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Extension of Rietveld Refinement for Benchtop Powder XRD Analysis of Ultrasmall Supported Nanoparticles
Chemistry of Materials ( IF 7.2 ) Pub Date : 2022-09-12 , DOI: 10.1021/acs.chemmater.2c00101 Jeremiah Lipp 1 , Ritubarna Banerjee 1 , Md. Fakhruddin Patwary 1 , Nirmalendu Patra 2 , Anhua Dong 1 , Frank Girgsdies 3 , Simon R. Bare 2 , J. R. Regalbuto 1
Chemistry of Materials ( IF 7.2 ) Pub Date : 2022-09-12 , DOI: 10.1021/acs.chemmater.2c00101 Jeremiah Lipp 1 , Ritubarna Banerjee 1 , Md. Fakhruddin Patwary 1 , Nirmalendu Patra 2 , Anhua Dong 1 , Frank Girgsdies 3 , Simon R. Bare 2 , J. R. Regalbuto 1
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We present a method for characterizing ultrasmall (<2 nm) supported crystallites with benchtop XRD. Central to the method is an understanding of the intensity effects at play; these intensity effects and their corrections are discussed in depth. Background subtraction─long considered one of the main barriers to ultrasmall crystal characterization─is solved by correcting the diffractogram of a separately measured support for the relevant intensity effects. Rietveld refinement is demonstrated to be an adequate analysis method for the general characterization of simple nanosystems. A 4.8% Pt/SiO2 sample (1.3 nm, volume-weighted average) is used as a case study; it is found that the Pt spontaneously oxidizes under ambient conditions and consists of a metallic core surrounded by a PtO2 shell. Both phases have average dimensions smaller than 1 nm. The XRD results also suggest lattice expansion of the Pt core as compared to bulk Pt.
中文翻译：
Rietveld 细化的扩展用于超小负载纳米颗粒的台式粉末 XRD 分析
我们提出了一种用台式 XRD 表征超小 (<2 nm) 支持的微晶的方法。该方法的核心是理解发挥作用的强度效应；深入讨论了这些强度效应及其校正。背景减法——长期以来被认为是超小晶体表征的主要障碍之一——通过校正相关强度效应的单独测量支持物的衍射图来解决。Rietveld 细化被证明是简单纳米系统一般表征的充分分析方法。以 4.8% Pt/SiO 2样品（1.3 nm，体积加权平均值）作为案例研究；发现 Pt 在环境条件下会自发氧化，并由被 PtO 2包围的金属核组成壳。两相的平均尺寸均小于 1 nm。XRD 结果还表明，与块状 Pt 相比，Pt 核的晶格膨胀。
更新日期：2022-09-12
中文翻译：
Rietveld 细化的扩展用于超小负载纳米颗粒的台式粉末 XRD 分析
我们提出了一种用台式 XRD 表征超小 (<2 nm) 支持的微晶的方法。该方法的核心是理解发挥作用的强度效应；深入讨论了这些强度效应及其校正。背景减法——长期以来被认为是超小晶体表征的主要障碍之一——通过校正相关强度效应的单独测量支持物的衍射图来解决。Rietveld 细化被证明是简单纳米系统一般表征的充分分析方法。以 4.8% Pt/SiO 2样品（1.3 nm，体积加权平均值）作为案例研究；发现 Pt 在环境条件下会自发氧化，并由被 PtO 2包围的金属核组成壳。两相的平均尺寸均小于 1 nm。XRD 结果还表明，与块状 Pt 相比，Pt 核的晶格膨胀。
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