Operando Microscopy 10:00 - 12:00 Thursday, 8Th July, 2021 Sessions Conference Session Session Organiser Hannah Nerl

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Operando Microscopy 10:00 - 12:00 Thursday, 8Th July, 2021 Sessions Conference Session Session Organiser Hannah Nerl Stream 3: Operando Microscopy 10:00 - 12:00 Thursday, 8th July, 2021 Sessions Conference Session Session Organiser Hannah Nerl Functional materials cannot be studied reliably when removing materials from their reaction environment. Recent operando studies aim to address this by correlating structure and function of materials under working conditions. Significant technical advances in instrumentation have led to the development and improvement of a range of operando techniques with great impact across scientific fields. These operando approaches have already been shown to allow for the visualization and analysis of materials during synthesis, degradation or function in well-defined environments. Aside from electron microscopy, relevant examples of emerging and improved operando techniques include X-ray microscopy, scanning probe microscopy, light microscopy and atomic force microscopy. This session will contain contributed and invited talks and posters that aim to highlight recent technical advances in operando approaches and the resulting science while studying a range of materials including 2D materials, nanoparticles and catalysts. 10:00 - 10:30 31 Seeing is believing: atomic-scale imaging of catalysts under reaction conditions Dr. Irene Groot Leiden Institute of Chemistry, Leiden University, Leiden, Netherlands Abstract Text The atomic-scale structure of a catalyst under reaction conditions determines its activity, selectivity, and stability. Recently it has become clear that essential differences can exist between the behavior of catalysts under industrial conditions (high pressure and temperature) and the (ultra)high vacuum conditions of traditional laboratory experiments. Differences in structure, composition, reaction mechanism, activity, and selectivity have been observed. These observations made it clear that meaningful results can only be obtained at high pressures and temperatures. Therefore, the last years have seen a tremendous effort in designing new instruments and adapting existing ones to be able to investigate catalysts in situ under industrially relevant conditions. In this talk, I will give an overview of the in situ imaging techniques we use to study the structure of model catalysts under atmospheric pressures and elevated temperatures. We have developed setups that combine an ultrahigh vacuum environment for model catalyst preparation and characterization with a high-pressure flow reactor cell, integrated with either a scanning tunneling microscope or an atomic force microscope. With these setups we are able to perform atomic-scale investigations of well-defined model catalysts under industrial conditions. Additionally, we combine the structural information from scanning probe microscopy with mass spectrometry measurements. In this way, we can correlate structural changes of the catalyst due to the gas composition with its catalytic performance. Furthermore, we use other in situ imaging techniques such as transmission electron microscopy, surface X-ray diffraction, and optical microscopy, all combined with mass spectrometry. In addition, we make use of near-ambient-pressure X-ray photoelectron spectroscopy to obtain chemical information on the model catalysts during reaction. Scientific cases that I will discuss are hydrodesulfurization of S-containing organic molecules on (Co-promoted) MoS2 and graphene growth on liquid copper. Keywords in situ measurements, scanning probe microscopy, optical microscopy, model catalyst, hydrodesulfurization, graphene growth, surface science, heterogeneous catalysis 10:30 - 10:42 247 In-situ hydration of calcium sulfate and the phase transformation pathways of bassanite to gypsum Dr Martha Ilett1, Dr Helen Freeman1, Dr Johanna Galloway1, Dr Zabeada Aslam1, Dr Ian McPherson2, Dr Oscar Céspedes1, Dr Yi-Yeoun Kim 1, Professor Fiona Meldrum1, Professor Rik Drummond-Brydson1 1University of Leeds, Leeds, United Kingdom. 