A new method forin situstructural investigations of nano-sized amorphous and crystalline materials using mixed-flow reactors,Acta Crystallographica Section A: Foundations and Advances

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A new method forin situstructural investigations of nano-sized amorphous and crystalline materials using mixed-flow reactors
Acta Crystallographica Section A: Foundations and Advances ( IF 1.9 ) Pub Date : 2019-08-23 , DOI: 10.1107/s2053273319008623
Alexandria Hoeher ₁ , Sebastian Mergelsberg ₁ , Olaf J Borkiewicz ₂ , Patricia M Dove ₁ , F Marc Michel ₁

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Structural investigations of amorphous and nanocrystalline phases forming in solution are historically challenging. Few methods are capable ofin situatomic structural analysis and rigorous control of the system. A mixed-flow reactor (MFR) is used for total X-ray scattering experiments to examine the short- and long-range structure of phasesin situwith pair distribution function (PDF) analysis. The adaptable experimental setup enables data collection for a range of different system chemistries, initial supersaturations and residence times. The age of the sample during analysis is controlled by adjusting the flow rate. Faster rates allow for younger samples to be examined, but if flow is too fast not enough data are acquired to average out excess signal noise. Slower flow rates form older samples, but at very slow speeds particles settle and block flow, clogging the system. Proper background collection and subtraction is critical for data optimization. Overall, this MFR method is an ideal scheme for analyzing thein situstructures of phases that form during crystal growth in solution. As a proof of concept, high-resolution total X-ray scattering data of amorphous and crystalline calcium phosphates and amorphous calcium carbonate were collected for PDF analysis.

中文翻译：

使用混流反应器研究纳米非晶和晶体材料原位结构的新方法

对溶液中形成的非晶相和纳米晶相的结构研究历来具有挑战性。很少有方法能够就地原子结构分析和系统的严格控制。混流反应器 (MFR) 用于全 X 射线散射实验，以检查相的短程和长程结构就地具有对分布函数 (PDF) 分析。适应性强的实验装置能够收集一系列不同系统化学成分、初始过饱和度和停留时间的数据。分析过程中样品的老化时间是通过调节流速来控制的。更快的速率允许检查较年轻的样本，但如果流速太快，则无法获取足够的数据来平均掉多余的信号噪声。较旧的样品流速较慢，但在非常慢的速度下，颗粒会沉降并阻塞流动，从而堵塞系统。正确的背景收集和扣除对于数据优化至关重要。总体而言，这种 MFR 方法是分析就地溶液中晶体生长过程中形成的相结构。作为概念证明，收集了无定形和结晶磷酸钙以及无定形碳酸钙的高分辨率总 X 射线散射数据以进行 PDF 分析。

更新日期：2019-08-23

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