Using the Spark Plasma Sintering System for Fabrication of Advanced Semiconductor Materials
Abstract
:1. Introduction
- An example of compacting grounded arc-melted materials with an SPS device (research performed before SPS upgrade).
- An original approach to an SPS system extension, allowing a detailed measurement of the sintering system.
- An approach to use an SPS device as an SHS reactor, which is possible due to multi-point parameter measurement.
- Annealing temperature—the highest maintained temperature over a process.
- Pressure—uniaxial pressure applied to the sample during the sintering process.
- Dwell time—sintering temperature holding time.
2. Materials and Methods
2.1. Materials
- Arc-melted semiconductor materials, HCST-x () for x = [0, 0.01, 0.02, 0.05, 0.10] and HZNSS-x ( (half-Heusler) for x = [0.01, 0.02, 0.05])
- Bismuth telluride-based materials synthesized by SHS technique materials (PBSTS-xxs). The reference material (PBSTq), fabricated inside a quartz vacuum tube, is also included for comparison.
Identification | Chemical Formula | Processing Method |
---|---|---|
HCST-01 | AM, SPS | |
HCST-02 | AM, SPS | |
HCST-05 | AM, SPS | |
HCST-10 | AM, SPS | |
HZNSS-01 | AM, SPS | |
HZNSS-02 | AM, SPS | |
HZNSS-05 | AM, SPS | |
PBSTq (pREF) | Melting, SPS | |
PBSTS-01s | SHS, SPS | |
PBSTS-06s | SHS, SPS | |
PBSTS-12s | SHS, SPS | |
PBSTS-18s | SHS, SPS |
2.2. SPS System
2.3. Arc Melting of HCST Cobalt Triantimonide and HZNSS Half-Heusler
- Cobalt triantimonide: T = 650 °C, P = 50 MPa, time = 15 min.
- Half-Heusler: T = 1000 °C, P = 50 MPa, time = 25 min.
2.4. Process Data Collection and Device Upgrade
- Acquisition of power supply parameters (voltage and current), allowed us to gain information about delivered power and, in some cases, the resistance of the sintering system.
- Constant stabilization of the pressing force. A hysteresis regulator was used previously, causing lower reproducibility of the pressure value over time. Now, a 5-way proportional valve driven by a quasi-logic controller is installed, resulting in high stability and reproducibility of the pressure.
- Up to 6 thermocouples (labeled as #1T1, #1T2, #2T1, #2T2, #3T1, #3T2) can be connected to determine the temperature gradient across the sample up to 950 °C. Figure 3 presents an example of thermocouple placement, where #1T1 is a process control thermocouple, and other sensors collect temperatures from different parts of the system allowing us to determine the temperature gradient. Before the upgrade only one temperature was acquired.
- Above 500 °C, infrared temperature measurement can be used. The infrared curve shows when the temperature exceeds 500 °C (Figure 5).
2.5. SHS
- Heating the system to 375 °C and maintaining this temperature for 60 s. This step realizes the first, exothermic stage of materials synthesis (SHS occurs during the first initial heating).
- Heating the system to 475 °C and maintaining this temperature for 300 s. This step was applied to fully react reagents and homogenize material.
2.6. XRD Diffraction
2.7. Thermal and Electrical Parameter Characterization
3. Results
3.1. Thermoelectric Properties of Arc-Melted and SPS-Processed Materials
3.2. SHS Results
3.2.1. Analysis of the SHS Stages
- PBSTS01sr—The material after the homogenization process in an automatic mortar. This is the analysis of the phase composition, in addition to confirming the presence of pure elements, i.e., tellurium (00-004-0555), antimony (00-077-3384) and bismuth (01-078-6571).
- PBSTS01sp—The fragmented material after synthesis SHS consisted mainly of the phase (01-082-7905) and bismuth oxide (01-078-0736). Some of the reflections are difficult to distinguish due to their overlap.
- PBSTS01ss—The material after the SPS technique contained the phase and probably bismuth oxide (01-078-0736).
3.2.2. Thermoelectric Properties of SHS-Processed Bismuth Telluride
4. Discussion
4.1. The Properties of Arc-Melted Materials
4.2. SHS
4.3. Thermoelectric Properties of SHS Materials
5. Conclusions
Author Contributions
Funding
Institutional Review Board Statement
Data Availability Statement
Acknowledgments
Conflicts of Interest
Abbreviations
SPS | Spark Plasma Sintering |
SHS | Self-propagating High-temperature Synthesis |
AM | Arc Melting |
ZT | Thermoelectric Figure-of-merit |
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Parameter | Value/Range | Unit |
---|---|---|
Operating temperature | RT-2000 | °C |
Sample diameter | 10–50 1 | mm |
Power supply max. current | 5000 | A |
Power supply max. voltage | 10 | V |
Power supply type | Alternate current | |
Ultimate vacuum | mBar | |
Pressing force (max) | 10 | Tons |
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Kaszyca, K.; Chmielewski, M.; Bucholc, B.; Błyskun, P.; Nisar, F.; Rojek, J.; Zybała, R. Using the Spark Plasma Sintering System for Fabrication of Advanced Semiconductor Materials. Materials 2024, 17, 1422. https://doi.org/10.3390/ma17061422
Kaszyca K, Chmielewski M, Bucholc B, Błyskun P, Nisar F, Rojek J, Zybała R. Using the Spark Plasma Sintering System for Fabrication of Advanced Semiconductor Materials. Materials. 2024; 17(6):1422. https://doi.org/10.3390/ma17061422
Chicago/Turabian StyleKaszyca, Kamil, Marcin Chmielewski, Bartosz Bucholc, Piotr Błyskun, Fatima Nisar, Jerzy Rojek, and Rafał Zybała. 2024. "Using the Spark Plasma Sintering System for Fabrication of Advanced Semiconductor Materials" Materials 17, no. 6: 1422. https://doi.org/10.3390/ma17061422