研究目的
To study the possibility of using the cold sintering process (CSP) to stabilize and densify thermodynamically unstable material system that undergoes decomposition at relatively low temperature.
研究成果
The cold sintering process (CSP) successfully densified thermodynamically unstable SnO without thermal decomposition, achieving up to 89% of theoretical density. The study demonstrated that CSP can be a viable method for processing materials with low thermal decomposition temperatures, offering opportunities for property exploration and development of functional composites at reduced temperatures and times.
研究不足
The study is limited by the thermodynamically unstable nature of SnO, which decomposes at low temperatures. The particle size reduction through ball-milling further decreases the thermal stability of SnO, adding challenges to densification and phase stability. The skeletal density measurements indicate possible formation of secondary or amorphous phases, closed porosity, or residue of transient liquid phase.
1：Experimental Design and Method Selection:
The CSP was employed to densify SnO below 300 °C by applying uniaxial pressure and using a transient liquid phase to mediate the dissolution-precipitation process.
2：Sample Selection and Data Sources:
Initial SnO powder was purchased from Alfa Aesar (
3：9%) and ball-milled to reduce agglomerate size. List of Experimental Equipment and Materials:
Equipment included a vibratory ball mill, manual hydraulic press with dual heating plates (Carver 4386), He gas pycnometer (Micromeritics Accupyc II 1340), laser particle size analyzer (Malvern Mastersizer 3000), thermogravimetric analyzer (TA Instrument TGA Q5500), BET surface area analyzer (ASAP 2020), scanning electron microscope (FEI Nova NanoSEM 630), X-ray diffractometer (PANalytical Empyrean), and four-point probe Seebeck coefficient and electrical conductivity measurement system (Linseis LSR-3). Materials included SnO powder, deionized water, 2 M acetic acid solution, and alumina grinding beads.
4：3). Materials included SnO powder, deionized water, 2 M acetic acid solution, and alumina grinding beads. Experimental Procedures and Operational Workflow:
4. Experimental Procedures and Operational Workflow: The SnO powder was ball-milled, mixed with a transient liquid phase, and cold sintered under uniaxial pressure at temperatures ranging from 70 to 265 °C. The density, surface area, microstructure, phase purity, and electrical properties of the sintered pellets were characterized.
5：Data Analysis Methods:
The density was measured using the Archimedes method and He gas pycnometry. The BET theory was used to analyze surface area reduction. XRD was used to assess phase purity and crystalline texture. Electrical properties were measured as a function of temperature.
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laser particle size analyzer
Malvern Mastersizer 3000
Malvern
Measurement of particle size distribution
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scanning electron microscope
FEI Nova NanoSEM 630
FEI
Imaging of microstructures
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X-ray diffractometer
PANalytical Empyrean
PANalytical
Characterization of phase purity and preferred orientation
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SnO powder
Alfa Aesar
Starting material for cold sintering process
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vibratory ball mill
Reduction of powder agglomerate size
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manual hydraulic press
Carver 4386
Carver
Application of uniaxial pressure during cold sintering
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He gas pycnometer
Micromeritics Accupyc II 1340
Micromeritics
Measurement of skeletal density
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thermogravimetric analyzer
TA Instrument TGA Q5500
TA Instrument
Determination of thermal decomposition temperature
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BET surface area analyzer
ASAP 2020
Measurement of specific surface area
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four-point probe Seebeck coefficient and electrical conductivity measurement system
Linseis LSR-3
Linseis
Measurement of electrical properties
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