Internship Report:

Magneto-transport study of
superconducting materials

By
Koustav Chandra
Dept. of Physics& Astronomy
National Institute of Technology, Rourkela

Under the guidance of

Dr. C.S. Yadav

School of Basic Science
IIT Mandi

Abstract:
Magneto-transport study were performed on FeTe0.6Se0.4 sample for determining
its low temperature electrical and magnetic properties. A transition in its
properties were observed at 12.75 K, thus marking its superconducting phase
transition. The upper critical field of Hc2 (0) =42.010 K was found from its
electrical properties. The magnetic susceptibility of the material shows the
material to be a bulk superconductor with the superconducting volume fraction
of 83.4 %. The polycrystalline samples of another superconductor PdTe2 were also
prepared in the light of further investigation. Also a brief theoretical study of the
related subject matter is provided for a complete understanding.

Acknowledgment
Dated: 21st Feb, 2015

It is not possible to prepare a project report without the assistance & encouragement of
other people. This one is certainly no exception.
On the very outset of this report, I would like to extend my sincere & heartfelt obligation
towards all the personages who have helped me in this endeavor. Without their active
guidance, help, cooperation & encouragement, I would not have made headway in the
project.
I am ineffably indebted to Surender Lal Sharma for conscientious guidance and
encouragement to accomplish this assignment.
I am extremely thankful and pay my gratitude to my guide and instructor Dr. C.S.
Yadav for his valuable guidance and support on completion of this project in its
presently.
I extend my gratitude to IIT Mandi for giving me this opportunity.
I also acknowledge with a deep sense of reverence, my gratitude towards my parents
and member of my family, who has always supported me morally as well as
economically.
At last but not least gratitude goes to all the members of the Low Temperature
Physics Lab who directly or indirectly helped me to complete this project report.
Any omission in this brief acknowledgment does not mean lack of gratitude.
Gracias
Koustav Chandra
Dept. Of Physics & Astronomy
NIT Rourkela

Sec A: Introduction
When in the year 1911, Kammerlingh Onnes found the perfect conductivity in mercury
(Hg) at 4.18 K, a new wing of Condensed Matter Physics cropped up known as the
Superconductivity. Over the years a lot of developments has taken place in the subject. For
the benefit of the readers a brief account of the necessary stuff related to the subject matter
is provided to suffice the theoretical understanding required to appreciate the results of the
experiments discussed in the report.
The name superconductor was awarded to those few compounds, alloys and elements
because of the vanishing resistance when cooled below a specific temperature thus marking
a phase transition from normal state to super-conducting state. The temperature
corresponding to it is named as the critical temperature (Tc).

Fig A-1: Picturing the difference in between normal materials and superconductors (source:
cyberphysics.co.uk)

Further a superconductor has an amazing property of mocking a perfect diamagnet;

meaning it repels all the applied magnetic flux lines. When resistance falls to zero, a current
can circulate inside the material without any dissipation of energy. Secondly, provided they
are sufficiently weak, external magnetic fields will not penetrate the superconductor, but
remain at its surface. The phenomenon named as Meisnner Effect after the first observer,
German physicist Walther Meissner. A sketch marking the difference in perfect
conductivity and superconductivity is shown in fig. A-2.
At any given temperature, T < Tc, there is a certain minimum field Bc (T), called the
critical field, which will kill superconductivity. It is found (experimentally and theoretically)
that Bc is related to T by the equation:
Bc = B0 [1 (T/Tc) 2], where B0 is the asymptotic value of the critical field as T 0 K.

Fig A-2: Explaining Meisnner Effect, in superconductor where the magnetic flux is completely
expelled out of the bulk material when cooled below Tc unlike the perfect
conductor.(Source:physics.ox.ac.uk)

The superconducting state can be destroyed by a rise in temperature or in the applied

magnetic field, which then penetrates the material and suppresses the Meisnner effect.
From this perspective, a distinction is made between two types of superconductors. Type-I
materials remain in the superconducting state only for relatively weak applied magnetic
fields. Above a given threshold, the field abruptly penetrates into the material, shattering
the superconducting state. Conversely, Type-II superconductors tolerate local penetration
of the magnetic field, which enables them to preserve their superconducting properties in
the presence of intense applied magnetic fields. This behavior is explained by the existence
of a mixed state where superconducting and non-superconducting areas coexist within the
material. For the type-II superconductors there are 2 associated values of critical magnetic
fields as shown in fig. A-5. The Hc2 is called upper critical field and lower one Hc1 as lower
critical field.

