction and radiation. Non-metallic honeycomb
cores used for radomes minimise heat flow from the outer skin. When the
structure is to act also as a heat shield, flow of heat can further be reduced by
filling the cells, so that convection within the cells can be eliminated. Special
foams are sometimes used, where possible water accumulation in the cells due
to skin damage must be prevented.
30~------------------------~
I /compressive
I' 1.25
Dielettrif
constan
-
1.20
c:
1.15 gVI
£ c:
2' 0
u
-
CII
u
!;
III
10 1.10 'i:
~
'ii
1.05 C
the electrical efficiency [27]. Both additive and condensation polymides can be
used in conjunction with syntactic foam to build high performance radomes.
Unpublished reports have shown good phase characteristics for radomes built
using syntactic foam.
RADOME
SIGNAL GUIDANCE
RECEIVER t - -...... PROCESSO
ANSMI
POWER PRIME FOWER
SUPPLY
head. The output is the guidance data which is fed to the autopilot for guiding
the missile path.
Sensor antenna and radome form an important subsystem of the missile
seeker. Compared to the microwave antenna, millimetric wave sensors offer
better resolution and adverse weather capacity. Millimetric wave sensors are
also being considered for re-entry interceptors for exo-atmospheric operations.
Seekers operating on radiometric principle require wider rf bandwidth sensors.
For better target discrimination, multi-mode seekers are used where information
from more than one sensor is used for guidance. In all cases, radome design
must be compatible with sensors.
Seekers employing common aperture for dual mode sensors present many
challenges in radome design. In such cases, the radome design will be required
to be optimised at several wavelengths which may be widely separated.
2.6.3 Materials
Conventional resin glass composites can be used only for low speed missiles,
which do not demand operation in high temperatures. For speeds of the order
of Mach 3 or above, it is necessary to use inorganic materials based on silicon,
glass, or ceramics. Apart from capability to withstand high temperature without
deterioration in performance, these materials can be designed to provide adequate
12
11
10
..... 9
c
E
VI
c
0
u 8
U
.....
L..
u
.!! 7
Q.I
0
Pyroceram 9606
6
Raycerom III
5
3
0 SOO 1000 1500 2000 2500
Temperature
0.010
..... 0.008
c
f
VI
VI
0.006
0.004
0
...J 0.002
0
0 500 1000 1S00 2000 2500
Temperature
Fig. 20. Electrical characteristics of some inorganic materials.
226 MICROWAVE MATERIALS
of alumina is about 9.6, that of glass ceramic is 5.65. Hence for halfwave
design, physical thickness of glass ceramic radomes is larger than of alumina.
Due to increased physical thickness, its mechanical properties are adequate in
most cases, even though some of the mechanical strength characteristics of
glass ceramic materials are poorer. Also, though density of glass ceramic is
less, it has only marginal weight advantage over similar alumina design. Both
materials being hard, can withstand rain erosior) and thermal shocks well. For
alumina, thermal differentials in excess of 400°C can result in failure. Above
500°C, mechanical strength of pyroceram deteriorates more drastically than of
alumina. In its pure form, permittivity of alumina increases from 9.6 at room
temperature to 11.4 at lOOO°C. By adding titanate, it can remain nearly constant
at about 11.6 over complete temperature range.
required for these low density material to provide resistance to water absorption
and to sand/rain erosion. The loss tangent can generally be kept less than 0.005
in all cases. It is observed that variations in dielectric constant with temperature
in silicon nitride are intrinsic in nature and little improvement can be achieved
by process variation. On the other hand, the loss is predominantly controlled
by intergranular phases and impurities. Monolithic radomes using reaction bonded
silicon nitride can be used for narrow band applications.
By having a two layer structure of low or medium density silicon nitride
core as a thickbase, with a thin skin of higher density silicon nitride, it is
possible to achieve acceptable radome performance over a wide range of
frequencies. The high density outer skin can provide erosion resistance and can
also form a suitable base for moisture sealent.
Chemical vapour deposited silicon nitride (CVDSN) has the ~ntial as a
multiple frequency window material and can be used in conjunction with sensors
operating at different wavelengths.
and Lexan are other thermoplastics which can be used in the form of thin flat
sheets or in the contour conforming to the platform. The dielectric constant of
Teflon is so low, that larger thickness of protective cover can be used compared
to glass laminates. It can be used even at subsonic speeds, if certain amount of
erosion can be tolerated.
