分别以TaCl5和ZrCl4为钽源和锆源,酚醛树脂为碳源,采用溶剂热结合碳热还原法合成单相固溶陶瓷粉末TaZr2.75C3.75(TZC)。通过热力学和原子尺寸效应值计算分析碳热还原法合成TaZr2.75C3.75粉末的可行性,研究乙酰丙酮含量、金属原子浓度以及溶剂种类等工艺参数对粉末相组成、微观形貌以及粒径的影响。结果表明,通过溶剂热结合碳热还原反应,1 700 ℃可制备晶粒尺寸为纳米级的单相TaZr2.75C3.75固溶陶瓷粉末。增加乙酰丙酮的含量可以提高粉末的分散性。随着金属原子浓度的提升,粉末从球形转变为不规则形态,平均粒径从微米级(~2.13 µm)减小至亚微米级(~0.140 µm)。相比丁醇溶剂,乙醇作为溶剂可获得分散性更好、颗粒尺寸更小的粉末。
Single-phase solid solution ceramic powders TaZr2.75C3.75 were synthesized by combining solvothermal and carbothermal reduction. In which, TaCl5 and ZrCl4 were used as the tantalum and zirconium source respectively and phenolic resin was used as the carbon source. The possibility of the synthesis of TaZr2.75C3.75 powders by the carbothermal reduction method was demonstrated by thermodynamic and atomic size effect. The effects of process parameters such as acetylacetone content, metal atom concentration and solvent type on the powder morphology and particle size were investigated. The results show that the single-phase TaZr2.75C3.75 solid solution ceramic powders can be prepared by the carbothermal reduction reaction at 1 700 ℃. Increasing the content of acetylacetone can improve the dispersibility of the powders. With increasing the concentration of metal atoms, the powder changes from a spherical shape to an irregular shape, and the average particle size decreases from the micron level (~2.13 µm) to the submicron level (~0.140 µm). Compared witn butanol solvent, better dispersion and smaller particle size of TaZr2.75C3.75 solid solution ceramic powders can be achieved with ethanol as a solvent.
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