Testing the nanocrystalline cores

1. Measurement of the quasi-static hysteresis

The measurement system was developed for testing toroidal samples prepared
from ultra-soft magnetic materials (Hc < 1 A/m). Nevertheless, the equipment can be
used for taking the hysteresis loop of semi-hard magnetic materials as well (Hc < 10
kA/m) due to the Kepco type DC power supply (Imax = 50 A). The measurement
system is shown in Fig. 1.

Sample
Walker
integrator

Signal
generator

Fig.1. Measurement system to measure, compute, plot and display the quasi-
DC hysteresis loop characteristics.

For the toroidal samples we use the less number of exciting and detecting coil
windings. For the ultra-soft magnetic materials (Finemet type nanocrystalline, zero-
lambda amorphous, etc) it is sufficient a linear conductor through the centre of the
toroid (one turn exciting coil).
1.a. The hardware of the measuring system.

For toroidal samples the slowly varying exciting field can be calculated with
eq.1, where the current is measured through the potential drop, UH, on a measuring
resistance, R, connected in series with the exciting coil, I = UH/R:

N1 I N1
H= = U H [A / m] (1)
l lR

The length of the magnetic path and cross section, S, are calculated by eq.2 and
eq.3, respectively:

di + do
l = [m] (2)
2

S=
m
l
m2[ ] (3)

The induced signal, Ui, is given by the eq. (4) as a function of cross section, S ,
measuring frequence, f, and the number of secondary turns, N2:

Ui = N2 S f
dB
[V ] (4)
dt

This signal is integrated by the Walker integrator yielding the magnetic

induction, B in Tesla:

1
B(t ) =
N2 S f
U i (t ) dt [T ] (4)

In our case N1 = 1 and N2 is varying between 10-100. The larger the N2 the
smaller is the drift of the integrator.

In order to generate the waveform of the exciting current we have the following
possibilities:

1. The built in waveform generator of Kepco power supply. This provides limited
number waveforms only.
2. The Agilent function generator provides the possibility of generating various
wave forms and it is used also as a DA converter to command the Kepco
power supply by any kind of computer composed wave forms.
 1.b The software of the measuring system.

The sampling resolution and frequency of the H and B values depend on the
detecting unit:

1. The resolution of the lock-in is the best (1 mV between -10 and +10 V) but the
sampling frequency (28 kHz) is the lowest comparing to the oscilloscope and AD
card. The sampling interval can be varied between 35 sec and 0.1 sec and
32 000 point/cycle can be maximal recorded.

2. The resolution of the oscilloscope is 20 mV/256, but only 1000/cycle can be

recorded with a sampling frequency of 1 MHz.

3. The sensitivity of the AD card is 2.5 V/4096 and the sampling frequency is
150 kHz.

The 3 AD converters (see the 1, 2 and 3 routes on the fig. 1) can be optimised
for different measuring tasks: For real quasi DC measurements (very low frequencies,
below 0.01 Hz) the AD converter of the lock-in is the best. At larger frequencies the
AD converter of the oscilloscope can be used exploiting the fact that the
measurement can be monitored and checked before processing the measured data.

Correspondingly, 3 different software was prepared in DELPHY language and

adapted to the 3 different AD converters
The common feature of all the 3 softwares are :

I. Excitation
II. Measuring the flux
III. Drawing the hysteresis loop.

The detecting equipments are very sensitive to the variation of temperature, this
is why constant temperature should be kept during the measurements. The parasitic
thermoelectric potential drops and the noise of the amplifier causes a drift which can
be corrected by the software.
 The flow diagram of the measurement is shown in Fig.2.

Reading the data of

the samples

Planning the waveform

of the exciting field

Zero set of the current probe; Set the amplification for

Input the calibration data for Initializing the measuring the oscilloscope; or lock-
the Walker integrator; Instruments in, or the A/D card
Zero set for the drift

Start measurement

Reading the data

Drift correction and

setting the zero level

Plotting the hysteresis loop

and determining the Hc, Br and
Bs values

Saving the data

Fig. 2. : Flow diagram for the quasi DC hysteresis loop

measurements
 3. Measuring setup for frequency dependence of permeability

Sheme of the measuring system is shown in Fig.3:

Sample

Adapter 4274A and GPIB

4285A 82357A
LCR meter Interface
PC

Impedance
analyzer

Fig.3. Measuring system for the permeability spectra

The impedance analyser (Hewlett-Packard 4274A s Agilent 4285A) provides the

equivalent Ls induction and Rs resistance
2
L= 0 . S * N (H)
l

"= ' *
R
L *

where

L: inductance in Henry, R resistance in Ohm

-7
0 : permeability of vacuum = 4.10 Vs/Am
: real part of the permeability
S: cross section (m2)
N: number of turns
l: magnetic path length (m)
: frequency
Using the measured data one can determine the quality factor, Q as a function of
frequency:

' L
Q= " =
R

Some representative measurements

In Fig. 4 the quasi-DC hysteresis loop is shown for a toroidal sample prepared from a
Finemet type nanocrystalline ribbon after a ROUND type heat treatment (540 oC/1h).
The first magnetization (virgin) curve was obtained after a careful demagnetization of
the sample.
B(T)
1.5 Virgin curve and major loop
0.5
Quasi DC f = 0.001 Hz
1.0
0.0

0.5
-0.5
-2 -1 0 1 2
0.0
-20 -15 -10 -5 0 5 10 15 20
-0.5 H(A/m)

-1.0

-1.5

Fig. 4. ROUND type hysteresis lop for a toroidal Finemet sample. In the inset the
resolution of the measurement is shown.
 The permeability spectra for the same sample is shown in the Fig.5.

ROUND Finemet
100000 120
mu' Q
mu'' 100
80000

80
60000
' and ''

60
40000
40

20000
20

0 0

0.1 1 10 100 1000 10000

f(kHz)

Fig. 5. The frequency dependence of the complex permeability and of the quality
factor for a ROUND type Finemet sample

The eddy current frequency limit is ~ 40 kHz, which corresponds to the frequency
whre the imaginary ppart of the permeability has a maximum. The quality factor
drops down to unity above 10 kHz.
The result of a heterogeneous heat treatment can be recognized from the WASP
shape of the hysteresis loop which is partial flattening at small fields due to an
inhomogeneosly induced transversal anisotropyn (see Fig.6.)
1.5

1.0
B(T)

0.5

0.0

-0.5

-1.0

-1.5
-30 -20 -10 0 10 20 30
H(A/m)

Fig.6. Result of partially induced transversal anisotropy: a WASP type hysteresis

loop.
 The heterogeneity of the heat treatment varies from sample to sample as can be seen
on the permeability spectra as well in Fig.7. For small exciting fields the permeability
is decreased compared to the ROUND type homogeneous core and the eddy current
frequency limit is shifted to higher values. The heterogeneity appears in the scatter of
the data for the samples marked with #1 and #2.

35000

f lim = 100 kHz sample #2

30000 f lim = 130 kHz sample #1

25000 #2 mu'
#2mu''
20000
#1Mu'
#1Mu''
' and ''

15000

10000

5000

0.1 1 10 100 1000 10000

f(kHz)

Fig. 7 The permeability spectra for samples having partial induced transversal
anisotropy.