Fig A-3: Critical field plotted against temperature for various type-I superconductors (source:
web.mit.edu/8.13)

To account for an explanation for these effects, the London brothers marked that
superconductivity was due to a macroscopic quantum phenomenon in which there was long
range order of the momentum vector. This implies condensation in momentum space. Fritz
London also realized that it is the rigidity of the superconducting wave function which is
responsible for perfect diamagnetism. The London equation,
J = -nq2A/m
was developed from Maxwells equations. This leads to an equation for the magnetic
field B (= A) of the form
2B = B/ 2
where is the London penetration depth. The demarcates the extent to which
the external field can penetrate within the superconductor (fig.A-4).

Fig A-4: Explaining the fall in Magnetic flux lines inside the superconductor (B=Boexp (-x/))

Unsatisfied by this explanation, Ginzburg proposed an extended version of Landau

theory arguing over the fact that the superconductivity of the sample is due to a phase
transition from normal to a superconducting state. From the free energy equation:
Fs = Fn + d3r [a (T)|(r)|2 + b2|(r)|4 + 1/2m | i (r) + 2eA(r)|2+ (B(r)B0)2/20]
where (r) = 0e i(r) is the complex order parameter and B0 is the applied field, he arrived
at
2 = / 2
where = 2/2m|a(T )| using the fact that near Tc we can neglect the b2 term because
0.The coherence length, gives the measure of the distance within which the
superconducting current carrier concentration cannot change drastically in a spatiallyvarying magnetic field. The real significance of the 2 length parameters are realized when
one takes the ratio = /. If < 1/ 2, we have a type I superconductor. If > 1/ 2, we
have a type II superconductor.

(A)
(B)
Fig A-5 :( A) For type-I superconductor, (B) For type-II superconductor

However none of these theory are rivaled when compared to the celebrated BCS theory.
The trio American physicist, put forward the fact that interaction between electron and
phonons(quantized lattice vibrations) causes a reduction in Coulombic repulsion between
electrons below Tc ,to provide a net long range attraction to form Bose-particles with
opposite momentum and spin known as Cooper pairs. Since they are bosons they have the
privilege of occupying the same quantum state. At T<Tc these cooper pairs condense into a
single quantum state accounting for zero resistance.
The quenching of superconductivity occurs when due to the added energy above Tc,
the Cooper pairs can no longer withstand the increasing repulsion thus breaking up into
constituent electrons.

(A)

(B)
(C)
Fig A-5: Discussing the formation of Cooper pairs. (A),(B) & (C)Shows how an approaching electron
distorts the ions in its neighborhood thus providing a region where the incoming electrons get
entrapped followed by another electron when it nears into the decreased positively charged
region(Source: physics.ox.ac.uk )

However the BCS theory failed when high temperature superconductivity came into
the scenario for BCS theory roughly predicted that one cant obtain superconductors
beyond a certain temperature. To fill in many theories are still being proposed but in vain.

Experimental Setup
Sec B: PPMS-Dynacool (Physical Property Measurement System)
The quantum design PPMS system is a cryogen-free instrument that helps in measurement
in physical property of the sample under investigation. Using this highly sophisticated
device measurement of resistivity against temperature was figured out. Since the sample
had undergone some form of corrosion, errors in the measurement was expected.

Resistivity Option
Since only resistivity was measured using this apparatus so a brief overview of the
Resistivity option for the device is provided. The Resistivity option can report resistance
as well as resistivity, conductance, and conductivity. Resistivity sample pucks (Fig B-2)
have four contacts one positive and one negative contact for current and voltage for
each user bridge board channel to which a sample may be conventionally wired. Up to
three samples may be mounted on a Resistivity puck, so the Resistivity option may
measure up to three samples at one time.

Fig B-1: PPMS-Dynacool system

Sample Mounting
The sample with dimension of just 2.83 mm and area of cross section of 0.36 mm 2 was
quite an uphill battle when it came to mounting for a greenhorn like me. So under the witty
advice of my guide the sample was stuck to a thin piece of mica sheet using GE varnish
along with 4 copper wires stripped at their ends only before mounting on Resistivity Puck
(Fig. B-2).
One of the end of the wires were then stuck to the sample using silver paste to ensure
perfect contact. The other ends of the wires were then soldered to the puck, and then scaled
on the Sample Wiring Test Station.

(A)

(B)

Fig B-2 :( A) Resistivity Puck with the 3 channels shown (B) A sketch of its birds eye view.

