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Exploring the Synthesis Parameters and Spark Plasma Sintering of Tantalum Carbide Powders Prepared by Solvothermal Synthesis

机译:通过溶剂质合成制备的钽碳化物粉末的合成参数和火花等离子体烧结

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Tantalum carbide is a technologically important material for use in ultra-high temperatures and corrosive environments. In this report, we describe the scalability of a low temperature solvothermal method for the preparation of this useful material. X-ray diffraction shows phase-pure powders with no change in average crystallite size or compound stoichiometry compared to synthesis in smaller batches, remaining at 25 nm and 0.94 respectively. Dynamic light scattering shows a slight decrease in particle size distribution with scale-up. Thermogravimetric analysis (TGA) in air shows a decrease in surface species on the powders, but the powders oxidize at a lower temperature when scaling the synthesis. Mass spectrometry performed alongside TGA in a helium atmosphere reveals that water is the most abundant species on the surface of the powders, but oxygen, carbon monoxide, carbon dioxide, and nitrogen are also detected. Oxygen analysis reveals that the oxygen content of the powders is high (>6%). The oxygen source and methods of decreasing oxygen content are discussed. Initial sintering trials were performed and demonstrate the need for further powder processing.
机译:碳化物是一种技术重要的材料,用于超高温和腐蚀性环境。在本报告中,我们描述了低温溶剂热方法的可扩展性,用于制备这种有用的材料。 X射线衍射显示与较小批次的合成相比,平均微晶尺寸或化合物化学计量没有变化的相纯粉末,分别为25nm和0.94。动态光散射显示粒度分布的略微降低,具有缩放。空气中的热重分析(TGA)显示粉末上表面物种的降低,但粉末在缩放合成时在较低的温度下氧化。在氦气气氛中沿TGA进行质谱表明,水是粉末表面上最丰富的物种,但也检测到氧气,一氧化碳,二氧化碳和氮。氧分析显示粉末的氧含量高(> 6%)。讨论了氧气源和降低氧含量的方法。进行初始烧结试验并证明需要进一步的粉末加工。

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