基于Rietveld方法的AlH_(3)晶型定量分析  

Quantitative analysis of AlH_(3) crystal form based on Rietveld method

作　　者：张政 秦明娜[2] 张璐瑶 石强[2] 陈熙萌[1] 郭艳玲[1] 陈林[1] ZHANG Zheng;QIN Mingna;ZHANG Luyao;SHI Qiang;CHEN Ximeng;GUO Yanling;CHEN Lin(School of Nuclear Science and Technology,Lanzhou University,Lanzhou 730000,China;Xi'an Modern Chemistry Research Institute,Xi'an 710065,China)

机构地区：[1]兰州大学核科学与技术学院,兰州730000 [2]西安近代化学研究所,西安710065

出　　处：《固体火箭技术》2022年第2期255-260,共6页Journal of Solid Rocket Technology

基　　金：西安近代化学所开放合作创新基金资助(No.SYJJ01)。

摘　　要：为高效准确地测定氢化铝产品中各晶型以及非晶的含量,利用X射线粉末衍射技术(XRD),结合Rietveld多相精修方法,通过向样品中掺入已知含量的内标单晶Si,分析指认了两种AlH_(3)产品中存在的晶型。A样品含α-AlH_(3)、α′-AlH_(3)、Al(OH);三种晶型,质量百分数分别为63.09%(±2.33)、9.74%(±0.65)、6.74%(±0.47),非晶含量为20.44%(±2.38);B样含α-AlH_(3)和Al两种晶型,质量百分数分别为24.00%(±0.75)、7.40%(±0.73),非晶含量为68.60%(±1.17)。结果表明,A样α-AlH_(3)含量较高,非晶含量相对较少,说明A样质量较优。相对标准偏差表明,采用Rietveld多相精修方法,对于相含量高的物相定量分析准确度更高。该方法对AlH_(3)中多种杂质晶型和非晶均可实现可靠的绝对定量分析,为评估AlH_(3)产品质量提供了重要参考依据,对未来AlH_(3)的规模化应用具有重要意义。In order to determine the content of crystal form and amorphous phase in aluminum hydride products efficiently and accurately,the internal standard single crystal Si with known content was added into the samples,and the crystal forms in two AlH_(3)products were analyzed and identified by using X-ray powder diffraction(XRD)and Rietveld multi-phase refinement method.The content ofα-AlH_(3),α’-AlH_(3),Al(OH);and amorphous phases in sample A was 63.09%(±2.33),9.74%(±0.65),6.74%(±0.47)and 20.44%(±2.38)respectively.Sample B contained 24.00%(±0.75)α-AlH_(3),7.40%(±0.73)Al and 68.60%(±1.17)amorphous phases.The results show that theα-AlH_(3)content of sample A is higher and the amorphous content is smaller,which indicates that the quality of sample A is better than that of sample B.The relative standard deviation indicates that Rietveld mult-phase refinement method is more accurate for quantitative analysis of high phase content.This method can realize reliable absolute quantitative analysis of various impurity crystal form and amorphous in AlH_(3),provides an important reference basis for evaluating the product quality of AlH_(3),and will be of great significance for the large-scale application of AlH_(3)in the future.

关 键 词：三氢化铝 XRD RIETVELD精修 内标法 

分 类 号：V512[航空宇航科学与技术—航空宇航推进理论与工程]