为了制备高纯的碳化钒粉末,对五氧化二钒为原料小批量制备所得碳化钒产物进行了真空热处理。采用X射线衍射仪（XRD）、扫描电子显微镜（SEM）、LECO碳氧分析仪等测试手段对热处理产物进行了表征,重点研究了热处理温度对碳化钒粉末的影响,并用X射线光电子能谱仪（XPS）测试探讨了热处理对碳化钒纯化的机理。结果表明：在1100℃的热处理温度下,可得到有序的V8C7相,游离碳和氧含量分别为0.18%、0.31%;热处理的过程使得碳化钒中的游离碳和氧的下降是粉末中游离碳和剩余的少量钒氧化物发生了进一步的还原反应和粉末中吸附水的消失造成的。
In order to prepare high purity vanadium carbide powder,the products obtained by carbonthermal reduction using vanadium pentoxide and nano-carbon black as raw materials were heat treated in vacuum and a small quantity of vanadium carbide was synthesized.The vacuum heat-treatment products were characterized by X-ray diffraction（XRD）,scanning electron microscopy（SEM）,LECO oxygen analyzer and X-ray photoelectron spectroscopy（XPS）.Influence of the heat treatment temperature on the vanadium carbide powders and effect of heat treatment on the mechanism of purification of vanadium carbide were studied.The results indicate the ordered V8C7 powder with 0.18% free carbon,0.31% oxygen content can be prepared by the heat treatmeant at 1100 ℃.During the vacuum heat-treatment of V8C7 powder,further reduction of a small amount of remaining free carbon and vanadium oxide in the powders occurs and adsorbed water is eliminated,which is the basic mechanism of its purification.
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