IIT Mandi Low Temperature Physics Laboratory

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

Summer 2015

IIT Mandi Low Temperature Physics Laboratory

Abstract
Magneto-transport study was 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 83.0%. The polycrystalline samples of another
superconductor PdTe2 were also prepared in the light for further investigation. Also, a
brief theoretical study of the related subject matter is provided for a complete
understanding.

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IIT Mandi Low Temperature Physics Laboratory

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. Special thanks to Juhi Pandey for editing
the report and suggesting requisite changes.
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

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IIT Mandi Low Temperature Physics Laboratory

Section 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 diamagnetic

material; 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 Meissner
Effect after the first observer, German physicist Walther Meissner. A sketch marking the
difference in perfect conductivity and superconductivity is shown in fig. A-1.
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.

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Fig A-2: Explaining Meissner 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 Meissner 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 two 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)

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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=Bo exp(-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|(r)|4 term
because 0. The coherence length, gives the measure of the distance within which
the superconducting current carrier concentration cannot change drastically in a
spatially-varying magnetic field. The real significance of the two length parameters is
realized when one takes the ratio = /. If < 1/ 2, we have a type I superconductor. If
> 1/ 2, we have a type II superconductor.

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

However, none of these theory is 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

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beyond a certain temperature. To fill in many theories are still being proposed but in vain.

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Section B: Experimental Setup

B.1 PPMS-DynaCool (Physical Property Measurement System)
The quantum design PPMS system is a cryogen-free instrument that helps in
measurement of 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.

B.1.1 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

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B.1.2 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 four 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 three channels shown (B) A sketch of its birds eye view.

After some measurements 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-2(B)). The voltmeter has a very
high impedance, so the voltage leads draw very little current. In theory, a perfect

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

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

B.2 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.

B.2.1 Sample Mounting

The cleaned sample was then stuck to brass half-tube sample holder (fig. B-3) 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
66 mm.

Fig B-3: 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 DC mode of measurement was used,
the process of centering was done in DC mode. This is done to ensure the sample is
present in the surrounding of the super-conducting magnetic coil where the magnetic field
is the strongest.

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Fig B-4: Graph showing about the centering of the sample.

Fig B-5: DC Centering Measurement and Measured SQUID Voltage Response

B.2.2 Magnetic Properties measurement using MPMS-3(Magnetic

Property Measurement System)
The measurements were carried out in DC Mode with the magnetic moment dependence
on temperature being measured at different temperatures while the magnetization

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dependence on magnetic field accomplished at 2 K temperature. To do so a sequence

suggesting the former was run in the MPMS MultiVu software. MPMS MultiVu
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 C-4: The MPMS-3 system

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Section C: Experimental Results & Analysis

C.1 The dependence of resistance with temperature

0.012

FeTe0.6Se0.4

(cm)

0.008

0.004

1-10T
0.000
4

12

16

T(K)
Fig C-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 12.5 K unlike the expected value of 14.5 K. Further as observed from
the graph C-1 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. C-2, 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 20.95 T for Tonset and 11.06 T for Tmid using the value of
temperatures at field of 8 T (arbitrary). To get a better result of the values the
WerthamerHelfandHohenberg (WHH) formula:
Hc2(0) =-0.693(dHc2/dT) Tc
was used. Using this formula, a value of 28.152 T for T mid and 42.010 T for T onset.

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IIT Mandi Low Temperature Physics Laboratory

15

12

FeTe0.6Se0.4

H(T)

Tonset

Tmid
6

0
6

12

T(K)

Fig C-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.

C.2 Magnetization Dependence with Temperature

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 Origin Lab Origin 9.01b.
The Magnetic moment dependence on temperature plot as shown in fig.C-3 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.

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IIT Mandi Low Temperature Physics Laboratory

0.005

FC

M(emu/gm)

0.000

ZFC

-0.005

FeTe Se

FeTe0.60.6
Se0.40.4
-0.010

-0.015

-0.020
0

10

15

20

25

Temperature (K)

Fig C-3: Magnetic moment dependence on temperature at 10 Oe 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.(C-4) 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.
0.2

FC

-4(emu/gm-Oe)

0.0

ZFC

-0.2

-0.4

FeTe0.6Se0.4
-0.6

-0.8
0

10

15

20

25

Temperature (K)

Fig C-4: 4 vs T at 10 Oe field

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

0.04

M(emu)

0.02

0.00

FeTe0.6Se0.4
-0.02

-0.04
-60000

-30000

30000

60000

H(Oe)

Fig C-5: M-H plot at 2 K

C.3 Change in Magnetization with Applied Magnetic Field

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.(C-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.(C-7) a conclusion can be
drawn that the specimen under investigation has been oxidized thus affecting its property.

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0.010

FC
0.005

ZFC

M(emu/gm)

0.000

-0.005

FeTe0.6Se0.4

-0.010

-0.015

-0.020
0

50

100

150

200

250

300

Temperature(K)

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

Conclusion
The Magneto-transport study performed on FeTe0.6Se0.4 sample for determining its
low temperature electrical and magnetic properties showed a transition in its properties 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 which was quite low as
compared to the expected one. This was because of the poor contact points that was
formed while creating the contacts. Assumption of oxidation of the sample can be
guessed to form ferromagnetic compound. The magnetic susceptibility of the material
shows the material to be a bulk superconductor with the superconducting volume fraction
of 83.0%.

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Sec D: Preparation of bulk superconducting compounds

D.1 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 0.7057 gm 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 75 kg/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 D-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 D-2: Lindberg Blue M TF55035A-1 Tube Furnace

D.2 Synthesis of bulk PdSe

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 65 gm/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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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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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.
For measurement of M-T at 10Oe.
1.
2.
3.
4.
7.
8.
9.
10.
11.
12.

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

For measurement of M-H at 2 K.

1. Set Temperature at 300 K @ 12 K/min in Fast Settle mode and wait for 10 s.
2. Set Magnetic Field at 1 T at 100 Oe/s in Linear Stable mode and delay for 30 s.
3. Next set Field to 0 Oe @ 100 Oe/s in Oscillatory mode and wait for 30 s.
4. Set temperature to 10 K @ 12 K/min in fast settle mode and pause for 30 s before
further action.
5. Next set to 2 K @ 1 K/min in fast settle mode and wait for 60 s.
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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 50000 Oe Step Linear
Auto-tracking was run next to it.
8. MPMS3 Moment(DC) vs Field 1 Quadrant 50000 Oe to -50000 Oe Step Linear
Auto-tracking was run next to it.
9. Before taking out the sample the field was set to 0 Oe @ 10 Oe/s and re-setting
temperature to 300 K @ 12 K/min thus completing the sequence algorithm.

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