20".
POLARISATION: PERPENDICULAR
DIELECTRIC CONST .4.0
z
o
;::
til
...
...J
.u
a:
a:
IIJ
3: 10 .,.
~
o~~~-----===t==---------L---------~~~
o 0.25 0.50 0.75
ERROR IN THICKNESS (mm)_
flying at supersonic speeds in heavy rain are subjected to erosion, and subsequent
poor electrical performance. A change of the order of 0.005" is not unreasonable
for a neoprene coated radome. In such cases, power reflection coefficient of
5% at X-band and upto 20% at Q band for 80° radome can be expected. Periodic
maintenance with recoating is the possible solution for overcoming this.
80
t 70
....
~
:... 60
z
Q
~ 50
~
11)
z 40
c(
a: a:
to- L!J
ffi 30 ~ 60
~
~
2 20~~ ______~______~_____
8.400 8.775 9.150 8.400 8.775 8.1S(
FREQUENCY(GHz) --....,..
~ FREQUENCY(GHz)-
~
~
ffi 150 :z:
t; 6
a::
>- z
<f'J w
W 100 a::
2: >-
<f'J
<f'J
lfl<f'J
IF.
w
g: 50
T300/976
2r ~~;;:'io DATA
~
o O~_-,--I_-l-_~
u
Ol:----:!--~----,J.
o 5 10 15
o 5 10 15 VOid Content (0'0)
Void Content (0/0}
~ 8,---------,
..,
.l<
!2 6
><
34-
::;)
c
~ 21-
mO'-----.JI'--___,JI_~
VI
o 5 10 15
Void Content ('/,)
15.----------.
\ T 300/976
b 2.4psio "t:J
C
.8
~ ~
::!
It..
10 ~4.30
.... VI
z
Z
....
III 8 4.20
Z !::1
o II::
u .... 4.10
c
(5
5 II!
-'
> ~ '.00
I DATA
-MODEL
O~---~--~ 2 3 5
o 50
Void Content ('/, by volume)
CURE PRE SSURE (psig)
been investigated in detail through suitable m~el studies [31, 32]. Experimental
measurements to relate the void content with cure pressure are done through
photomicrographic analysis [33]. The relationship between cure pressure, void
content and compression strength for a thermoset resin composite system is
given in Fig. 23. Factors during operation, such as temperature variations and
any moisture absorption would result in change of dielectric constant If moisture
content is high, pressures produced by heated vapours of air trapped in the
voids can cause variations in its electrical characteristics, as well as result in
physical change. This aspect must be viewed seriously if sandwich radomes
using honeycomb core is subjected to large temperature variations.
as are used for actual radome fabrication. All other parameters are also kept
identical so that the flat panels truly characterise the radome wall.
Electrically, the flat panel is tested for transmission loss and insertion phase
by following free space method. A typical set-up wherein measurements can
be carried out using a network analyzer is shown in Fig. 24. Corrections to
accommodate effects due to multiple reflections can be incorporated to improve
accuracy [35]. By rotating the sample panel, transmission coefficient can be
Test Panel
(>30 lC 3D)
-
Adjustable
e,
~
1
0
*
ill 30 •
Reference
PhOse Network
Locked Analyzer
Source
Fig. 24. Free space panel measurement set-up.
necessary to verify the correctness of the steps followed in the fabrication. Any
manufacturing error due to oversight or fall in quality of workmanship may
prove to be costly to be rectified when detected at the final stage. Even after
production, it is worth checking the performance of the radome using some
gauges prior to shipment and installation with antenna assembly. These gadgets
are normally evolved from simple original concepts to suit the specific
requirements.
INTER DIGITAL
ELECTRODES
10dB PADS
r-:OC==D~O==S::""I"""LL'-'/Ii.""';rOR~
~---I &POWER SUPPLY 1H DIA APERTURE
(AVANTEIQ
NETWORK
~--+ ANALYZER
PHASE
MAGNITUDE
DISPlAY
COAX
LOW-REfLECTION
HORN
HIGH-DIRECTIVITY
WIG DIRECTIONAL COUPLERS
IREC~;D",II----------IN~~~:~~ZEER
x- y
RECORDER
AMPliTUDE PHASE
Fig. 27. Microwave hom stethoscope.
calibrated panels can qualify the radome. The same principle can also be used
for assessing the quality of anti-static coatings and also any defects in radome
wall such as moisture pick-up or wall thickness variations due to erosion [38].
