实现用于实验室源X射线反射率测量的温度控制原位蒸汽注入
Enabling temperature controlled in-situ vapor dosing for lab source X-ray reflectivity measurements
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中文总结 AI 辅助
研究针对XRR测量在实验室衍射仪上受限的问题，提出一种能进行原位蒸汽注入和温度相关实验的XRR透射池，通过案例研究展示其能力，建立了温度控制蒸汽注入的新方法，具备多种优势。
中文摘要 AI 辅助
X射线反射率（XRR）是探测与薄膜、膜和电池应用等相关复杂系统中埋藏界面的重要技术。然而，许多操作中和原位反射率测量池专为同步加速器设施设计，限制了这些测量的广泛可及性。我们展示了一种XRR透射池，可在实验室衍射仪上进行原位蒸汽注入和温度相关实验。通过两个案例研究证明了其能力：水在硅上聚酰胺（PA）膜中的吸附以及氧化铝上聚苯乙烯（PS）伪刷的温度相关重构。蒸汽注入可控制蒸汽释放，能在从粗真空到饱和的广泛条件下运行。歧管能达到饱和压力的90 - 95%，测量范围为0 - 250毫巴。在25至200摄氏度间的加热研究表明能分辨表面结合聚合物中埃级结构变化。这些结果建立了一种在实验室衍射仪上进行温度控制蒸汽注入的新型简化方法，提供直接的探针分子交换、真空密封操作和可变温度能力。
英文摘要
X-ray Reflectivity (XRR) is a valuable technique for probing buried interfaces in complex systems relevant to thin-film, membrane, and battery applications, among others. However, many operando and in situ reflectivity cells are designed for use at synchrotron facilities, limiting the broader accessibility of these measurements. We present an XRR transmission cell that enables in situ vapor dosing and temperature-dependent experiments on in-house diffractometers. We demonstrate its capabilities with two case studies: the adsorption of water into polyamide (PA) membranes on silicon and temperature-dependent restructuring of polystyrene (PS) pseudo brushes on alumina. Vapor dosing allows for controlled release of vapor into the cell, allowing operation across a wide range of conditions from rough vacuum to saturation. We demonstrate that the manifold can reach 90-95% of saturated pressures, with the measurements presented here spanning 0-250 mbar, which is desirable for adsorption isotherms. Heating studies performed between 25 and 200C demonstrate the ability to resolve Ångstrom scale structural changes in a surface bound polymer. These results establish a novel streamlined approach to temperature controlled vapor dosing on a laboratory diffractometer, offering straightforward probe-molecule exchange, vacuum-sealed operations, and variable temperature capabilities.
