Improved Method for Electron Powder Diffraction-Based Rietveld Analysis of Nanomaterials

Author:

Kis Viktória K.12,Kovács Zsolt3ORCID,Czigány Zsolt1

Affiliation:

1. HUN-REN Centre for Energy Research, Institute of Technical Physics and Materials Science, Konkoly-Thege Miklós út 29-33, H-1121 Budapest, Hungary

2. Department of Mineralogy, Eötvös Loránd University, Pázmány Péter sétány 1/c, H-1117 Budapest, Hungary

3. Department of Materials Physics, Eötvös Loránd University, Pázmány Péter sétány 1/a, H-1117 Budapest, Hungary

Abstract

Multiphase nanomaterials are of increasing importance in material science. Providing reliable and statistically meaningful information on their average nanostructure is essential for synthesis control and applications. In this paper, we propose a novel procedure that simplifies and makes more effective the electron powder diffraction-based Rietveld analysis of nanomaterials. Our single step in-TEM method allows to obtain the instrumental broadening function of the TEM directly from a single measurement without the need for an additional X-ray diffraction measurement. Using a multilayer graphene calibration standard and applying properly controlled acquisition conditions on a spherical aberration-corrected microscope, we achieved the instrumental broadening of ±0.01 Å in terms of interplanar spacing. The shape of the diffraction peaks is modeled as a function of the scattering angle using the Caglioti relation, and the obtained parameters for instrumental broadening can be directly applied in the Rietveld analysis of electron diffraction data of the analyzed specimen. During peak shape analysis, the instrumental broadening parameters of the TEM are controlled separately from nanostructure-related peak broadening effects, which contribute to the higher reliability of nanostructure information extracted from electron diffraction patterns. The potential of the proposed procedure is demonstrated through the Rietveld analysis of hematite nanopowder and two-component Cu-Ni nanocrystalline thin film specimens.

Funder

National Research, Development and Innovation Fund Office, Hungary

European Structural and Investment Funds

Publisher

MDPI AG

Reference40 articles.

1. The role of solid nanoparticle technology in the parenteral delivery of poorly water–soluble drugs;Kipp;Int. J. Pharm.,2004

2. Application of dental nanomaterials: Potential toxicity to the central nervous system;Feng;Int. J. Nanomed.,2015

3. Acquisition and evaluation procedure to improve the accuracy of SAED;Kis;Microsc. Res. Tech.,2023

4. Line Profiles of Neutron Powder–Diffraction Peaks for Structure Refinement;Rietveld;Acta Crystallogr.,1967

5. Zuo, J.-M., Lábár, J.L., Zhang, J., Gorelik, T.E., and Kolb, U. (2019). International Tables for Crystallography Vol. H, John Wiley & Sons.

Cited by 1 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