研究目的
Investigating the thermoelectric properties and microstructures of Na-doped PbTe compounds synthesized by various milling and sintering processes, focusing on grain growth mechanisms and their impact on performance.
研究成果
The research concludes that SPS induces abnormal grain growth and higher lattice strains/defects compared to HP, leading to reduced electrical conductivity and power factor, despite lower thermal conductivity. Lattice strains and defects are more critical for thermoelectric performance than grain size control, suggesting that SPS may not be optimal for enhancing ZT in these materials.
研究不足
The study is limited to Na-doped PbTe compounds and specific milling/sintering conditions; results may not generalize to other materials or processes. Defect quantification from TEM is qualitative, and EDS measurements have limitations in detecting light elements like Na. The focus on lattice strains and defects as primary factors may overlook other influences on thermoelectric performance.
1:Experimental Design and Method Selection:
The study involved synthesizing Na-doped PbTe compounds using different milling processes (hand milling and ball milling) and sintering methods (hot press and spark plasma sintering) to investigate their effects on microstructure and thermoelectric properties. Theoretical models included the Williamson-Hall equation for lattice strain analysis and Gibbs free energy considerations for grain growth mechanisms.
2:Sample Selection and Data Sources:
Crystalline ingots of Pb0.96Na0.04Te were synthesized by direct melting of high-purity elements (Pb, Na, Te). Powders were prepared by hand milling and ball milling (10 min and 30 min), followed by sintering via HP or SPS. Data sources included XRD, SEM, TEM, EBSD, EDX, and thermoelectric property measurements.
3:96Na04Te were synthesized by direct melting of high-purity elements (Pb, Na, Te). Powders were prepared by hand milling and ball milling (10 min and 30 min), followed by sintering via HP or SPS. Data sources included XRD, SEM, TEM, EBSD, EDX, and thermoelectric property measurements. List of Experimental Equipment and Materials:
3. List of Experimental Equipment and Materials: Equipment included a planetary ball mill (Pulverisette-5, Fritsch), XRD with Cu Kα radiation, SEM (MERLIN, Carl Zeiss), TEM (JEOL 2100F), FIB (Nova 600 nanolab), thermoelectric measurement system (ZEM-3 ULVAC), laser flash apparatus (LFA-457, NETZSCH), and PPMS (Quantum Design). Materials included high-purity Pb (99.999%), Na (99.95%), Te (99.999%), and stainless steel balls.
4:999%), Na (95%), Te (999%), and stainless steel balls. Experimental Procedures and Operational Workflow:
4. Experimental Procedures and Operational Workflow: Ingots were melted, annealed, pulverized by milling, and sintered under specific conditions (HP: 40 min at 873 K, 50 MPa; SPS: 5 min at 873 K, 50 MPa). Characterization involved XRD for phase identification, SEM and TEM for microstructure analysis, EBSD for grain size distribution, and measurements of electrical conductivity, Seebeck coefficient, thermal diffusivity, and Hall carrier concentration.
5:Data Analysis Methods:
Data analysis included lattice parameter calculation from XRD, lattice strain estimation using the Williamson-Hall equation, Hall carrier density calculation from Hall coefficient, thermal conductivity derivation from density, thermal diffusivity, and specific heat, and power factor and ZT calculation from measured properties.
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Scanning Electron Microscope
MERLIN
Carl Zeiss
Microstructure and composition analysis
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Transmission Electron Microscope
JEOL 2100F
JEOL
High-resolution imaging and lattice strain analysis
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Physical Property Measurement System
PPMS Dynacool 14 T
Quantum Design
Measuring specific heat and Hall coefficient
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Physical Property Measurement System
16 T PPMS DynaCool
Quantum Design
Measuring Hall coefficient under magnetic field
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Planetary Ball Mill
Pulverisette-5
Fritsch
Pulverizing ingots into powders for milling processes
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X-ray Diffractometer
Phase identification and structural characterization
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Focused Ion Beam
Nova 600 nanolab
Ion etching for clean TEM sample surfaces
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Thermoelectric Measurement System
ZEM-3
ULVAC
Measuring Seebeck coefficient and electrical resistivity
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Laser Flash Apparatus
LFA-457
NETZSCH
Measuring thermal diffusivity
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