After some measurement on the puck, to ensure near perfect contacts using multimeter the
sample was mounted into the PPMS system. The PPMS DynaCool uses an innovative style
of sample mounting by providing at the bottom of the sample chamber a 12-pin connector
pre-wired to the system electronics. This connector allowed to plug in a removable sample
insert (or puck) for convenient access to electrical leads and sample mounting.

Why 4-probe measurement used?

Using four wires to attach a sample to a sample puck greatly reduces the contribution of
the leads and joints to the resistance measurement. In a four-wire resistance measurement,
current is passed through a sample via two current leads, and two separate voltage leads
measure the potential difference across the sample (Fig B-9(B)). The voltmeter has a very
high impedance, so the voltage leads draw very little current. In theory, a perfect voltmeter

draws no current whatsoever. Therefore, by using the four-wire method, it is possible to

know, to a high degree of certainty, both the current and the voltage drop across the sample
and thus calculate the resistance with Ohms law.

10

Sec C: MPMS-3(Magnetic Property Measurement System)

The MPMS-3 system is a Squid (Superconducting Quantum Interference Device)
magnetometry device that provides three possible measurement modes: DC Scan Mode,

VSM Mode and AC Susceptibility Mode. In the report an outlook of the DC mode is
given for it was the one used in the measurement procedure.

Sample Packing
The cleaned sample was then stuck to brass half-tube sample holder (fig. B-1) using GE
low temperature varnish after proper cleaning of the sample holder using ethanol and cotton
buds. It was then centered using sample mounting station to ensure it lies in about 66mm.

Fig C-1:- Brass Half-tube Sample Holder

The sample is mounted in a sample holder that is attached to the end of a rigid sample
rod. The sample rod was then introduced into the sample space through a special type of
double seal (called the lip seal) designed to allow the rod to be actuated by a drive
mechanism located outside of the chamber. Since I was using the DC Mode of measurement,
I had to do the process of centering in the DC mode. This is done to ensure the sample is
present in the surrounding of the super-conducting magnetic coil where it is the strongest.

11

Fig C-2:- Graph showing about the centering of the sample.

Fig C-3: DC Centering Measurement and Measured SQUID Voltage Response

Measurements
Magnetic Properties
Measurement System)

measurement

using

MPMS-3(Magnetic

Property

As cited earlier the measurements taken was in the DC Mode using which measurements

12

of magnetic moment of sample against an applied field of 10 Oe at various temperature and

variation of magnetic moment against magnetic field at 2K temperature was measured. To
do so a sequence suggesting the former was run in the MPMS Multi-Vu software. MPMS
Multi-Vu integrates all system operations into one versatile and easy-to-use Windows 7
interface. The sequence was programmed in a fashion after the proper set of measurement
algorithm was known (Appendix-B).

Fig B-3:-The MPMS-3 system

13

Sec D: Experimental Analysis

For Resistivity vs. Temperature

0.014
0.012
0.010

(cm)

0.008

FeTe0.6Se0.4

0.006
0.004
0.002

1-10T

0.000
0

10

12

14

16

18

T(K)

Fig D-1: Temperature dependence of the resistivity of FeTe0.60Se0.40 single crystals, measured in the
magnetic fields (from right to left) H = 0, 1, 2, 3, 4, 5, 6, 7, 8, 9 & 10T

From the experimental data it was confirmed that the sample shows a superconductive
phase transition at 12.5K unlike the expected value of 14.5K. Further as observed from the
graph B-10 it can be seen that the sample shows a gradual conversion into superconductive
phase transition rather than the sharp transition expected as usual. The error can be
accounted to the failure on my part to make perfect silver point contacts in the sample.
In the Fig. B-11, a H-T phase diagram was plotted for the crystals, corresponding to
the temperatures where the resistivity drops to 90% of the normal state resistivity n, (where
n is taken at temperature T = 16 K) and 50% of n, where the two are labeled as T onset and
T mid respectively. Using these data, the value of Hc (0), critical magnetic field at 0K using
the formula:
Hc=Hc (0)[1-(T/Tc)2]
which was found to be at 20.95T for T onset and 11.06T for T mid using the value of
temperatures at field of 8T (arbitrary). To get a better result of the values the Werthamer
HelfandHohenberg (WHH) formula:
Hc2 (0)=-0.693(dHc2/dT)Tc
was used. Using this formula a value of 28.152T for T mid and 42.010T for T onset.

