Investigation of Ion Beam Properties and Coating Material During IBS
Investigation of Ion Beam Properties and Coating Material During IBS
Investigation of Ion Beam Properties and Coating Material During IBS
IBS
M. Jupé1, 2, S. Malobabic1, 2, C. Schmitz1, C. Gouldieff†, H. Steffen*, R. Wiese* and D. Ristau1, 2
1
Laser Zentrum Hannover e.V., Department of Laser Components, Hannover, Germany
2
Quest: Centre for Quantum Engineering and Space-Time Research, Hannover, Germany
* Leibniz-Institute for Plasma Science and Technology e.V., Greifswald, Germany
†
Institut Fresnel, Marseille, France
Abstract
Ion beam sputtering (IBS) is a well-established process to manufacture lowest loss coatings of highest
complexity of spectral behavior. Nevertheless, the losses due to absorption in the bulk materials are still orders
of magnitude lower than in the corresponding coatings, indicating that a further optimization of the process is
possible. Such an improvement in quality requires a more detailed knowledge of the correlation between the
process parameters and the coating quality.
The present paper reports on a preliminary study based on a parameterization strategy for IBS processes. The
propagation properties of the ion beam were investigated in detail, where both, the total dissipation of energy and
the argon ion velocity distribution of the beam were measured and analyzed. Furthermore, research was
concentrated on the sputtered material considering the dependence of the optical losses of the deposited
dielectric layers on the physical properties of the adatoms. The energy distribution and the charge state of the
material particles were investigated with respect to the implementation of a phase separating IBS process.
1. Introduction
In the development of modern dielectric optical components, a growing specialisation can be observed. With
respect to the field of application, the coating material, the coating process and process parameters are optimized.
As a consequence of this development, some research groups are focussing their activities on the optimization of
one special parameter. The most prominent example is the optimization of the damage threshold for high power
lasers. Few other groups are working on the minimization of optical losses. In the past, the requirement of lowest
loss optics was mainly driven by special applications in high precision laser measurement technology or high
power laser systems. In this context, the development of mirrors with extremely small backscatter values for
laser gyros and the reduction of absorption losses in cavity mirrors for gravitational wave detectors are
prominent examples. During the last decades, the process of optimization of low loss components is further
intensified by the development in the optical sensor technology [1].
Within the scope of the cluster of excellence “QUEST” the Einstein-Telescopes and the optical clocks require a
new generation of optical components with respect to the optical losses. Nowadays, Ion Beam Sputtering (IBS)
is an attractive and convenient deposition process that can achieve highest-quality standards in optical thin films
close to these requirements. The IBS-technology allows the production of coatings with unsurpassed properties
in terms of scatter and absorption losses. According to the current state of the art, dielectric mirrors with losses in
the range of below one ppm are available for the NIR-spectral range around 1 µm, but an improvement of one
order of magnitude would be desirable. In scientific and commercial applications the IBS-technology is very
well engineered and optimized. Consequently, a further improvement of the coating quality seems to be only
achievable by a fundamental change of the coating process. A promising approach can be the realisation of a
separator for the adatoms. The main aim of the separator concepts is a drastic reduction of the concentration of
so called macroparticles. The presence of macroparticles during the coating process leads to defects, causes
topographical problems and can lead to inhomogeneous inclusions and rough films. Separator technologies are
established for arc-deposition techniques in combination with magnetic or electrical atom and particle filters [2-
6]. Usually, arc-deposition techniques are designed for metallic coating. An application for dielectric materials is
rather not commented.
Advances in Optical Thin Films IV, edited by Michel Lequime, H. Angus Macleod, Detlev Ristau,
Proc. of SPIE Vol. 8168, 816825 · © 2011 SPIE · CCC code: 0277-786X/11/$18
doi: 10.1117/12.905363
Methods of Characterization
The understanding of the adatom fluxes requires a detailed and precise characterization of the plasma beam to
obtain a more complex insight into the coating process. Applying a combination of high-precision
characterization tools, a consistent survey on the plasma properties at the sampling position can be derived. In
the following, several different measurement systems for the analysis of plasma are shortly discussed. A
Langmuir probe [7], a Retarding Field Analyser (RFA) and thermo probes were used to identify and extract
properties of correlated structures associated with the propagation of the plasma, which is emitted from the target
during the sputter process.