A simple gauge based on same principle uses short circuit stubs and shaped
grooves on its flange to make measurements more reliable and accurate [39].
A flexible conducting foil is held in intimate contact with the internal surface
of radome and acts as a back plate of the cavity. The gauge has been found to
be useful for pre-shipment checks.
5.1 Specifications
5.1.1 Materials
L-P-383 Plastic Material. Polyester Resin, Glass Fiber Base, Low
Pressure Laminated
MIL-C-7439 Coating System, Elastomeric, Rain Erosion Resistant,
and Rain Erosion Resistant with Anti-Static Treatment,
for Exterior Aircraft and Missile Plastic Parts
MIL-R-7575 Resin, Polyester, Low Pressure Laminating
MIL-C--8073 Core Material, Plastic Honeycomb, Laminated Glass
Fiber Base, for Aircraft Structural Applications
MIL-C--8087 Core Material, Foamed in-Place Polyester Disocyanate
Type, Interchangeability and Replaceability of Compo-
nent Parts for Aircraft and Missile
MIL-C-9084 Cloth, Glass, Finished, for Polyester Resin Laminates
MIL-R-9299 Resin, Phenolic, Laminating
MIL-R-9300 Resin, Epoxy, Low Pressure Laminating
MIL-R-25042 Resin, Polyester, High Temperature Resistant, Low
Pressure Laminating
MIL-P-25395 Plastic Materials, Heat Resistant, Low Pressure, Lami-
nated Glass Fiber Base, Polyester Resin
MIL-P-25421 Plastic Materials, Glass Fiber Base-Epoxy Resin, Low
Pressure Laminated
MIL-R-25506 Resin, Silicone, Low Pressure Laminating
MIL-P-25515 Plastic Materials, Phenolic Resin, Glass Fiber Base,
Laminated
MIL-P-25518 Plastic Materials, Silicone; Resin, Glass Fiber Base, Low
Pressure Laminated
MIL-C-27315 Coating Systems, Elastomeric, Thermally Reflective and
Rain Erosion Resistant
MIL-C--81773 Coating, Polyurethane, Aliphatic Weather Resistant
MIL-C--83231 Coatings, Polyurethene, Rain Erosion, Resistant for
Exterior Aircraft and Missile Plastic Parts
MIL-C--83286 Coating, Urethane, Aliphatic Isocyanate, for Aerospace
Applications
MIL-Y--83370 Yam, Roving and Cloth, High Modulus, Organic Fiber
REFERENCES
7. M.I. Skolnik. "Radar Handbook". (Ch 14).• New York: McGraw-Hili. 1970.
8. Proc. Symposia on Electtomagnetic Windows. Georgia Inst. of Technology.
Atlanta-Held on number of years starting from 1955.
9. International Conferences on Electromagnetic Windows. Paris-Held on number
of Years starting from 1967.
10. G.S. Mani et al. "Electrical Design Report of 14 GHz Radome". DLRL report
no. DLRL. : R : 86 : 020 (Restricted). March 1986.
11. G .S. Mani and Ramsingh. "Design and fabrication of radomes for a broadband
spiral antenna". DLRL technical notes (Restricted). Vol 2. March 1981.
12. R.H. Cary. "Some novel techniques for avoiding obscurations". lEE Conf.
Publication NO. ISS. 1971.
13. E.L. Rope and G.P. Tricoles. "Anisotropic Dieleclrics. Tilted grooves on nat
sheets and an axially symmetric radomes". IEEE International Symp. Antenna
Propag. Dig .• pp 610-611. JlUle 1979.
14. D.L. Loyet. "Broadband radome design techniques". Proc. 13th EM Window
Symposium. Georgia Institute of Technology. pp 169-173. 1976.
IS. D.C. Seller, "Abberation of dieleclric patches and rings". Proc. Int. Conf. on
EM Windows. Paris. 1967.
16. A. Cohen. P. Davis. S.C. Nilo and J.F. Orabona. "A 150 feet metal space frame
radome". Proc. OSU-WALDC Radome Symp. WADC Tech. Report 57-314.
17. Pelton and Munk. "A Streamlined Metallic Radome". IEEE Trans. Ant. and
Prop.• Vol. A. pp. 22. no. S. pp. 799-803.1974.
18. A. Cohen and A.P. Sondski. "Effect of rain on satellite commlUlication earth
terminals and rigid radomes". Microwave Journal. Vol 9. no. 9. pp 111-121.