14

14

FeTe0.6Se0.4

12

T onset

H(T) (T)

10
8

T mid

6
4
2
0
0

10

11

12

T(K)

Fig D-2: The upper critical field versus temperature phase diagram is shown for the points where
electrical resistivity drops to 90% &50% of n, shown by T onset and T mid.

For Magnetic Moment vs Temperature measurement

The temperature dependence of magnetic moment obtained from the MPMS3 was used in
getting an idea about temperature dependence of susceptibility which was graphed against
temperature using OriginLab Origin 9.01b.
The Magnetic moment dependence on temperature plot as shown in fig. (B-4) exhibits a
transition of the sample from its normal state to its superconducting state at a temperature
of about 12.75 K. The error exhibited while measurement could have been due to oxidation
of the sample.

15

0.00005

0.00000

FeTe0.6Se0.4

M(emu)

-0.00005

-0.00010

-0.00015

-0.00020

-0.00025

-0.00030
0

10

15

20

25

T(K)

Fig D-3: Magnetic moment dependence on temperature at 10Oe field

To investigate upon the fact a plot of 4 vs. T using the data obtained and the
electrodynamics relations:
M=H
B=H (1+4)
From the plot in fig. (B-5) we figure out the fact that there is a gradual drop and not an
abrupt fall as expected from the theoretical data and previous experimental measurements
as performed by other individuals.
0.4

0.2

-4(emu/gm-Oe)

0.0

FeTe0.6Se0.4

-0.2

-0.4

-0.6

-0.8
0

10

15

20

25

T(K)

Fig D-4: 4 vs. T at 10Oe field

Further as clearly visible from the plot the transition does not stop at 1.8 K, the point beyond

16

which the MPMS-3 used cant cool. So we can surmise that the sample which had been
boxed up for so long had been oxidized to a certain extent that has led to it unveiling its
ferromagnetic property even at that low temperature instead of undergoing a phase
transition into diamagnetic state as expected from Meissner effect on superconductor.
DC Moment Fixed Ctr (emu)

M(emu)

0.04

0.02

0.00
-60000

-30000

30000

60000

H(Oe)
-0.02

FeTe0.6Se0.4

-0.04

Fig B-6: M-H plot at 2K

For Magnetization vs. Magnetic Moment

To determine the dependence of the duo the M-H algorithm was run in the MPMS-3 system
and using the obtained data points a trace was made. As shown in the fig. (B-6) the line
scatter diagram shows a hysteresis curve of a ferromagnetic sample rather than an expected
a mirror-anthill illustration. So a further confirmation about the sample rusting away with
time can be uttered.
To extract a further evidence an M-T measurement at higher applied magnetic field is
done and from its field cooling plot as manifested in the fig. (B-7) a conclusion can be
drawn that the specimen under investigation has been oxidized thus affecting its property.

17

0.010

0.005

M(emu)

0.000

FeTe0.6Se0.4

-0.005

-0.010

-0.015

-0.020
0

50

100

150

200

250

300

T(K)

Fig B-7: M-T plot at 100Oe field

Conclusion
So, the data obtained and the plots displays a lot of erroneous results caused primarily due to
corrosion of FeTe0.6Se0.4, the sample under investigation. Yet a lot of experience gained at the
end of the day on the subject concerned. An experimental outlook on how the magnetic
properties of the sample undergoes a turmoil when cooled beyond its transition temperature is
learned in first hand, an experience to ponder upon.

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Sec E: Preparation of bulk superconducting

compounds
Synthesis of bulk PdTe2,
Poly-crystalline bulk PdTe2 compound was synthesized via solid state route. For the
preparation of 1gm of sample 0.2942 gm. of Pd(99.9%-3N) and 0.7057gm of Te(99.99%4N) from Sigma Aldrich was mixed and grounded to ensure a molar ratio of 1:2 using
mortar and pestle for a period of over 1 hour to ensure they form a finely mixed powder.
The well mixed sample was then made into a pellet using a clean pellet press by applying
a pressure of 75kg/cc. The pressed pellets were then sealed off inside an evacuated quartz
tube(<10-3 torr) and put into a tube furnace immediately for heating at 850oC at the rate of
100oC/h for 24h before cooling it off at 500oC to which it was dropped at the rate of 50oC/h
until it was finally stopped.

Fig E-1: Mortar with pestle

The shiny black sample was taken out from inside the quartz tube, grounded into fine
powder, pelletized and kept back vacuumed and sealed inside the tube furnace following
the same sequence as earlier for sintering. The dense, shiny gray one-piece was taken out,
wrapped in a butter paper for further experiments to be performed upon.

