Dries Vandenabeele, Nikolaus Doppelhammer, Martin Rosenthal, Wauter Wangermez, Bernhard Jakoby, Christine Kirschhock, Eric Breynaert
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引用次数: 0
Abstract
A simple and robust high-pressure cell designed for in situ transmission X-ray crystallization studies is presented. The performance of the cell for in situ small/wide-angle X-ray scattering experiments and microscopy imaging is demonstrated for zeolite crystallization from highly alkaline hydrated silicate ionic liquids at 500 K and 150 bar N2 pressure. The simple design in combination with commercial finger-tight connections allows for convenient sample loading of powders, liquids and gases. The cell can be used in dead-end or flow-through mode and can be pressurized with gases or liquids via standard high-performance liquid chromatography capillary tubing. The capillaries are easily cleaned or replaced. The wetted parts are polyether ether ketone and sapphire, which are resistant to many corrosive substances, thus enabling in situ characterization under challenging conditions.
介绍了一种用于原位透射x射线结晶研究的简单而坚固的高压电池。在500 K和150 bar N2压力下,高碱性水合硅酸盐离子液体的沸石结晶实验证明了该电池在原位小/广角x射线散射实验和显微镜成像中的性能。简单的设计与商业手指紧连接相结合,可以方便地装载粉末,液体和气体样品。该细胞可在终端或流动模式下使用,并可通过标准的高性能液相色谱毛细管对气体或液体进行加压。毛细血管很容易清洗或更换。浸湿的部分是聚醚醚酮和蓝宝石,它们可以抵抗许多腐蚀性物质,从而能够在具有挑战性的条件下进行原位表征。
期刊介绍:
Many research topics in condensed matter research, materials science and the life sciences make use of crystallographic methods to study crystalline and non-crystalline matter with neutrons, X-rays and electrons. Articles published in the Journal of Applied Crystallography focus on these methods and their use in identifying structural and diffusion-controlled phase transformations, structure-property relationships, structural changes of defects, interfaces and surfaces, etc. Developments of instrumentation and crystallographic apparatus, theory and interpretation, numerical analysis and other related subjects are also covered. The journal is the primary place where crystallographic computer program information is published.