Langmuir probe
A relatively uncomplicated probe concept was suggested by Langmuir [9], originally, and optimized by
Laframboise [10] and Allen et al. [11]. This so-called Langmuir probe measures the current into a metallic test
area depending on the applied voltage in correlation to the potential and carrier distribution inside the plasma.
The schematic drawing of the Langmuir probe is displayed in Figure 1. From the voltage versus current curve
characteristic parameters like the electron temperature, the floating potential and the ion density can be extracted
(See Figure 2.).
20,0µ
C u rre n t [A ]
ρIon=-7,35E-7/(eA)
2
Langmuir probe are mainly of interest. This range is
-6
-1,0x10 = 7,46E13 Ion/cm
defined by a retarding of the electrons with a
-6
-2,0x10
-20 -15 -10 -5 0 5 negative potential at the effective surface of the
0,0 Bias Voltage [V]
probe [12]. If the voltage at the surface is low
enough, the electrons are blocked, completely, and
the current is solely induced by the ions. A
-20,0µ
Cha11005 decreasing voltage causes an increasing influencing
-1000 -800 -600 -400 -200 0 200 sphere of the electric field and consequently a
Bias Voltage [V] decreasing current. The ion flux density without an
external voltage can be determined by the
Figure 2: Langmuir probe measurement extrapolation of the linear section of the curve until
it intersects with the vertical axis [13].
I 0 (U = 0)
ρ Ion = (1)
eA
Herein, A is the effective area of the probe, I0 (U=0) the intercept point of the linear fit, and e the elementary
electric charge, respectively.
Additionally, the current versus voltage curve indicates the floating potential. It is defined as the potential which
is measured from the metallic body without an external field. In this case, the current induced at the Langmuir
probe is exactly zero. The Langmuir probe can be a powerful instrument and versatile tool in plasma diagnostics
[14].
δI/δUBias [Ω ]
-1
75n are blocked by a negative potential on the
-200n
Current [A]
-400n
50n suppressor grid (see Figure 1). In the used set-up,
25n
the ions are slowed down by a variable positive
-600n
retarding field on the collector [15]. The ion current
0
-800n is decreasing with an increasing retarding field, and
δI/δUBias
-1µ
Cha11007
-25n the first derivate of the current-voltage-curve
0 5 10 15 20 25 30 displays the energy dispersive ion distribution g(E):
UBias[V]
dI n ⋅ e
= g(E) (2)
dE m
charge, and m is the mass of the ion. Usually, with respect to theoretic approximations, n is set to one.
The ion current Icup (Uret) is directly linked to the velocity distribution of ions g(v) according to:
mv 2 dI ev 2
E= = g (v) (3)
2 dU ret 2U ret
Where v is the velocity of the particle, and Uret is the retarding field. Figure 3 shows a typical example for an
energy dispersive distribution of a RFA measurement.
Balance point of the dI (U ) For the interpretation of the measurement result, the
ion distribution ∫ dU dU maximum of the energy dispersive ion distribution is an
U BP = ret
important parameter. In many cases, there are complex
∂I max
structures and the maximum is not determined. In such
∂U ret
cases, the balance point of the curve can be used.
maximum of the
energy dispersive ion
Thermo probe
The Langmuir probe, as well as the RFA measures only the ions of the plasma. The part of the neutral adatoms
does not contribute to the measurement signals. The thermal probe allows a direct access to the neutral and the
charged part of the plasma by the determination of the heat transferred to a thermal mass of the test sample by
the impinging species. Particularly, the induced temperature rise is a result of the collision of ions, as well as
adatoms or other particles on the probe, but furthermore additional thermal radiation sources can influence the
measurement [16]. Consequently, the sensor has to be isolated from unwanted heat sources. In the presented
investigations two different types of thermo probes are applied. The active thermo probe was mainly used for the
beam characterization of the sputter source. For this type of sensor the temperature of the probe is stabilized by
an electrical heater, which is coated onto the backside of the thermo probe. The power of the heater controlled to
stabilize the probe at a nominal temperature. As a consequence, the impact energy can be directly derived from
the difference of the initial heat power to the resulting heat power including the external sources. The resolution
of the probe is about several tenths of mW/cm2, and therefore, the thermo probe is well appropriate for powerful
sources. For the measurement of low power sources, the passive thermal probe is recommended. A schematic
drawing of the set-up is displayed in Figure 1. The temperature of the test sample is measured by thermistors
(NTC- Negative Temperature Coefficient), which are calibrated by a standard PT100 resistor. The calibration of
the NTCs is displayed in Figure 4. The temperature - resistance curve of the NTC is not linear, but can be
approximated linearly for the temperature range of the coating process, which is also applied for the passive
thermo probe measurements.
