Nayak Chandrani, Jain Preeti, Vinod C P, Jha S N, Bhattacharyya D
Atomic and Molecular Physics Division, Bhabha Atomic Research Centre, Mumbai 400085, India.
Catalysis and Inorganic Chemistry Division, CSIR - National Chemical Laboratory, Dr Homi Bhabha Road, Pune 411008, India.
J Synchrotron Radiat. 2019 Jan 1;26(Pt 1):137-144. doi: 10.1107/S1600577518015588.
This article describes the setting up of a facility on the energy-scanning EXAFS beamline (BL-09) at RRCAT, Indore, India, for operando studies of structure-activity correlation during a catalytic reaction. The setup was tested by operando X-ray absorption spectroscopy (XAS) studies performed on a Co-based catalyst during the Fischer-Tropsch reaction to obtain information regarding structural changes in the catalyst during the reaction. Simultaneous gas chromatography (GC) measurements during the reaction facilitate monitoring of the product gases, which in turn gives information regarding the activity of the catalyst. The combination of XAS and GC techniques was used to correlate the structural changes with the activity of the catalyst at different reaction temperatures. The oxide catalyst was reduced to the metallic phase by heating at 400°C for 5 h under H at ambient pressure and subsequently the catalytic reaction was studied at four different temperatures of 240, 260, 280 and 320°C. The catalyst was studied for 10 h at 320°C and an attempt has been made to understand the process of its deactivation from the XANES and EXAFS results.
本文描述了在印度印多尔的RRCAT的能量扫描扩展X射线吸收精细结构谱线（BL-09）上建立一个用于催化反应过程中结构-活性相关性原位研究的装置。通过在费托反应期间对钴基催化剂进行原位X射线吸收光谱（XAS）研究来测试该装置，以获取有关反应过程中催化剂结构变化的信息。反应期间同时进行的气相色谱（GC）测量有助于监测产物气体，这反过来又提供了有关催化剂活性的信息。XAS和GC技术的结合用于在不同反应温度下将结构变化与催化剂活性相关联。在室温常压下于氢气中400°C加热5小时将氧化物催化剂还原为金属相，随后在240、260、280和320°C这四个不同温度下研究催化反应。在320°C下对催化剂进行了10小时的研究，并已尝试根据XANES和EXAFS结果了解其失活过程。
