This paper describes new sample cells and techniques for in situ powder X-ray diffraction specifically designed for gas absorption studies up to ca 300 bar (1 bar = 100 000 Pa) gas pressure. The cells are for multipurpose use, in particular the study of solid-gas reactions in dosing or flow mode, but can also handle samples involved in solid-liquid-gas studies. The sample can be loaded into a single-crystal sapphire (Al2O3) capillary, or a quartz (SiO2) capillary closed at one end. The advantages of a sapphire single-crystal cell with regard to rapid pressure cycling are discussed, and burst pressures are calculated and measured to be 300 bar. An alternative and simpler cell based on a thin-walled silicate or quartz glass capillary, connected to a gas source via a VCR fitting, enables studies up to 100 bar. Advantages of the two cell types are compared and their applications are illustrated by case studies.
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机译:本文介绍了用于原位粉末X射线衍射的新样品池和技术,这些样品池和技术专门设计用于最高300 bar(1 bar = 100 000 Pa)气压的气体吸收研究。该池具有多种用途,特别是在定量或流动模式下研究固-气反应,但也可以处理涉及固-液-气研究的样品。可以将样品加载到单晶蓝宝石(Al2O3)毛细管或一端封闭的石英(SiO2)毛细管中。讨论了蓝宝石单晶电池在快速压力循环方面的优势,爆裂压力经计算和测量为300 bar。另一种基于薄壁硅酸盐或石英玻璃毛细管的替代且更简单的样品池,通过VCR配件连接到气源,可进行高达100 bar的研究。比较了两种电池类型的优势,并通过案例研究说明了它们的应用。
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