XRD技术在纳米WC-Co复合粉制备过程中的应用
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摘要
介绍了X射线衍射技术(XRD)的原理及其在钨粉末冶金中的运用,并结合笔者对纳米WC-Co复合粉的研究,重点介绍了XRD技术在纳米WC-Co复合粉制备过程中的应用,包括物相定性分析、晶粒尺寸测定及点阵参数测定等方面的应用。以可溶钴盐、偏钨酸铵(AMT)、有机碳源为主要原料,通过喷雾转化、连续低温还原碳化法制备出了纳米晶WC-Co复合粉,用XRD技术对制备过程中样品进行分析,结果表明:采用喷雾转化、连续低温还原碳化工艺可制备出仅有WC和Co两相的复合粉末,W被完全碳化,WC晶粒度约60nm,Co相为面心立方结构。
The principle of X-ray diffraction(XRD)and its application in tungsten powder metallurgy are introduced.Combined with the authors' research on WC-Co nanocomposite powder,the application of XRD technique in preparation of WC-Co nanocomposite powder is emphatically introduced,including qualitative phase analysis,grain size determination and lattice parameter determination.Using soluble cobalt salt,ammonium metatungstate(AMT)and organic carbon source as main raw materials,WC-Co nanocomposite powder was prepared by spray conversion and continuous low-temperature reduction carbonization and the samples were analyzed by XRD during preparation.The results show that the composite powder only having the two phases of WC and Co can be prepared by spray conversion and continuous low-temperature reduction carbonization,W is completely carbonized,the grain size of WC is about 60 nm,and Co phase exists with face-centered cubic structure.
The principle of X-ray diffraction(XRD)and its application in tungsten powder metallurgy are introduced.Combined with the authors' research on WC-Co nanocomposite powder,the application of XRD technique in preparation of WC-Co nanocomposite powder is emphatically introduced,including qualitative phase analysis,grain size determination and lattice parameter determination.Using soluble cobalt salt,ammonium metatungstate(AMT)and organic carbon source as main raw materials,WC-Co nanocomposite powder was prepared by spray conversion and continuous low-temperature reduction carbonization and the samples were analyzed by XRD during preparation.The results show that the composite powder only having the two phases of WC and Co can be prepared by spray conversion and continuous low-temperature reduction carbonization,W is completely carbonized,the grain size of WC is about 60 nm,and Co phase exists with face-centered cubic structure.
引文
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[3]解其云,吴小山.X射线衍射进展简介[J].物理,2012,41(11):727-735.
[4]麦振洪.晶体X射线衍射的发现及其深远影响[J].物理,2012,41(11):721-726.
[5]储刚.含非晶相样品的X射线衍射增量法定量相分析[J].物理学报,1998,47(7):1 143-1 148.
[6]沈春玉,储刚.X射线衍射定量相分析新方法[J].分析测试学报,2003,22(6):80-82.
[7]洪汉烈,陈建军,杨淑珍,等.水泥熟料定量分析的全谱拟合法[J].分析测试学报,2001,20(2):5-8.
[8]徐君,黄金萍,骆红山,等.X射线衍射全谱拟合相定量分析新方法:Le Bail直接比对法[J].实验室研究与探索,2010,29(11):219-222.
[9]曾蒙秀,宋友桂.麦夸特算法在X射线衍射物相定量分析中的应用[J].地球科学——中国地质大学学报,2013,38(2):431-440.
[10]何崇智,张志军,李艳萍.多相全谱拟合无标样定量相分析[J].物理测试,2011,(Z):170-174.
[11]羊建高,吕健,朱二涛,等.连续还原碳化法制备纳米WC-Co复合粉研究[J].有色金属科学与工程,2013,4(5):23-27,107.
[12]吕健,羊建高,陈颢,等.喷雾干燥与低温还原碳化法制备纳米晶WC-Co复合粉末[J].粉末冶金材料科学与工程,2013,18(6):835-839.
[13]权淑丽,郑开宇.X射线衍射仪在冶金行业的应用[J].浙江冶金,2013,(3):20-23.
[14]张力德,牟季美.纳米材料和纳米结构[M].北京:科学出版社,2001.147-148.
[15]林晨光,袁冠森.纳米晶WC-Co硬质合金中WC晶粒度的定量测量[J].中国有色金属学报,2005,15(6):823-828.
[16]羊建高,谭敦强,陈颢.硬质合金[M].长沙:中南大学出版社,2012.7-9.
[17]郭圣达,羊建高,陈颢,等.纳米WC-Co复合粉末形貌的影响因素[J].粉末冶金材料科学与工程,2014,19(6):1 000-1 005.
[18]吴厚平,张立,王元杰,等.化学包裹粉工艺制备粗晶粒WC-Co硬质合金[J].中国有色金属学报,2010,20(4):701-705.