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Fig E-2: Lindberg Blue M TF55035A-1 Tube Furnace

Synthesis of bulk Pd1Se1

Poly-crystalline bulk PdSe compound was prepared via solid state reaction. A mixture of
the ingredients Pd (99.9%-3N) and Se (99.99%-4N) from Sigma Aldrich in 1:1
ratio(Amount of Pd=0.5741gm & amount of Se=0.4259gm for 1 gm. of sample) was
pelletized by 65gm/cc pressure and were then sealed in an evacuated quartz tube(which
was vacuumed to 10-6 torr using diffusion pump). The sealed tube along with its contents
were then kept in a tube furnace at a temperature of 750oC with a heating rate of 100oC/h
for a period of over 24h and then cooled to 500oC @ 50oC/h until the furnace was switched
off. The obtained sample was then ground, pelletized and sintered at the same temperature
to give the final product which was then made available for further experiments to be
performed upon.

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Appendix-A
The resistivity of the sample was carried out based on the following algorithm.
For R-T Measurement
1.
2.
3.
4.
5.

Set Temperature at 2 K @ 1 K/min uniformly without overshoot and resistivity was

measured at every point.
The temperature is increased 20 K @ 0.2 K/min uniformly without any overshoot and
resistivity is measured at every point.
A field of 1 T was set and the temperature was dropped to 2 K.
The temperature is increased 20 K @ 0.2 K/min uniformly without any overshoot and
resistivity is measured at every point.
The above 2 steps are iterated for magnetic fields of 2,3,4,5,6,10 T

Appendix-B
The measurements of magnetic-properties were carried out based on these set of
algorithms.

Measurement Algorithm
For measurement of M-T at 10Oe.
6.
7.
8.
9.
10.
11.
12.
13.
14.
15.

Set Temperature at 300K @ 12K/min in Fast Settle mode and wait for 10 s.
Set Magnetic Field at 1T at 100 Oe/s in Linear Stable mode and delay for 30s.
Next set Field to 0Oe @ 100 Oe/s in Oscillatory mode and wait for 30s.
Set temperature to 10K @ 12K/min in fast settle mode and pause for 30s before further
action
Next set to 2K @ 1K/min in fast settle mode and wait for 60s.
Set Field to 10Oe @ 10 Oe/s in Linear Stable mode and hold for 10s.
DC Moment was measured against temperature from 2 K-25 K in sweep continuous
mode.
Set temperature to 2K @ 1K/min in fast settle mode and pause for 60s.(Field Cooling)
DC moment was next measured against temperature from 2 K to 25 K in sweep
continuous mode.
The field is next set to 0Oe @ 10Oe/s in Linear Stable mode followed by setting
temperature to 300K to complete the measurement sequence.

For measurement of M-H at 2K.

1.
2.
3.
4.

Set Temperature at 300K @ 12K/min in Fast Settle mode and wait for 10s.
Set Magnetic Field at 1T at 100 Oe/s in Linear Stable mode and delay for 30s.
Next set Field to 0Oe @ 100 Oe/s in Oscillatory mode and wait for 30s.
Set temperature to 10K @ 12K/min in fast settle mode and pause for 30s before further

21

action.
5. Next set to 2K @ 1K/min in fast settle mode and wait for 60s.
6. MPMS3 Moment (DC) vs Field 1 Quadrant 0 to 10000 Oe Step Linear Auto-tracking
was done.
7. MPMS3 Moment (DC) vs Field 1 Quadrant 10500 Oe to 50000Oe Step Linear Autotracking was run next to it.
8. MPMS3 Moment (DC) vs Field 1 Quadrant 50000 Oe to -50000Oe Step Linear Autotracking was run next to it.
9. Before taking out the sample the field was set to 0 Oe @ 10oe/s and re-setting
temperature to 300K @ 12K/min thus completing the sequence algorithm.

22

Bibliography
1.

Prof.

G. Rangarajan,

Lectures

on

Condensed

matter

Physics,

nptel.ac.in/courses/115106061

2.
3.
4.

Charles Kittel, Introduction to Solid State Physics(8th edition) ,chapter-10

superconductivity
Upper critical field, lower critical field and critical current density of FeTe0. 60Se0.
40 single crystals(CS Yadav, PL Paulose)New Journal of Physics 11 (10), 103046
PdTe: a 4.5 K type-II BCS superconductor(B Tiwari, R Goyal, R Jha, A Dixit, VPS
Awana)Superconductor Science and Technology 28 (5), 055008

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