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用于表面X射线衍射和掠入射小角X射线散射研究的超高真空/高压流动反应器,接近工业催化条件。

Ultrahigh vacuum/high-pressure flow reactor for surface x-ray diffraction and grazing incidence small angle x-ray scattering studies close to conditions for industrial catalysis.

作者信息

van Rijn R, Ackermann M D, Balmes O, Dufrane T, Geluk A, Gonzalez H, Isern H, de Kuyper E, Petit L, Sole V A, Wermeille D, Felici R, Frenken J W M

机构信息

Kamerlingh Onnes Laboratory, Leiden University, P.O. Box 9504, RA Leiden 2300, The Netherlands.

出版信息

Rev Sci Instrum. 2010 Jan;81(1):014101. doi: 10.1063/1.3290420.

Abstract

A versatile instrument for the in situ study of catalyst surfaces by surface x-ray diffraction and grazing incidence small angle x-ray scattering in a 13 ml flow reactor combined with reaction product analysis by mass spectrometry has been developed. The instrument bridges the so-called "pressure gap" and "materials gap" at the same time, within one experimental setup. It allows for the preparation and study of catalytically active single crystal surfaces and is also equipped with an evaporator for the deposition of thin, pure metal films, necessary for the formation of small metal particles on oxide supports. Reactions can be studied in flow mode and batch mode in a pressure range of 100-1200 mbar and temperatures up to 950 K. The setup provides a unique combination of sample preparation, characterization, and in situ experiments where the structure and reactivity of both single crystals and supported nanoparticles can be simultaneously determined.

摘要

已开发出一种多功能仪器,用于在13毫升流动反应器中通过表面X射线衍射和掠入射小角X射线散射对催化剂表面进行原位研究,并结合质谱法对反应产物进行分析。该仪器在一个实验装置中同时弥合了所谓的“压力间隙”和“材料间隙”。它允许制备和研究具有催化活性的单晶表面,还配备了一个蒸发器,用于沉积薄的纯金属膜,这对于在氧化物载体上形成小金属颗粒是必要的。反应可以在100 - 1200毫巴的压力范围和高达950 K的温度下以流动模式和间歇模式进行研究。该装置提供了样品制备、表征和原位实验的独特组合,其中单晶和负载型纳米颗粒的结构和反应性可以同时测定。

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