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用于电子粉末衍射(e-PDF)技术实施及氧化铁纳米晶体局部结构研究的粉末电子衍射背景优化。

Background optimization of powder electron diffraction for implementation of the e-PDF technique and study of the local structure of iron oxide nanocrystals.

作者信息

Mogili Naga Vishnu Vardhan, Verissimo Nathália Carolina, Abeykoon A M Milinda, Bozin Emil S, Bettini Jefferson, Leite Edson Roberto, Souza Junior João Batista

机构信息

Laboratório Nacional de Nanotecnologia (LNNano), Centro Nacional de Pesquisa em Energia e Materiais, Rua Giuseppe Máximo Scolfaro, 10.000 Polo II de Alta Tecnologia de Campinas, Campinas, São Paulo 13083-100, Brazil.

Photon Sciences Division, Brookhaven National Laboratory, Upton, New York 11973, USA.

出版信息

Acta Crystallogr A Found Adv. 2023 Sep 1;79(Pt 5):412-426. doi: 10.1107/S2053273323005107. Epub 2023 Jul 25.

DOI:10.1107/S2053273323005107
PMID:37490406
Abstract

The local structural characterization of iron oxide nanoparticles is explored using a total scattering analysis method known as pair distribution function (PDF) (also known as reduced density function) analysis. The PDF profiles are derived from background-corrected powder electron diffraction patterns (the e-PDF technique). Due to the strong Coulombic interaction between the electron beam and the sample, electron diffraction generally leads to multiple scattering, causing redistribution of intensities towards higher scattering angles and an increased background in the diffraction profile. In addition to this, the electron-specimen interaction gives rise to an undesirable inelastic scattering signal that contributes primarily to the background. The present work demonstrates the efficacy of a pre-treatment of the underlying complex background function, which is a combination of both incoherent multiple and inelastic scatterings that cannot be identical for different electron beam energies. Therefore, two different background subtraction approaches are proposed for the electron diffraction patterns acquired at 80 kV and 300 kV beam energies. From the least-square refinement (small-box modelling), both approaches are found to be very promising, leading to a successful implementation of the e-PDF technique to study the local structure of the considered nanomaterial.

摘要

使用一种称为对分布函数(PDF)(也称为约化密度函数)分析的全散射分析方法,探索了氧化铁纳米颗粒的局部结构特征。PDF 谱是从背景校正后的粉末电子衍射图(e-PDF 技术)推导出来的。由于电子束与样品之间存在强烈的库仑相互作用,电子衍射通常会导致多重散射,使强度重新分布到更高的散射角,并使衍射图谱中的背景增加。除此之外,电子与样品的相互作用会产生不良的非弹性散射信号,这主要对背景有贡献。目前的工作证明了对潜在复杂背景函数进行预处理的有效性,该背景函数是不相干多重散射和非弹性散射的组合,对于不同的电子束能量来说并不相同。因此,针对在 80 kV 和 300 kV 束能量下获得的电子衍射图,提出了两种不同的背景扣除方法。通过最小二乘法精修(小盒建模)发现,这两种方法都非常有前景,从而成功实现了 e-PDF 技术来研究所考虑纳米材料的局部结构。

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