EP401P – Engineering of Instrumentation

Lab Report - 3
Experiment - RT
Rashmi, B19218
Group - D

Objective: To measure the electrical resistivity of a sample for temperatures in the range of 80-450K.

Apparatus: Physical Quantities Measurement System (PQMS) which includes the following:

1. Cryostat (for maintaining the low temperature)

Working Principle:

For measurement of the resistivity of the sample for varying temperatures, we need a
temperature-controlled environment.

A cryostat is an apparatus for maintaining very low temperatures. It has double-walled insulation for
improved temperature control. Here we have used Liquid Nitrogen as a Cryogenic liquid. Liquid N2 has a
boiling point of 77K.
 Fig 2: Cryostat

For cooling the sample to 80K, the outermost chamber of the cryostat is filled with liquid N2. The inner
side of the outer chamber is filled with Helium gas. Helium has 4.21K boiling point, less than liquid N2.
Therefore, it is used as an exchange gas which creates a good thermal contact either between the sample
and the heater or the heater and the environment. Helium is flushed into the heater chamber (outer) and
the sample chamber (inner). The sample is placed inside the sample chamber on the sample rod using the
4-probe insert. In this way, the sample temperature starts decreasing by making a connection with liquid
nitrogen using helium gas. We can achieve a temperature range of 77K (-196°C) to 450K (+177°C) by
using liquid nitrogen and exchange gas.

Fig 3: The front and rear view of the source-meter

For temperature measurement and control, a Pt100 sensor is used. Pt100 is a resistance temperature
detector (RTD) which changes its resistance with the varying temperature. It is made of Platinum and
gives 100 Ohm resistance at 0°C. Resistance is calculated using Ohm's Law, 𝑅 = 𝑉/𝐼 and then resistivity
is calculated using sample dimensions. 4-Probe Insert is used for mounting of the sample. In this, two
probes are for current source and other two are for measuring the voltage. These probes are connected to
the I-V source and measurement device which consists of a microprocessor controlled electronic unit and
its associated driver and utility software. The device has one output channel to supply DC voltage or DC
current and 3 input channels to measure the supplied current, driving voltage and external voltage. This
system is connected to the computer which has Data acquisition and control software, Qrius for easy
control of all experimental parameters. It gives real time measurement, recording and plot of physical
quantities like Resistivity versus Temperature. It has user-selectable temperature, current, and voltage
sweep rates.

Fig 5: 4-Probe Insert

Once the sample is cooled to 80K, then we have to heat the sample. For heating, the sample should not be
in contact with liquid nitrogen. Therefore, we will evacuate helium from the heater chamber and create a
vacuum, especially for temperatures above 200K, so that all the heat goes to the sample only. For
temperatures below 200K (-73°C), good thermal contact is needed between the liquid nitrogen and the
sample, so exchange gas should be present in both the sample and heater chambers.

For evacuation and flushing of the chambers, there are 4 independent on/off valves. 2 for the heater
chamber and the other two for the sample chamber. For evacuation of the heater chamber, we will open
the valve of the heater chamber which is connected to the rotary pump i.e. heater chamber evacuation
port. The pump used is the double-stage Rotary Pump and is connected to the Pirani Gauge with a readout
unit. Pirani gauge can measure the pressure for low vacuum i.e. 10-3 mbar. On opening the port, the
pressure on the Pirani gauge will rise and then after some time, it will fall again due to the rotary pump in
action.

The sample chamber (inner chamber) has a heating coil around it which is powered by the temperature
control unit. It helps the sample to heat up to 450K. The heater has winding of non-magnetic nichrome
and heater power is of 40 Watt. In this way, the sample gets heated up and we can get the corresponding
temperature-resistivity plot on the computer screen using the installed software.

While handling this system, precautions must be taken. Liquid nitrogen can be hazardous so don't come in
direct contact with it. Do not cool the cryostat if the air is present in any of the chambers because this will
lead to the condensation of moisture present in the air and may cause deterioration inside.

After completing the experiment, the system should be shut down by following the proper procedure.
First, take out the cryostat and cut off the connections to the pump. Open the evacuation ports and make
sure that there should be some exchange gas in both chambers. Wait for the system to get to room
temperature. Sample heater can be used for fast heating. Open the release valve to let air in. After that, the
sample insert can be removed safely. Do not leave the insertion port open. At last, close all the valves and
switch off all the power supplies.
Results: In this experiment, we took measurements for 10mA current and 5V voltage with the rate of
2K/min for a maximum temperature of 300K. The following graphs are obtained for Mn3ZnC sample and
above current-voltage values.

1. In the resistance versus temperature graph, it can be seen that the resistance of the sample
(Mn3ZnC) is increasing with the temperature. Temperature values in the graph are from 80K to
142K.
2. In the temperature vs time graph, there are two line graphs, one for sample temperature and the
other for heater temperature. It can be seen that the sample temperature lags the heater
temperature.
Conclusion: In this experiment, we learn about the temperature dependence of the resistivity of the
sample. We understand the working of the cryostat. We learn that by using the cryogenic liquid (liquid
nitrogen) and exchange gas (Helium) in the cryostat, one can provide a temperature-controlled
environment to the sample. Resistivity measurement for different temperatures is done using the
four-probe insert and the temperature sensor. This whole mechanism is controlled by the electronic units
known as I-V measurement and temperature controller units which are further connected to the Qrius
software in the computer.

Reference:

http://quazartech.com/xplore-1-2/