Sep.1966.
19. M.M. Schwartz. "Composite Materials Handbook.... New York: McGraw-Hili.
1983.
20. G. Lubin. "Handbook of Advanced Composites". New York: Van Nostrand
Reinhold. 1982.
21. "Kevlar Use". Aviation Week and Space Technology. pp. 37. April 7. 1986.
22. 1. Cook. "Reinforcements for plastics intended for electrical and electronic
applications". Journal of Naval Sciences. Vol. 1. No.3. pp. 221-233. July 1975.
23. R.H. Cary. "Avionic Radome Materials". AGARD report no. AGARD AR-7S.
24. ''The basics on bonded sandwich construction". Hexcel Corporation Book Part
no. TSB 120 m:td TSB 124.
25. G.M. Brydon and R.H. Cary. "Some Radome materials with superior dielectric
and temperature characteristics". Proc. Int. Conf. on EM Windows. Paris. 1967.
26. G.S. Mani. et al. "Development of Broadband Radomes for Electronic Equipment
Pod". DLRL report No. DLRL R : 86 : 024 (Reslricted). April 1986.
27. M.S. Cray and M.G. Taylor. "Syntactic foam-A new method for radome
construction". Presentation given at Fourth Int. Conf. on EM Windows. Barcol.
France.
28. M.B. Punnett. "Raydel-Microwave transmissive fabric radome composites".
Proc Int. Conf. on EM Windows. Georgia Inst. of tech. pp. 117-123. 1978.
29. Joseph 1. Prifti. "Hardened TlUled-wall plastic radome for military radar".
30. "Astrocoat-Sterling erosion resistant coating system". Sterling Lacquer Mfg.
Co.• 3150. Brannon Avenue. St. Louis. M063139. USA.
31. G.S. Springer. "A model for curing process of epoxy malrix composites". Progress
in Science and Engineering of Composites. Japan Society of Composite Materials
pp 25-35. 1982.
Radome Materials 239
32. T.G. Gutowski, "A resin flow/fiber defonnation model for composites", Advances
in Technology in Materials and Processes, SAMPE, pp. 925-934, 1985.
33. 1.M. Tanged et al, "Effects of cw-e pressure on resin flow, voids and mechanical
properties", Jour. of Composite Materials, Vol. 21, pp. 421-440, May 1987.
34. M.N. Afsar, 1.R. Birch and R.N. Clarke, "The measurements of properties of
materials", Proc: IEEE, Vol 74, No. I, pp. 183-199, January 1986.
35. W. W. Ho, "High temperatw-e millimetric dielectric characterization of radome
materials", Proc. SPIB-Int. Soc. opt. Engrs, Vol. 362, pp. 190-195, 1982.
36. F.I. Shimabukuro et ai, "A quasi-optical method for measuring complex
permittivity of materials", IEEEE Trans. on Microwave Theory and Tech, Vol
MTT--32,no. 7,pp. 659-665, 1984.
37. T. Larry Norin and Luis L. Oh, "Monitoring AWACS radar radome fabrication",
Proc. 14th EM Window Symposium, Georgia Inst. of Tech., pp 137-145, 1978.
38. N.R. Ray, "A portable radome tester", Proc. 12th Symp. on EM Windows,
pp 117-124, June 1974.
39. Leon 1. Ricardei and Seymong Sutlcin, "A microwave radome perfonnance
verification gauge", IEEE Trans. on Ant. and Prop., Vol. 39, no. 2, pp. 131-
142, Feb 1991.
40. Gladius Lewis, "Selection of Engineering Materials", New Jersey, Prentice-
Hall,199O.
9
High Frequency Applications of High-Tc
Superconductors
C.M. Srivastava
Advanced Centre fot Research in Electronics and Department of Physics
Indian Institute of Technology. Bombay. India
1. INTRODUCTION
The current investigations on the technological impact of the high temperature
superconductors (HTSC) indicate that the most promising applications of these
materials are in the high-frequency devices. The replacement of waveguides
and coaxials circuits by microwave integrated circuits more than two decades
ago heralded a revolution in the field of microwave circuits. The main reasons
for the widespread use of microwave integrated circuits are increased reliability,
improved reproducibility and significant reduction in size, weight and cost.
These gains are of vital importance in space and satellite electronic circuits.
