研究目的
To in-situ synthesize nano-SiC whiskers in Li2O-Al2O3-SiO2 ternary system for preparing highly densified mullite-SiCw composite ceramics used for solar heat transmission pipeline, investigating the mechanisms of synthesis and the impact on composite properties.
研究成果
Nano-SiC whiskers were successfully in-situ synthesized in the Li2O-Al2O3-SiO2 ternary system, primarily through LS and VS mechanisms. Li2CO3 additive enhanced SiC yield by increasing liquid content and reducing viscosity. The composites showed improved mechanical and thermal properties, with sample BS1 exhibiting optimal performance: high density, bending strength, and thermal conductivity. This makes the composites suitable for solar heat transmission pipelines due to enhanced thermal shock resistance and conductivity.
研究不足
The study used Li2CO3 as a flux, which generates CO2 gas during decomposition, potentially increasing porosity. Residual silicon was not fully consumed, which might affect properties. The mechanisms (LS and VS) were identified but may have limitations in controlling whisker growth uniformly. Sintering temperatures up to 1460 °C were used, which might be high for some applications.
1:Experimental Design and Method Selection:
The study involved in-situ synthesis of nano-SiC whiskers in a Li2O-Al2O3-SiO2 ternary system using carbothermal reduction and mechanisms like Liquid-Solid (LS) and Vapor-Solid (VS). Raw materials were mixed, formed into compacts, and sintered in a carbon bed in a molybdenum disilicide furnace at temperatures from 1400 to 1460 °C with a heating rate of 5 °C/min and holding time of 2 hours.
2:Sample Selection and Data Sources:
Samples were prepared with varying Li2CO3 additions (0 to 2.22 wt%) and sintered at different temperatures. Natural raw materials included kaolin, spodumene, quartz, graphite, and silicon powder.
3:22 wt%) and sintered at different temperatures. Natural raw materials included kaolin, spodumene, quartz, graphite, and silicon powder. List of Experimental Equipment and Materials:
3. List of Experimental Equipment and Materials: Equipment included a ball mill for mixing, uniaxial press for forming, electrical oven for drying, molybdenum disilicide furnace for sintering, electronic analytical balance for density measurements, electronic universal test machine for bending strength, laser flash thermal constant analyzer for thermal conductivity, thermal dilatometer for CTE, X-ray diffractometer for phase analysis, SEM and TEM for microstructure observation, and EDS for elemental analysis. Materials included Longyan kaolin, spodumene, quartz, graphite, silicon powder, Li2CO3, and PVA binder.
4:Experimental Procedures and Operational Workflow:
Powders were mixed by ball milling, formed into compacts under 10 MPa pressure with PVA binder, dried at 100 °C for 24 hours, sintered in a carbon bed at specified temperatures, and characterized for physical, mechanical, and thermal properties.
5:Data Analysis Methods:
XRD patterns were analyzed using the Reference Intensity Ratio (RIR) method for semi-quantitative phase content. SEM and TEM images were used for microstructure analysis. EDS was used for elemental composition. Physical properties were measured using Archimedes' principle, bending strength tests, and thermal property measurements.
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SEM
SU-8010
Hitachi
Observing microstructure of samples
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EDS
INCA Energy 350
Oxford
Elemental analysis using energy dispersive spectroscopy
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electronic analytical balance
JA5003B
Shanghai Techcomp Co., Ltd
Testing water absorption, open porosity, and bulk density based on Archimedes' principle
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electronic universal test machine
Shanghai Yanrun Light-Machine Technology Co., Ltd.
Measuring bending strength of samples
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laser flash thermal constant analyzer
LFA 457
Netzsch GmbH Co., Ltd
Measuring thermal conductivity of samples
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thermal dilatometer
DIL 402C
Netzsch GmbH Co., Ltd
Testing coefficients of thermal expansion
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X-ray diffractometer
D8 Advance
Bruker AXS Co., Ltd
Collecting XRD patterns for phase analysis
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TEM
JEOL Ltd.
Observing morphology of crystalline phases
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molybdenum disilicide furnace
Sintering samples in a carbon bed
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ball mill
Mixing powders of raw materials
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uniaxial press
Forming compacts under pressure
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electrical oven
Drying formed compacts
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