4,0
Calibration of passive thermo probe
3,5
3,0
2,5
Sensitivity
2,0
S=15,46 K/V
U [V]
R=99,93 %
1,5
1,0
0,5
measurement values
test sample temperature
0,0 during coating process
cha11006
20 30 40 50 60
temperature [°C]
Figure 4: Calibration of passive thermo probe Figure 5: Example of passive thermo probe
measurement
The resolution of the detector is in the order of few 10-2 K, which corresponds to a heat power of below
0.01 mW/cm2. In the application, the signal is influenced by external noise sources, and consequently, a
∂Wtot 1 ∂Wtot
= N Ion ρ ⇒ N Ion = (6)
∂U Bias ρ ∂U Bias
Wtot, WNeutal, and WIon are the total power impact, the impact of neutral adatoms and the impact of ions,
Ion , Neutral
E kin E Ion
represents the kinetic energy, and NNeutal, Ion is the adatom density, respectively. Colomb is the
coulomb potential with the voltage Ubias and the charge ρ. In particular, the slope of the impact power as a
function of the bias voltage is proportional to the density of ions. The main problem of this method is the
electrical isolation of the test sample by the dielectric coating. Therefore, in the case of dielectric coatings the
error budget of the measurement is difficult to estimate.
First, plasma analysis was employed for the ion source characterization. In this issue, the active thermo probe
from Leibniz-Institute for Plasma Science and Technology (INP) and the RFA were applied for the
determination of both, energy density distributions and the three dimensional ion beam distribution. In the
experiments involving the active thermo probe the sensor was moved on a circular pass through the beam. The
radius of the mounting is large compared to the diameter (r=380 mm) of the ion beam (r=80 mm). The distance
to the source can be arbitrarily set.
1,00
2
2
1,0
0,75
0,9
0,3
0,50
0,2
0,25
1,8 Distance from the front shield of the Ion source 22,5 cm 1,4 Source parameter Distance from | total Power
Measurement of Veeco three focus grid (500V, 200mA) VBeam: 500V
1,6 Measurement of Veeco "low contamination" grid (600V, 250 mA) IBeam: 200mA
the front shield|
1,2 12.5 cm | (133.2 W)
1,4 22.5 cm | (127.5 W)
Power density [W/cm²]
1,0 38 cm | (104.3 W)
1,2
1,0 0,8
0,8
0,6
0,6
0,4
0,4
0,2
0,2
0,0 0,0
-200 -150 -100 -50 0 50 100 150 -200 -100 0 100 200
Distance from the beam center [mm] Distance from the centre of the beam [mm]
Figure 9: Power density profiles of the ion source with Figure 10: Power density profiles of the ion source with
the low contamination grid and the one with the three the low contamination grid in three different distances
focus grid. from the ion source.
0,6
0,4
0,2
0,0 cha11007
Additional information of the plasma beam can be gained by the RFA- measurements. Herein, an RFA is
mounted on the target translator in combination with a wire pull system. The set-up is displayed in Figure 11. As
mentioned, the RFA measures solely the ions of the plasma, and the applied RFA measures a relative ion
density. The comparison of the ion distribution with the power density distribution in approximately the same
measuring plane is shown in Figure 12, whereas both profiles are normalized to one. The form of the profile is
equivalent within the measurement accuracy. Consequently, the ion distribution and the plasma follow the same
behavior. In detail, in the dimension of the coating plant a larger divergence of the charged particle is not
observed. However, in Figure 13 the beam profiles of the plasma beams of the high power source applying three
Current [A]
-5 0 5 10 15 20 25 30 35 -10 -5 0 5 10 15 20 25 30 35
UBias [V] Bias [V]
Figure 14: RFA – measurement of the plasma of a Figure 15: RFA – measurement of the plasma of a
titanium target and in front of a silicon target for silicon target for different reactive gas fluxes.
different beam voltages.
