Structure determination of thermal decomposition products from laboratory X-ray powder diffraction

Author:

Bataille Thierry,Audebrand Nathalie,Boultif Ali,Louër Daniel

Abstract

Abstract Ab initio structure determination from powder diffraction data of compounds resulting from solid state transformations is still rather limited. Two major factors influence the stages of the structure elucidation of these solids, i.e. the lower precision in peak position for indexing and the strong line overlap for extracting integrated intensities. The present study deals with the consideration of these two problems for solving the crystal structure of two thermal-decomposition inorganic products, Nd(NO3)3 · 4 H2O and Pb3O2(NO3)2. The new features of DICVOL04, as zero shift refinement, a priori zero search and tolerance of spurious lines have been used for indexing several phases obtained during the thermal treatment of neodymium nitrate hexahydrate. The crystal structures of Nd(NO3)3 · 4 H2O and Pb3O2(NO3)2 have been solved with the direct methods and the structure model of Pb3O2(NO3)2 has been completed using a global optimisation approach. The monoclinic structure of neodymium nitrate tetrahydrate [a = 10.1744(4) Å, b = 8.9716(5) Å, c = 11.7295(5) Å, β = 97.384(4)°, V = 1061.80 Å3, S.G. P21/c] is built from isolated ten-fold coordinated Nd polyhedra. The orthorhombic structure of lead oxide nitrate [a = 7.6034(4) Å, b = 5.7691(4) Å, c = 18.5817(9) Å, V = 815.09 Å3, S.G. Pnma] is built from double chains of edge-sharing OPb4 tetrahedra connected by nitrate groups. In order to estimate the chance of solving crystal structure of nanocrystalline powdered compounds, a comparison of the efficiency of direct methods and direct-space approaches is made from powder diffraction patterns simulated for various crystallite sizes from the crystal structure of the decomposition product γ-Zn2P2O7.

Publisher

Walter de Gruyter GmbH

Subject

Inorganic Chemistry,Condensed Matter Physics,General Materials Science

Cited by 11 articles. 订阅此论文施引文献 订阅此论文施引文献,注册后可以免费订阅5篇论文的施引文献,订阅后可以查看论文全部施引文献

同舟云学术

1.学者识别学者识别

2.学术分析学术分析

3.人才评估人才评估

"同舟云学术"是以全球学者为主线,采集、加工和组织学术论文而形成的新型学术文献查询和分析系统,可以对全球学者进行文献检索和人才价值评估。用户可以通过关注某些学科领域的顶尖人物而持续追踪该领域的学科进展和研究前沿。经过近期的数据扩容,当前同舟云学术共收录了国内外主流学术期刊6万余种,收集的期刊论文及会议论文总量共计约1.5亿篇,并以每天添加12000余篇中外论文的速度递增。我们也可以为用户提供个性化、定制化的学者数据。欢迎来电咨询!咨询电话:010-8811{复制后删除}0370

www.globalauthorid.com

TOP

Copyright © 2019-2024 北京同舟云网络信息技术有限公司
京公网安备11010802033243号  京ICP备18003416号-3