Chapter 6 Experimentation
6.4 AC Susceptibility Measurements
6.4.2 AC Susceptibility Measurements as a Function of Applied Magnetic Field
The focus was to design and implement a working AC susceptometer that could be used to characterise a superconducting specimen (in this case YBCO). AC susceptibility measurements against magnetic field were done to investigate about the grain couplings of YBCO, which is one of the numerous characteristics that can be investigated with an AC susceptometer.
104 6.4.2.1 Experimental setup
The susceptometer together with the YBCO specimen were submerged in a liquid nitrogen bath. As shown in Figure 6.15, the YBCO sample was fixed to an aluminium probe using Apiezon thermal grease. Aluminium was selected because it is non-magnetic and the diamagnetic response of the YBCO sample is high compared to the magnetic response of aluminium. The purpose of this setup was to measure the AC susceptibility response of the specimen tested with respect to magnetic field generated at the primary coil. From susceptibility against magnetic field plots, information about the critical current density can be obtained using a modified version of Bean critical state model [22] and information about the grain coupling.
LakeShore CH 1:Temperature CH 2:Temperature
IO Tech Daqbook 2000
Heater Differential Amplifier
Variac
PT-100 connected toLakeshore Controller
Primary coil Secondary coil
Liquid Nitrogen YBCO Sample Mains Filter
A Ameter
X Y Z
Aluminium Probe 50 ohm
resistor
Reference Signal
Model 336 Temperature Controller
Figure 6. 15 AC Susceptibility setup at constant temperature for characterisation.
105
The liquid nitrogen bath kept the experiment at a constant temperature of 77.0 K and the magnetic field at the primary coil was varied by altering the current input to the primary coil. To generate the current, a variac together with a mains filter to filter high harmonics, were used. The maximum magnetic field produced was about 20 mT (estimated analytically from the current driving the primary coil generated by the variac). The resolution of the variac was improved by connecting a 50 Ω high power rating resistance in series with the variac and the primary coil as shown in Figure 6.15.
At the time this research was conducted, the material science laboratory was not equipped with hall effect sensors to measure magnetic field. So, an alternative way was developed to measure magnetic field generated at the primary coil. The „empty‟ balanced secondary coil was used as a sensor to measure the magnetic field at the primary coil. In fact, even though the values for magnetic field measured were not very accurate, that was not a serious issue as long as the measurements were consistent – initially we were looking for trend changes. The sensor was calibrated at 77.0 K (in liquid nitrogen bath) and its repeatability was accessed (refer to Appendix D for calibration curve). The results were very reliable showing good repeatability. After each experiment, the sensor was recalibrated at 77.0 K. The calibration curves agreed perfectly with each other. No adjustment of the gains of the differential amplifier was required.
Since the magnetic field inside the primary coil changes with position or distance along the coil‟s interior, the secondary coils were ensured to remain at the same position inside the primary coil for each experiment. The secondary coils were temporarily sealed during experiment to prevent them from moving or vibrating during experiments. If movements or vibrations occurred, this could have corrupted the experiments carried out.
The voltages induced at the secondary coils were fed to the inputs of the differential amplifier for balancing and amplification purposes. The output from the amplifier X (input voltage at the empty secondary coil) and amplifier Z were fed to the IOTech Daqbook 2000 card (operated at a reference voltage of resolution). The values output at X were processed by DASYLab to measure the magnetic field generated and the values from Z was processed by the software-based lock-in amplifier implemented in DASYLab to measure the real and the imaginary voltage components from which and values of the sample
106 could be estimated .
The Lake shore module 336 was used to measure the temperature of the aluminum probe and the liquid nitrogen. It was also used to regulate the temperature during the hydrogen
„annealing‟ experiment.
6.4.2.2 Annealing Experiment
After each magnetic experiment „run‟, the specimen was subjected to „annealing‟
experiment under zero magnetic field. The PT-100 thermometer was positioned next to the sample and the nichrome heater was brought closer to the sample. The nitrogen was allowed to evaporate and nitrogen/cold air having a temperature of about 90.0 K existed inside the vessel.
The sample was maintained in the cold air/nitrogen vapour and the Lake shore 336 temperature controller was used to regulate the temperature to an „annealing‟ temperature above 90.0 K not exceeding 240 K, for not more than 5.0 minutes (details of „annealing‟ temperatures and time are given in Chapter 7).
The aim of the „annealing‟ experiment was to allow the hydrogen atoms to diffuse to grain boundaries in the samples‟ lattice with the aim that they might diffuse to places that may relieve stresses in the material‟s lattice at grain boundaries. The „annealing‟ experiment was done under cryogenic temperature above the critical temperature to allow the hydrogen to diffuse slowly in a controlled manner into the material‟s lattice. Gas such as hydrogen has a high diffusivity and is in motion at any temperature (apart at absolute zero) [70]. The hydrogen experiment was done with the philosophy that the H2 molecules would be collected at grains boundaries and to relieve the stresses at the dislocations. The „annealing‟ experiment was done to identify the correct temperature that would be enough to move mobile H2 molecules around but once the H2 molecules are “stuck” at the dislocations, there would be not enough energy to “unstick” them.
107 6.4.2.3 Experimental procedures
The magnetic field was varied by changing the voltage from the variable AC supply.
The magnetic field and the relative AC susceptibility were logged by a computer through DASYLab interfacing. The relative imaginary AC susceptibility were determined from which the grain connections in a sample could be characterised after successive hydrogen doping.
The magnetic field was manually increased up to a magnetic field of about 20 mT. This magnetic field was generated by a current of about 0.7 A. Joule heating was minimized since the primary coil was operated under cryogenic conditions. A magnetic field of 20.0 mT was enough to characterize the intergranular coupling of bulk YBCO specimens.
The following summarises the experiment procedure:
1. The AC susceptibility response of the alumium probe without the superconducting specimen (in the nitrogen bath) was logged versus magnetic field by the IO Tech Daqbook 2000 module (an „empty run‟).
2. The sample, attached to the aluminium probe placed inside the susceptometer, was submerged into liquid nitrogen as shown in Figure 6.15.
3. The magnetic field at the primary coil was manually varied from the variac making sure to record at least 50 different values of magnetic field well scattered between 0 to 20 mT .
4. The values of AC susceptibility and magnetic field were measured and logged by IO Tech Daqbook 2000 module, interfaced via DASYLab software.
5. „Annealing‟ experiment was done under zero field.
6. Steps 2 to 5 were repeated on the same sample but each time the „annealing‟
temperature and time were randomly varied.
7. The sample was then removed from the vessel after four „annealing‟ runs and allowed to dry before undergoing hydrogenation. The hydrogenated sample was then subjected to steps 2 to 5 again before undergoing the next hydrogenation.
Steps 2 to 5 were repeated until the sample stop superconducting.
108