【作者】 刘晓明；

【导师】 范荫恒； 单文娟；

【作者基本信息】 辽宁师范大学 ， 物理化学， 2008， 硕士

【摘要】 1.在温和条件下采用催化法、卤代烃引发法和金属经活化后利用溶剂效应三种方法首次制备出纳米氢化铥。借助X射线粉末衍射（XRD）、透射电镜（TEM）、差热分析和BET法对产物进行了表征。测试结果表明催化法制备的氢化铥具有六方晶系结构,分子式为TmH_2.87;另外两种方法制备的氢化铥均为立方晶系结构,分子式为TmH₂。通过谢乐公式计算出上述三种方法制得的氢化铥的平均粒径分别为30 nm、14 nm和15 nm,与TEM测得的数值基本吻合。BET测得氢化铥的比表面积分别为11.0 m²/g、13.6 m²/g和36.6 m²/g。对纳米氢化铥进行了加氮性能实验。实验结果表明,纳米氢化铥在常温时不与N₂反应,而升温至200℃开始反应,产物的XRD测试与JCP2卡中已有的数据不吻合,但经过反复实验测得的XRD数据均一致,推测产物可能为一种新的氮化物晶型,进一步的验证工作正在进行。通过谢乐公式计算出加氮产物平均粒径为15 nm。2.在温和条件下,采用络合催化法、卤代烃引发法合成金属铥有机中间体,并利用其热不稳定性,在真空条件下进行热分解制备纳米尺寸铥金属粉末。制备的纳米金属铥粉末活性很高,暴露在空气中有火花,对合成出的纳米铥粉末进行了加氢、加氮性能实验。实验结果表明,纳米铥粉末在常温常压下就能与H₂发生反应,XRD测试表明生成的氢化铥是立方和六方晶型的混合物,由谢乐公式计算其平均颗粒大小为19 nm,BET测试其比表面积为22.8 m²/g。通过谢乐公式计算出加氮产物平均粒径为13 nm,与TEM测得的数值基本吻合。3.在讨论和重复实验的基础上进一步修正了组内前人所做的数据。温和条件下,采用络合催化法、卤代烃引发法合成金属铝有机中间体,并利用其热不稳定性,在真空条件下进行热分解制备纳米尺寸铝金属粉末。XRD测试表明产物为面心立方晶型,通过谢乐公式计算平均粒径为30 nm,与TEM测试结果一致。BET测得产物的比表面积为33.8 m²/g。更多还原

【Abstract】 Content:1.Nanosized thulium hydride was first successfully synthesized by using catalytic method,halogenated hydrocarbon solicitation method and metal activation method under mild conditions.The product was characterized by using XRD,TEM and BET methods.XRD patterns of thulium hydride,which was synthesized by using catalytic method,were identified to have hexagonal structures,and the molecular structure was TmH_2.87.The rest was cubic crystal structures,the molecular structure was TmH₂.The average particle sizes calculated from XRD images by Scherrer formula are 30 nm,14 nm and 15 nm respectively,which are in agreement with the results from TEM images.And they had large specific areas of 11.0 m²/g,13.6 m²/g and 36.6 m²/g correspondingly.The result of the nitriding experiment of nanosized thulium hydride indicated that nanosized thulium hydride does not react with N₂ at atmosphere temperature,but the reaction took place at 200℃.XRD pattern showed the data can’t consistent with JCP2 card,but repetitious data are same.So we considered it’s a new product.The average particle size calculated from XRD images by Scherrer formula is 15 nm.2.A simple and easy way was reported to prepare nanometric thulium powder by the thermal decomposition of organo-thulium under vacuum. The results of the hydrogenation and nitriding experiments of nanosized Tm indicated that nanosized Tm can react with H₂ at atmosphere temperature and normal pressure.XRD pattern showed that the product was thulium hydride with mixture crystal structures of cubic and hexagonal system.The average particle size calculated from XRD images by Scherrer formula is 19 nm.And it has a large specific area of 22.8 m²/g. The average particle size calculated from XRD images of nitriding product by Scherrer formula is 13 nm,which are in agreement with the results from TEM images.3.Under the base of discussion and repeated experiments, Organo-aluminium intermediate was prepared by using coordination catalysis method and halogenated hydrocarbon solicitation method under mild conditions.Heat instability of the intermediate was considered to prepare nanosized aluminium by vacuum pyrogenation for it.The average particle size calculated from XRD images of nanosized aluminium by Scherrer formula is 30 nm,which are in agreement with the results from TEM images.And they had a large specific area of 33.8 m²/g.更多还原