Further in military applications, where equipments are subjected to severe shock
and vibrations, MIe devices provide .better mechanical integrity than waveguides
bolted together.
Even before the advent of HTSe superconductors were used in some special
high frequency circuits and cavities [1,2,3]. The reason is that lower conductor
losses result in lower noise, higher speed and wider bandwidth. Amongst the
major systems applications is the use of superconducting microwave cavities
for accelerating charged particles. The possibility of using HTSe in super-
collider experiment is currently being examined.
Several successful attempts [4, 5, 6] have been made to develop passive
microwave devices like resonators, filters and delay lines using HTSe. These
devices are in the stripline configurations. A strip line is a thin narrow strip of
metal which is placed a short distance above a metal ground plane. The strip
is placed parallel to the ground plane and is separated from it by a thin dielectric
slab. The transmission occurs via the transverse electromagnetic (TEM) mode
much in the same manner as in a two wire line. A stripline is lossier than a
waveguide but it is smaller and cheaper and hence is extensively used.
The losses in stripline primarily originate from the dielectric and the conductor.
With improvement in the microwave dielectric materials the conductor losses
in stripline devices today dominate even when the best quality copper or gold
High Frequency Applications ofHigh-T. Superconductors 241
is used. With the advent of HTSC and use of liquid nitrogen as coolant for the
device it is possible to reduce the conductor losses and enhance the quality
factor of the device in a cost effective manner.
The possibility of complete elimination of refrigeration below ambient
temperature exists in a space environment where temperature close to 100 K
can be obtained from radiative cooling. If Tc can be further pushed by about
30 K from the existing maximum of 125 K for thallium based compounds it
should be possible to use many of these devices in aerospace industry without
additional refrigeration.
Although today several high Te superconducting compounds are known, most
of the high frequency applications have been attempted on YBa2Cu3O,(YBCO)
films. Only recently some results on Tl-Ca-Ba-Cu-O thin films have also been
reported.
There are however some problems which need to be solved before the rapid
deployment of the HTSC microwave device is possible. The fabrication of
these devices require development of good quality epitaxial thin films with
high Je , low RI , long term stability, methods of patterning without affecting the
superconducting properties, ohmic contacts and large size spbstrates of good
qUality. The device performance is critically dependent on these parameters of
the film. Further, the type of correlation which exists between the structural
and microwave properties of HTSC films is not clear at present. It is therefore
not possible to predict the device performance from the measurements on the
unpatterened films.
In this article, we discuss the electromagnetic properties of good conductors
and superconductors. Specially, we examine the dependence of the propagation
characteristics on surface· resistivity for a microstripline. We then describe
some of the microwave components which have been successfully fabricated
using HTSC materials. Finally, we give the current trends and future potential
applications.
2. ELECTROMAGNETIC PROPERTIES
carriers of charge transport cannot then interact with the external rf field and
exchange energy. This leads to anomolous skin effect and results in high value
for the high-frequency surface resistance compared to the d.c. resistance.
In the region where anomolous skin effect is absent (8) I), the normal state
surface resistance is given by
R. =_1
(18
=(tr /J,tcP)ll2 (2)
For copper at 300 K, p = 1.7 J,tO-cm andJl.c- Jlo = 4trx 10-7 HIm. For 10 GHz
we obtain R. = 40 mn. At 77 K, (1cu (77)/(1cu (300) - 16. We then have at
77 K,R.-10 mn.
The dependence of surface resistance on temperature and frequency for
copper has been measured by Hammond et al [7]. It is found that R, varies as
ro1/2 for the metals in the normal state. Further, since (1 increases as temperature
is lowered, R. decreases with temperature at constant frequency.
where
(1sc =(11 - j(12 (3a)
is the conductivity of the superconductor. Using the BeS weak coupling theory
[9] Mattis and Bardeen [10] have obtained the expressions for (11 and (12. Since
these expressions involve complicated integrations over the quasi-particle energy
states we adopt a simplified semi-classical model which to some extent reproduces
the results of quantum mechanical calculations.
For superconductors, zero resistivity leads to the acceleration equation
mv=eE
=
Since J nev, where n is the number of charge carriers per unit volume, we
can write this equation as
. ne2 (4)
J=-E
m
We consider the two fluid model [11] in which the current is assumed to be
a superposition of a normal (resistive) I n and a superconductive component J.