2University of Warwick, Warwick, United Kingdom Abstract Text The nucleation, growth, and phase transformation of calcium sulfate must be understood to improve the performance of construction materials, reduce scaling in industrial processes and better understand the natural environment. Recent studies suggest that classical nucleation theory does not apply to calcium sulfate systems where a multi-stage process occurs instead, involving several intermediate phases. Through a variety of in-situ experimental work, there is a growing body of evidence which shows an oriented-attachment-like crystallisation process. In this work we have used advanced in-situ electron microscopy to study the phase transformation in real time to understand the mechanistic processes involved. Both liquid cell (LC) and cryogenic (cryo) transmission electron microscopy (TEM) were used to monitor the phase transformation of bassanite (calcium sulfate hemihydrate CaSO4·0.5H2O) to gypsum (calcium sulfate dihydrate CaSO4·2H2O) during hydration in an aqueous, undersaturated calcium sulfate solution. An FEI Titan3 Themis G2 operating at 300 kV and equipped with a Gatan OneView CCD was used for in-situ electron microscopy studies, alongside Raman spectroscopy of both bulk and confined calcium sulfate systems. By collecting real-time images and videos using LCTEM we have been able to follow the aggregation and alignment of bassanite nanoparticles at the nanoscale. When coupled with Raman spectroscopy our results show there is a period where the two phases (bassanite and gypsum) co-exist. In addition, comparisons between LCTEM and cryo-TEM will allow us to evaluate any beam induced changes in LCTEM where it would be predicted these would be ‘frozen out’ in cryo-TEM. Early comparisons between the two techniques using a model nanoparticle system suggest beam induced dissolution observed in LCTEM and caused by changes in pH can be prevented using cryo-TEM. Ultimately, this work has allowed real time observation of the phase transformation of bassanite to gypsum alongside comparisons between LC and cryo TEM, which can advance the application of both techniques within materials science research. Keywords Calcium sulfate In situ TEM 10:47 - 10:59 205 Direct observation of the chemical dynamics of Pt nanoparticles in CO oxidation reaction by operando TEM Dr. Milivoj Plodinec1,2, Dr. Hannah C. Nerl3, Dr. Thomas Lunkenbein2, Prof. Dr. Robert Schlögl2,4 1ETH Zurich, ScopeM, Zurich, Switzerland. 2Fritz-Haber Institute of the Max-Planck Society, Department of Inorganic Chemistry, Berlin, Germany. 3Humboldt-Universität zu Berlin, Department of Physics, Berlin, Germany. 4Max Planck Institute for Chemical Energy Conversion, Mülheim an der Ruhr, Germany Abstract Text Introduction Up to date, regardless of our advances in synthesis and characterization methods, the empirical approach towards the discovery of new catalysts still prevails. Clearly, this is a very inefficient and time-consuming endeavor. The key point still missing is the knowledge of the structure-function relationships of catalysts. Without that, the often-claimed tailored design of catalysts partially remains in the domain of wishful thinking.1 Moreover, the capability to design novel and more efficient catalysts is limited by the lack of a detailed understanding of catalytic reactions on an atomic scale, particularly since catalyst dynamic active structures and surfaces under reaction conditions are mostly unknown.1,2 The only way to probe the catalyst working state is to use operando characterization techniques. Recently, many studies have shown that catalysts are metastable and dynamic systems, where the nature of the active state depends on the applied chemical potential and associated “chemical dynamics”, and the formation of transient active sites.1,3-5 Thus, the morphological and structural changes which relate to the induced surface and bulk transformations of the catalyst can be defined by the term chemical dynamics.1,3 Moreover, since the working catalysts are thought to be metastable, the active surfaces could be unstable at non-active conditions, which could lead to the detection of inactive structures by ex situ studies. Therefore, catalysts should be exclusively studied in their working state, under operando conditions. Methods and Materials For the experiment, we use a homebuilt gas feed and analysis system coupled with a quadrupole mass spectrometer (QMS, with a response time < 20s) and using commercially available gas flow TEM holder for the catalytic reactions inside the column of an aberration-corrected 300 kV FEI Titan (scanning) transmission electron (STEM).3 Using this system, we are able to correlate structural and morphological changes of catalysts with activity in the pressure between 20-1000 mbar, and in the temperature between 20-1000°C. The studied platinum catalysts were prepared either in situ by the thermal decomposition of tetraamineplatinum(II) nitrate 3,4 in synthetic air: 20%O2 in helium (He), at 400°C for 3h (Figure 1a) or ex situ by magnetron sputtering of Pt nanoparticles (NPs) directly on the top of SiNx membrane of microelectromechanical system (MEMS) chip (Figure 1b). The reaction conditions for CO oxidation were: temperature ramp 1°C/min and 2°C/min, pressure:700 mbar, flow rate: 20 mL/min, and gas feed: CO:O2:He = 1:5:19. Result and discussion In this study, we will show that using operando TEM approach we are able to visualize changes of Pt catalysts with different NPs shapes and sizes during different activity regimes. Moreover that we are able to directly correlate differences in conversion rates
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