In the first step, the influence of the material is discussed. In Figure 14, the energy dispersive distributions of
titania and silica are compared. The ions emitted by the titanium and the silicon target have characteristic
distributions. The energy dispersive distribution of ions from the titan target has a maximum at around 7 eV, but
the maximum of the distribution of the ions from the silicon target are located around 17 eV. Figure 15 displays
for the example of titanium that the energy distribution is changing with the concentration of the reactive gas.
For the present example of titanium and titania, the maximum of the distribution is shifting from 17 eV without
oxygen to 7 eV for titania. The properties of the material are mainly influence by processes on the surface.
Currently, these processes are not understood in detail, but for the dimensioning of the electromagnetic field of
the separator the measurement is essential. In particular, the kinetic energy of the adatoms has to be measured for
the construction of magnetic coils [3, 4].
An additional factor is the ionization state of the plasma and the ion density in the plasma, because the maximum
efficiency of a separator is dependent on the ion density in the plasma. Both, the ion density and the development
of the ion density as a function of the distance from the target are important parameters of the plasma process. As
14 Cha11012
14
5,0x10 1,6x10
TiO2
14
14
4,5x10 SiO2 1,4x10
Ion flux density [1/(cm²s)]
14 14
1,2x10
2
4,0x10
14 14
3,5x10 1,0x10
14 13
3,0x10 8,0x10
14
2,5x10 6,0x10
13
14
2,0x10 4,0x10
13
14
1,5x10 13 Distance 190mm
2,0x10
14 TiO2
1,0x10 cha11012 0,0 SiO2
60 80 100 120 140 160 180 200
Distance from the target [mm] 0 200 400 600 800 1000 1200 1400
Beam Voltage [V]
Figure 16: Ion density distribution depending on the Figure 17: Ion density distribution, dependence on the
distance to the target measured by Langmuir probe. beam voltage measured by Langmuir probe
(Distance to the target 19cm).
However, all results of the Langmuir probe measurements indicate a significant ion flux density from the target.
In the following, the power density and the charge of the adatoms are investigated by the passive thermo probe
measurements. In these experiments, two different configurations were used. In the first series, the
measurements were performed using a metallic titanium target. The distance to the target was 17 cm and the
thermo probe was placed exactly in the center of the sputter distribution. An additional shutter was mounted on
the thermo probe. In the second case, the thermo probe was placed in the position of the substrates typical for the
coating process. In this case, the thermo probe was placed in a distance of 19 cm from the target and shifted
10 cm in the direction of the sputter source. For the second measurement series, the substrate shutter of the
coating plant was used for the interruption of the material flux from the target. It has to be noted that the
quantitative values of the both series are not completely comparable. In both series, a negative bias voltage was
applied to the metallic probe body accelerating the positive ions onto the probe surface. Figure 18 depicts the
4 2,0
3 1,5
2 1,0
metalic titanium
TiO2 measurement a Ta2O5
0,5
1 SiO2 Measurement 1
TiO2 measurement b
SiO2 Measurement 2
SiO2 measurement c cha11013
cha11013 0,0
0
0 10 20 30 40
-10 0 10 20 30 40 50 60 70 80
UBias [V]
UBias [V]
Figure 18: Result of passive thermo probe Figure 19: Result of passive thermo probe
measurements of the first measurement series measurements of the second measurement series
resulting power density impact depending on the bias voltage for metallic titanium, dielectric titania, and silica,
respectively. The resulting power impact densities are in the range of a few mW/cm2, and, as expected, all curves
show a small positive slope. The highest power density impact is observed for titania, which was manufactured
in a reactive process with oxygen from a metal target. In contrast, the metallic process reveals the lowest power
density flux. The coating rate in the center of the sputter distribution was 0.240 nm/s for titanium and 0.127 nm/s
for titania in the experiments with a static calotte. Consequently, the rate is not the main cause of the different
power impacts. The reason for this effect has to be investigated in further experiments. Possibly, the oxidation on
the sample surface increases the power impact, but also the change of the spherical sputter distribution can
influence the result. However, in comparison to titania the coating with silicon involves half of the power.
