XAFS & IR data from publication entitled: A High Pressure Operando Spectroscopy Examination of Bimetal Interactions in ‘Metal Efficient’ Palladium/In2O3/Al2O3 Catalysts for CO2 hydrogenation

.xlsx spreadsheets with ascii data recorded during reduction and reaction.

 X-ray absorption spectroscopy was performed at Diamond Light Source, UK, at B18, through proposal SP30647 (August 2022) for the Pd/Al2O3, Pd/TiO2 and Pd/In2O3/Al2O3 species. Data was collected at the Pd and In K-edges in transmission mode using a QEXAFS setup with fast scanning Si(311) crystal monochromators. The time resolution here was roughly 90 seconds per spectrum. Samples were packed into an in-house custom-made capillary system designed and constructed by Diamond Light Source. 50 mg of 200-300 μm catalyst particles were packed between 3 cm of quartz wool.

DRIFTS measurements were performed on a Bruker VERTEX 80 system, with a custom-built high-pressure dome, capable of holding 25 bar of pressure within a high pressure chamber DiffusIRTM PIKE Technologies accessory. Argon and a 25% CO2/75% H2 mixture gas were delivered through high pressure EL-FLOW® Bronkhorst mass-flow controllers, into an in-house custom-made gas manifold. 30 mg of sample was used for the measurements. Initially, the sample was reduced in 25 mL/min of 25% H2 and 75 % Ar. The system was heated to 300 °C at a ramp rate of 5 °C/min and held for 1 hour. The samples were then cooled to 30 °C and either pressurised to 20 bar with 30 mL/min of 75% H2 and 25 % CO2 for the 20 bar measurements or kept at atmospheric pressure for the 1 bar measurements. Once the intended final pressure was reached, the system was heated at 10 °C/min, while holding at 50, 100, 150, 175, 200, 225, 250, 275 and 300 °C for 30 minutes for spectra to be collected. Mass-spectrometry data was collected throughout to observe the evolution of different species, using a Pfeiffer OmniStar.

采用 ASCII 格式记录的.xlsx 电子表格数据，涵盖了在反应和还原过程中所收集的数据。
X射线吸收光谱学实验在英国的 Diamond Light Source 的 B18 室进行，实验提案编号为 SP30647（2022年8月），针对 Pd/Al2O3、Pd/TiO2 以及 Pd/In2O3/Al2O3 物种。数据采集是在 Pd 和 In 的 K 边缘，通过透射模式，使用配备快速扫描 Si(311) 晶体单色器的 QEXAFS 设备完成的。每个光谱的时间分辨率约为 90 秒。样品被装入由 Diamond Light Source 设计和构建的定制毛细管系统中。在 3 厘米石英棉之间填充了 50 毫克的 200-300 微米催化剂颗粒。
在 Bruker VERTEX 80 系统上进行了 DRIFTS 测量，该系统配备了一个定制的高压穹顶，能够在高压室内的 DiffusIRTM PIKE Technologies 附件中承受高达 25 巴的压力。通过高压 EL-FLOW® Bronkhorst 质量流量控制器，将氩气和 25% CO2/75% H2 混合气体输送至定制的气体歧管。测量使用了 30 毫克的样品。最初，样品在 25 mL/min 的 25% H2 和 75% Ar 气氛下还原。系统以 5 °C/min 的升温速率加热至 300 °C，并保持 1 小时。随后，样品被冷却至 30 °C，并通过 30 mL/min 的 75% H2 和 25% CO2 将压力增加到 20 巴，以进行 20 巴的测量；或者保持在大气压力下进行 1 巴的测量。达到预定最终压力后，系统以 10 °C/min 的速率加热，同时在 50、100、150、175、200、225、250、275 和 300 °C 下保持 30 分钟，以收集光谱。使用 Pfeiffer OmniStar 进行了质谱数据收集，以观察不同物种的演变。