氢化-脱氢法制备锆粉及其性能表征  

Fabrication and properties characterization of Zr powder by hydrogenation-dehydrogenation combined method

作　　者：康建刚[1] 江垚[1] 贺跃辉[1] 高海燕[1] 

机构地区：[1]中南大学粉末冶金国家重点实验室,长沙410083

出　　处：《粉末冶金材料科学与工程》2015年第4期655-660,共6页Materials Science and Engineering of Powder Metallurgy

基　　金：国家自然科学基金青年基金资助项目(51404301)

摘　　要：以海绵锆为原料,采用氢化-脱氢法制备一种高纯、粒度可控、分布集中的锆粉。研究脱氢温度、球磨时间、球料比对粉末粒度、纯度的影响。采用扫描电子显微镜(SEM)、激光粒度测试仪、元素含量测试等手段对锆粉表面形貌、粒度及氧、氮、氢含量进行表征。结果表明:采用氢化-脱氢法制备的锆粉为不规则形状,呈现机械破碎的特性;海绵锆在700℃渗氢1 h,氢的质量分数达1.98%,渗氢完全;最佳脱氢温度580℃,脱氢时间1 h,氢含量降至0.002 2%,脱氢完全且无大面积结块;最佳球料比8:1,球磨时间60 min,制备的锆粉中位径D50=18.36μm;脱氢前后O元素的质量分数分别为0.17%、0.45%,制备过程中粉末氧含量均得到了有效控制,符合低氧制备锆粉的要求。A type of particle size controllable high-purity zirconium powder was fabricated by hydrogenation- dehydrogenation （HDH） method with zirconium sponge as raw materials. The effects of dehydrogenation temperature, ball-milling time and ball-to-powder mass ratio on the particle size and purity of zirconium powder were investigated. The morphology and particle size distribution of the zirconium powder, as well as the content of oxygen, nitrogen and hydrogen were characterized by scanning electron microscopy （SEM）, laser-diffraction diameter tester and element content tester, etc. The results show that zirconium powder appears as mechanically crushed and has an irregular shape. The zirconium sponge absorbs hydrogen completely after hydrogenation at 700℃ for 1 h, with a hydrogen content of 1.98%. Under the optimum dehydrogenization temperature of 580 ℃ for 1 h, the Zr powder is dehydrogenated completely without noticeable large lumps, with the content of hydrogen decreasing to 0.0022%; Zr powder with D50=-18.36μm is fabricated after ball-milling for 60 rain under the optimum ball-to-powder mass ratio of 8：1 with an effective control of the oxygen content during the process, it only increases from 0.17% to 0.45% during dehydrogenization, which meets the low oxygen content requirement for the fabrication of zirconium powder.

关 键 词：氢化-脱氢法 温度 球磨 粒度分布 元素含量 

分 类 号：TF123[冶金工程—粉末冶金]