We present a comprehensive scale-bridging characterization approach for supported catalytically active liquid metal solutions (SCALMS) which combines lab-based X-ray microscopy, nano X-ray computed tomography (nano-CT), and correlative analytical transmission electron microscopy. SCALMS catalysts consist of low-melting alloy particles and have demonstrated high catalytic activity, selectivity, and long-term stability in propane dehydrogenation (PDH). We established an identical-location nano-CT workflow which allows us to reveal site-specific changes of Ga–Pt SCALMS before and after PDH. These observations are complemented by analytical transmission electron microscopy investigations providing information on the structure, chemical composition, and phase distribution of individual SCALMS particles. Key findings of this combined microscopic approach include (i) structural evolution of the SCALMS particles’ GaO_x shell, (ii) Pt segregation toward the oxide shell leading to the formation of Ga–Pt intermetallic phases, and (iii) cracking of the oxide shell accompanied by the release of liquid Ga–Pt toward the porous support.

中文翻译：

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Ga-Pt 支撑的催化活性液态金属溶液中 GaOx 壳和金属间相的结构演化

我们提出了一种用于支持催化活性液态金属溶液 (SCALMS) 的全面尺度桥接表征方法，该方法结合了基于实验室的 X 射线显微镜、纳米 X 射线计算机断层扫描 (nano-CT) 和相关分析透射电子显微镜。 SCALMS 催化剂由低熔点合金颗粒组成，在丙烷脱氢 (PDH) 中表现出高催化活性、选择性和长期稳定性。我们建立了相同位置的纳米 CT 工作流程，使我们能够揭示 PDH 前后 Ga-Pt SCALMS 的位点特异性变化。这些观察得到分析透射电子显微镜研究的补充，提供有关单个 SCALMS 颗粒的结构、化学成分和相分布的信息。这种组合微观方法的主要发现包括 (i) SCALMS 颗粒 GaO _x壳的结构演变，(ii) Pt 偏向氧化物壳，导致形成 Ga-Pt 金属间相，以及 (iii) 氧化物破裂壳伴随着液态 Ga-Pt 向多孔载体的释放。