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

IF 1.9 4区 材料科学 Q3 CHEMISTRY, MULTIDISCIPLINARY
Naga Vishnu Vardhan Mogili, Nathália Carolina Verissimo, A M Milinda Abeykoon, Emil S Bozin, Jefferson Bettini, Edson Roberto Leite, João Batista Souza Junior
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引用次数: 0

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.

粉末电子衍射背景优化,实现e-PDF技术,研究氧化铁纳米晶的局部结构。
利用一种称为对分布函数(PDF)(也称为约密度函数)分析的全散射分析方法,探讨了氧化铁纳米颗粒的局部结构特征。PDF轮廓是由背景校正的粉末电子衍射图(e-PDF技术)导出的。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次散射,导致强度向更高的散射角重新分布,并增加衍射剖面中的背景。除此之外,电子-试样的相互作用产生了一个不希望的非弹性散射信号,主要有助于背景。目前的工作证明了对潜在的复杂背景函数进行预处理的有效性,该背景函数是对不同电子束能量不可能相同的非相干多重和非弹性散射的组合。因此,本文针对80kv和300kv束流能量下的电子衍射图,提出了两种不同的背景减法。从最小二乘细化(小盒建模)来看,这两种方法都非常有前途,从而成功地实现了e-PDF技术来研究所考虑的纳米材料的局部结构。
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来源期刊
Acta Crystallographica Section A: Foundations and Advances
Acta Crystallographica Section A: Foundations and Advances CHEMISTRY, MULTIDISCIPLINARYCRYSTALLOGRAPH-CRYSTALLOGRAPHY
CiteScore
2.60
自引率
11.10%
发文量
419
期刊介绍: Acta Crystallographica Section A: Foundations and Advances publishes articles reporting advances in the theory and practice of all areas of crystallography in the broadest sense. As well as traditional crystallography, this includes nanocrystals, metacrystals, amorphous materials, quasicrystals, synchrotron and XFEL studies, coherent scattering, diffraction imaging, time-resolved studies and the structure of strain and defects in materials. The journal has two parts, a rapid-publication Advances section and the traditional Foundations section. Articles for the Advances section are of particularly high value and impact. They receive expedited treatment and may be highlighted by an accompanying scientific commentary article and a press release. Further details are given in the November 2013 Editorial. The central themes of the journal are, on the one hand, experimental and theoretical studies of the properties and arrangements of atoms, ions and molecules in condensed matter, periodic, quasiperiodic or amorphous, ideal or real, and, on the other, the theoretical and experimental aspects of the various methods to determine these properties and arrangements.
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