Roorda Tycho, Achour Hamed, van Spronsen Matthijs A, Cañas-Ventura Marta E, Roobol Sander B, Onderwaater Willem, Bergman Mirthe, van der Tuijn Peter, van Baarle Gertjan, Bakker Johan W, Frenken Joost W M, Groot Irene M N
Leiden Institute of Chemistry, Leiden University, Rapenburg 70, Leiden, 2311 EZ, Netherlands.
Leiden Institute of Physics, Leiden University, Rapenburg 70, Leiden, 2311 EZ, Netherlands.
Beilstein J Nanotechnol. 2025 Mar 21;16:397-406. doi: 10.3762/bjnano.16.30. eCollection 2025.
Previous work has shown the ReactorSTM and ReactorAFM, capable of studying materials under industrially relevant conditions. Here we show current developments of the ReactorAFM/STM, implementing a qPlus sensor to add the ability of combining atomic force microscopy (AFM) and scanning tunneling microscopy (STM) techniques to study the geometric and electronic structure of materials under reaction conditions. We demonstrate this by imaging a Pd(100) single crystal at 450 K with combined AFM/STM. The surface is compared under ultrahigh vacuum and under 0.5 bar O pressure showing a notable increase in RMS current, which we attribute to oxidation. Also, we study cobalt nanoparticle catalysts on an aluminum oxide support, industrially relevant in the Fischer-Tropsch synthesis. The catalysts are imaged before and after reaction at 430 K as the current maximum temperature of the qPlus sensor used falls just below the reaction temperature. Quadrupole mass spectrometry data show the reaction taking place by monitoring product gases during heating and cooling of the sample under CO and H gas pressures of 2 bar. The monitored gases include HO as byproduct and the hydrocarbons ethane (/ = 30), propane (/ = 44), and hexane (/ = 86), which all show increases in counts while between 490 and 550 K. The added ability to scan various surfaces with combined AFM/STM while monitoring the reaction products demonstrates the versatility offered by the ReactorAFM/STM to study catalysts under realistic industrial conditions.
先前的工作已经表明，反应式扫描隧道显微镜（ReactorSTM）和反应式原子力显微镜（ReactorAFM）能够在与工业相关的条件下研究材料。在此，我们展示了反应式原子力显微镜/扫描隧道显微镜（ReactorAFM/STM）的当前进展，它采用了qPlus传感器，增加了结合原子力显微镜（AFM）和扫描隧道显微镜（STM）技术的能力，以研究反应条件下材料的几何和电子结构。我们通过在450 K下对Pd(100)单晶进行联合AFM/STM成像来证明这一点。在超高真空和0.5 bar O压力下对表面进行了比较，结果显示均方根电流显著增加，我们将其归因于氧化。此外，我们研究了用于费托合成的、与工业相关的负载在氧化铝载体上的钴纳米颗粒催化剂。由于所使用的qPlus传感器的当前最高温度略低于反应温度，因此在430 K下对催化剂在反应前后进行了成像。四极质谱数据通过在2 bar的CO和H气体压力下监测样品加热和冷却过程中的产物气体来显示反应的发生。监测的气体包括作为副产物的H₂O以及碳氢化合物乙烷（m/z = 30）、丙烷（m/z = 44）和己烷（m/z = 86），在490至550 K之间，它们的计数均有所增加。在监测反应产物的同时，利用联合AFM/STM扫描各种表面的附加能力证明了反应式原子力显微镜/扫描隧道显微镜（ReactorAFM/STM）在实际工业条件下研究催化剂方面所提供的多功能性。
