Preparation of ultrafine tungsten powders by in-situ hydrogen reduction of nano-needle violet tungsten oxide

Ultrafine tungsten powders with a grain size below 0.5 mu m are key raw materials for fabricating ultrafine cemented carbides. Conventional hydrogen reduction technique has been utilized to prepare the ultrafine tungsten powders. In the present work, highly pure nano-needles of violet tungsten oxide (WO2.72) were reduced by dry hydrogen. Nucleation and growth of the metallic tungsten in the early stage of hydrogen reduction have been studied by XRD, FESEM and HRTEM. Mechanism of formation of nano-size tungsten powders is proposed and a concept of in-situ hydrogen of the nano-needle WO2.72 is presented. Empirical relations between an average diameter of nano-needle WO2.72 and an average particle size of the resultant tungsten powders in both stage of nucleation and industrial conduction have been established. These empirical relations could be a reasonable guidance for suitably choosing the raw materials of nano-needle WO2.72 to prepare ultrafine tungsten powders. It has been determined that the BET special surface areas of the in-situ hydrogen-reduced tungsten powders with the average particle size of 0.2 mu m and 0.3 mu m which were produced from the raw nano-needle WO2.72 powders with the average diameter of 60 nm and 80 nm, are 6.03 m(2)/g and 4.65 m(2)/g, and the oxygen contents are 0.35% and 0.29%, respectively. (C) 2011 Elsevier Ltd. All rights reserved.