Cha11015
In the second experimental series tantala and silica
Titan metalic
14
1,4x10 are compared in Figure 19. In this case the coatings
TiO2
Ion flux density [1/cm s]
SiO2
14
where performed using a rotating calotte. The
2
1,2x10
Ta2O5
1,0x10
14 coating rates of the materials are 0.069nm/s and
13
0.061nm/s for tantala and silica, respectively. The
8,0x10
power impact density is reduced by a factor of two,
13
6,0x10 which is attributed to the changed position of the
4,0x10
13
thermo probe. The power impact for tantala is a
13 factor of two larger than the power impact of silica.
2,0x10
The experiment confirms a significant influence of
0,0
the material and the geometric position.
Figure 20: Ion density flux calculated on the basis of the For a particle control by electro-magnetic forces, the
passive thermo probe measurements. content of ions has to be determined from the slope
of the curves. Obviously, a significant noise level is
observed for the measurement. In addition, the slope of the curve depends on the thickness of the coating. For
thick coatings no significant dependency on the power impact density on the bias voltage can be observed. The
measurement 2 of silica in Figure 19 demonstrates this effect. In these cases, coverage by a dielectric layer is
assumed. The ion densities with freshly polished test sample are displayed in Figure 20, and the highest ion
Conclusion
The presented studies were motivated by fundamental exploration of the properties of the sputtered particles,
with respect to the realization of an efficient magnetic filter system. For the realization of a filter system, the
nature of the plasma has to be understood in detail.
The first investigation was focused on the determination of the beam profile of the sputter source scaling the
dimension of the ion pipe. Herein, the plasma beam of a sputter source - applying three different grids was
investigated. For each grid, a three dimensional distribution of the ion of the plasma was measured by RFA
mappings, and a characteristic beam propagation was observed for each configuration. Two of the grids lead to a
continuous divergent beam. The beam diameters on the target were measured to range between 8 and 30 cm, and
the diameter depends on the applied grid system. Consequently, the entrance aperture of the separator system has
to be constructed in the respective dimension. The measurements of the beam diameter of the sputter source
were also correlated to scans using an active thermo probe in front of the sputter source. The lateral profiles were
in agreement for RFA and for the thermo probe measurements. Additionally, the power impact of the plasma
beam was measured and calculated in three different distances in front of the ion source, and the results of the
thermo probe investigations indicated a significant decrease of the average beam power with increasing distance
from the source. This fact has to be investigated in further experiments.
The second issue was concentrated on the plasma properties of the sputtered material emitted from the target. As
diagnostic methods, the Langmuir probe, the passive thermo probe and the RFA were used. In these
measurements the plasma from silicon, titanium as well as tantalum targets was investigated.
Due to the fact that this project is targeted to the development of an electromagnetic separator, the investigation
in the plasma properties were concentrated on the charged part of the sputtered material. An important parameter
is the ion density inside the plasma because the efficiency of a separator is limited by this parameter. For the
experimental determination, a Langmuir probe and a passive thermo probe with variable electric potential were
employed. The evaluation of the experiments yielded ion densities of 1013 to 1014 ions/(cm2s), which would lead
to approximately half of the coating rate compared to other IBS processes depending on the efficiency of the
separator. Additionally, the measurement of dielectric materials is afflicted with a systematic imperfection,
which seems to lead to a covering effect for electrical fields. Nevertheless, the measurement shows a sufficient
ion density at the beginning of the experiments for the separation. In this frame also the kinetic energy of the
ions is of importance, because the kinetic energy determined the Larmour radius of the electrons as well as the
ions, which is essential for the generation of stable conditions in the ion pipe. The energy dispersive function of
ions was measured by an RFA. Hereby, ion energy in the order of a few eV was determined and therefore, the
energy is in accordance with the results presented for other published separation processes. The energy of the
ions is specific for the materials.
1
The mass of the test sample was 9.8 g. Therefore, the polishing of the test sample does not show a significant
influence on the measurement results.
The authors thank the German Research Foundation (DFG) as part of the cluster of excellence 201 QUEST-
Centre for Quantum Engineering and Space-Time Research. Additionally, the work was supported by the
German Ministry for Science and Education in the frame of the project “Plasma und optische Technologien –
Pluto” (BMBF, contract 13N10462 and contract 13N10460).
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