J = I n + J. (5)
High Frequency Applications ofHigh-T. Superconductors 243
with
JD = O'E (Sa)
where (J is the normal state conductivity of the metal. Then, neglecting
displacement current
v x H = O'E + J. (6)
and so
v x V x H = O'V X E + V X J.
or
(7)
From Eq. (4)
. ne 2 ne 2J.1. • (8)
V x J. = - V x E = - - - H
m m
Using Eq. (7) and (8), we obtain
V2 H = 0'J.LiI + 12 H (9)
- .t2 + :li
Y2 -..L ~2
(11)
where ~ is the ~kin depth (Eq. 1) and y is the propagation constant in the
superconductor.
The surface impedance is defined by the ratio of the electric field Ell to the
magnetic field HII tangential to the conductor surface
Ell . jOJJ.I.
Z. = -H =R. +JX. = - - (12)
II Y
In the normal state (T > TJ .t = 00 and Eq. (11) gives
y= 1+ i = UOJJ.l.O')1I2 (13)
Using Eqs. (12) and (13) we obtain the expression for R, which agrees with
Eq. (2).
For the superconductor ( T < Tc), .t is finite and can be very small at low
temperatures compared to ~, so Eq. (11) determines the characteristics of
microwave propagation. Substituting from Eq. (11) into Eq. (12), we obtain
(A.« 0) (15)
(16)
(18)
and
R2 +X2
(19)
A. = CO J.l. (~;
_ ;;)1/2
The conclusion thatR, is proportional to co 2 and XI is proportional to ro has
been derived by Hartwig [12].
Many studies of the temperature dependence of surface resistivity of
superconducting rums have been reported [7, 13, 14]. This data can be compared
with the expression for R, in Eq. (15). According to two fluid model a oc 14
and A.2 oc (1 -1 4rl, where 1 =Tae• So R; can be expressed as [1]
J.l.2an(1~)A.~C02 t4
R, - 2 (1 _ (4) (20)
I00c-------+---------,
9.55 GHz
-
E
aE
- -
10
CF HC Cu ..... --
.....
~ .....
B
1/1
'iii
III
II:
t:. #: V 262
III
•'*
x :ij: V 266
.9
5
III
V 302
o 100 200
Tllmperature (K)
Fig. 1. The measured surface resistance vs temperature at low power for three
Tl-Ca-Ba-Cu-O thin films. The complete temperature scan for film # V302 is
shown. The other two fJ.J.ms were measured at 4.2. 77 and 150 K. At 77 K the
R. for all three films is at least 20 times smaller than copper at the same
temperature [7].
where R(ro, 1) is given by Eq. (20) or (21). Rres is a sample dependent constant
whose origin is yet not known. Amongst several possible causes of residual
resistance are the presence of normal conducting materials, tunneling across
cracks, generation by phonons by the rf field and grain boundary scattering of
charge carriers. It is observed that for T,;/T > 5, Rres invariably dominates.
Ground
plane
Fig. 2. Geometry of a micros trip line. The ground plane and the strip mayor may not
be of the same metal. The dielectric substrate is a low microwave loss material.
Ow' is the width and ',' is the thickness of the strip and 'h' is the thickness of
the dielectric substrate.
(24)
where the subscripts c, d and m stand for conductor, dielectric and modal
contributions to a and p.
Using the transmission line equation
(25)
for the propagation of a sinusoidal voltage V (X, m)eimt on the microstrip line,
it can be shown that r is approximately given by
(29)
Detailed analysis of the losses in microstrips using normal metals has been
given by Pucel et al [20]. Caulton [21] has given a simplified formula for such
striplines
High Frequency Applications 0/High-Tc Superconductors 247
a R. (1.. + 1 ).
= Zo m-I (30)
c w 2h+w
Here Rs is the surface resistivity of the conductor. w is the width of the strip
and h is the thickness of the dielectric substrate.
The characteristic impedance ~ is given in terms of Er. w and h by an empirical
relation obtained by Wheeler [22]
(31)
This gives similar results as the simplified expressions obtained for Zo by
Schneider [23] for the two limits of wide (w/h > 1) and narrow (w/h < 1) microstrip
lines.
(32)
1
Zo=--60ln -+-
.JEcff
(8hw 4hw) (33)
where
Er + 1 Er - 1 ( 10h)-1/2
Ecff=-2-+-2- 1+ W (34)
The effective dielectric constant is given by Eq. (31) only upto the cut-off
frequency
f c -- c
4h (Er _ 1)1/2
(35)
Eq. (35) gives the region (0 </ </J in which the lowest order longitudinal TEl
mode for the microstrip dominates. For /> !C. £eff becomes frequency dependent
and is not given by Eq. (34).
Dispersion at high frequencies has been analyzed by Mittra and Itoh [24]
and Atwater [25]. At very high frequencies the transmission line behaves as a
waveguide with the wave completely confined to the dielectric region.
Consequently the effective dielectric constant £eff approaches Cr as the frequency
is increased to a very high value.
It is convenient to relate Eeff to a dielectric filling factor q by
Ecff - 1 (36)
q = Er - 1
=
For a 25 mil alumina substrate with Er 10, Ie from Eq. (35) is 40 GHz.
= = =
With hlw 1 Eq. (34) gives eerr 6.86. This gives q 0.65. Yamashita et al
[26] have discussed numerical methods for the estimate of £err beyond Ie. This
is needed to estimate the modal phase factor Pm in Eq. (24)
= =
For I 10 GHz, A. 5000 Aand Zo = 50 n since 82 - 1 we obtain Pc - 1 rad/m.
For £err if) - 16, from Eq. (37), Pm - 102 rad/m. Thus Pm » Pc.
It can be shown that in general Pc « Pm. It is therefore not necessary to
include Pc in the calculation of the phase velocity. We then have
211:1 c
vpb =-- =
Pm ~eeff(f)
(39)
Ekholm and McKnight [19] have calculated the phase velocity as a function
of frequency for a microstrip line with wlh = =
I, h 0.5 mm and Er 27.0. =
They have used numerical approximation of Yamashita et al [26] to estimate
eerr (f). From Eq. (35)1c is nearly 20 GHz. Their result for Vpb vslis shown
in Fig. 3. The decrease in Vpb occurs due to increase in £err (f) in the frequency
band between 1 and 100 GHz.
7-10 7
7
5-10
10 8 1010
Frequency (Hz)
From our approximate analysis the low frequency phase velocity limit
should be C/.JEeff' where Eeff is given by Eq. (34) while the high frequency
phase velocity limit should be c/Fr. These two values are 7.55 x 107 m/s and
5.77 x 107 m/s respectively which are close to the values given in Fig. 3
obtained from a more accurate analysis.
It may be noted that the dispersion in phase velocity arising from Eeff (f )
spreads over a large frequency band, 1 to 100 GHz. If a pulse propagates on
the microstrip line which has dominant frequency components in this region
severe distortion in the shape of the pulse will occur due to this dispersion.
The transition from the higher to lower phase velocity occurs near 10 GHz.
At this frequency the wavelength within the substrate is A/ Fr - 0.57 cm and
is comparable to the transverse dimension of the microtrip. The dispersion
therefore is primarily arising from geometry related modal effects which
determines the redistribution of energy from the TEl mode to higher order modes
for f > !c. On the other hand the attenuation in the system is determined both
by the contributions by the conductor and the dielectric.
The loss in the dielectric substrate which fills the region between the conductors
in the transmission line is small. An approximate expression for ad in Eq. (24)
is given by [19]
ad~ n Er tan
~
0 ~
1
m-I (40)
"V Eeff 11.0
where Ao is the free space wavelength and tan 0 is the loss tangent of the dielectric.
Lanthanum aluminate (LaAl03) and lanthanum gallate (LaGa03) have been
extensively used as substrates in HTSC microstrip line. At 77 K these materials
have [27] Er - 23 and tan 0 - 2 X 10-4. Using Eqs. (34) and (40) for stripline
= =
with w/h 1, we obtain l1.! 1.08 dB/m.
For a copper microstrip line on LaAI03 substrate at 80 K and 9.55 GHz, Rs
has a value [7] nearly of 10 mn. With w/h = 0.25 and w ::;: 0.5 mm, we get a
value of about 56 n for Zo from Eq. (33) and obtain lXc - 3.5 dB/m from
Eq. (30).
Compared to copper at 80 K TI-Ca-Ba-Cu-O film deposited on LaAl03 has
Rs - 0.5 mn [7]. In this case then <Xc would be 20 times smaller than the copper
microstripline. It would then also be smaller than the attenuation ~ produced
by the dielectric.
Sec. 3 shows that at 60 K the HSTC line should be significantly less attenuating
than the coper line at the same temperature. The application of HTSC microstrip
lines at frequencies above 10 GHz appears to be most useful on account of
very high attenuation of cooled copper at these frequencies.
Winter and Rose [29] have studied the transmission properties of high Tc
superconductor waveguide. Their results show that these have the potential of
100 GHz of band-width for transmission over long distances with low attenuation.
They also show that the millimeter waveguide would have the advantage over
optical systems since they can have much lower carrier frequency which would
result in wider dynamic range.
Despite attractive advantages widespread use of high Tc superconductors in
high-frequency devices have not been possible due primarily to the difficulties
of fabrication of reproducible high quality films for microstrip lines. Likewise
HTSC microwave cavities for accelerating charged particles have been
investigated but the progress is slow due to difficulties arising from the techniques
used for their fabrication.
One of the major problems arising from imperfection in structure due to the
methods used for synthesis is the discrepancy between theoretical and experimental
results which in the case of attenuation constant may be of a few orders of
magnitude. The disagreement may also be due to the inadequacy of the theoretical
models like those used in Sec. 3 [30] for the analysis of the properties of HTSC
materials.
*Ytttia-stabilized zirconia.
The most commonly used HTSC material is TBCO. The films are generally
prepared by laser ablation deposition followed by post-deposition thermal
processing.
In Table 1. we have also given reference to the work in which these substrates
have been used to make a microstrip line. We have also indicated in the table
=
the cut-off frequency !C. obtained from Eq. (35) with h 0.5 mm. At frequencies
greater than!c the microstrip line supports a variety of waveguide modes in
addition to the quasi-TEM mode of low frequencies. This has important effects
High Frequency Applications ofHigh-T, Superconductors 251
W= 143 l-1 m
t1 =0.5 )1m
t s =254pm
tt =0.1 )1m
·t 2 =1.0)lm
Fig. 4. 35 GHz ring resonator structure fabricated from laser ablated YBCO thin film
on lanthanum aluminate substrate. The film is c-axis aligned and its Tc is
89.8 K. The metal ground plane is deposited by first evaporating 100 A. of Ti
for adhesion followed by 1 micron of gold [36].
-1 = -
1 1
+- 1
+- (41)
Q ac Qr C?!
Radiation losses are reduced by choosing smaller lateral waveguide dimensions.
252 MICROWAVE MATERIALS
(43
254 MICROWAVE MATERIALS
and V = 1/30 m3, Ep - 9.5 J per cavity. The energy loss per cavity is given
by
w= Epl (44)
Q
For copper cavity, Q - 6 x 1<t. Iff - 1 GHz, W - 170 kW. The total power
consumption for 400 cavities is then 68 MW. At present such high powers can
be produced at high frequencies only in the pulse mode. If the surface resistance
can be reduced by three to four orders of magnitude the Q can be substantially
improved and the power dissipation reduced to a level that continuous operation
of a Linac would be possible. This possibly can be achieved with the help of
a HTSC superconductors at 77 K.
We note that the performance of the microwave cavity is limited by two
parameters-the critical field (He) and the surface resistance (R.). It is in fact
the superheating critical field Hsh, which determines the peak power handling
capability of the cavity without loosing the superconducting properties through
the relation
For Nb, H.h - 1600 Oe, so Emu - 60 MV/m. In HTSC material, H.h is much
higher. For example, in YBCO the thermodynamic critical field is 27,000 Oe
and the superheating critical field is 20,000 Oe. One can, therefore, take for
HTSC that H.h is 10 times higher than Nb so the accelerating voltage capability
of a HTSC cavity increases to 600 mV/m. This leads to substantial reduction
in the number of cavities required to ahieve the same energy.
The improvement in Q due to reduction in surface resistance when HTSC
cavity is used leads to lower power dissipation and thereby to lower cost of
operation. The Q of the cavity is given by
Q = Jlo VI (46)
R.A
where f is the frequency and V /A is the volume to surface ratio of the cavity.
Assuming VIA - 0.1 m, f =1 GHz, R. - 10-7 n approximate for a superconductor
for Tc/T > 5, we obtain Q - 108 • This is four orders of magnitude larger than
for a copper cavity.
Attempts to use HTSC cavities in Linac are in progress [41] and it is likely
that soon attractive economic benefits will be realised in this application.
6. CONCLUSION
The high frequency properties of high temperature superconductors have been
dis~ussed and in particular their surface impedance has been examined as a
High Frequency Applications ofHigh-Tc Superconductors 255
REFERENCES