Insights on Morphology and Thermal Stability of Hollow Pt Nanospheres by In Situ Environmental TEM
The fields of catalysis and energy storage nowadays quote the use of nanomaterials with well-defined size, morphology, chemical composition, and thermal stability in the high-temperature range and under harsh conditions of reactions. We present herein an approach based on in situ environmental scann...
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MDPI AG
2025-02-01
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| Series: | Molecules |
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| author | Josephine Rezkallah Xavier Sauvage Bernhard Witulski Simona Moldovan |
| author_facet | Josephine Rezkallah Xavier Sauvage Bernhard Witulski Simona Moldovan |
| author_sort | Josephine Rezkallah |
| collection | DOAJ |
| description | The fields of catalysis and energy storage nowadays quote the use of nanomaterials with well-defined size, morphology, chemical composition, and thermal stability in the high-temperature range and under harsh conditions of reactions. We present herein an approach based on in situ environmental scanning transmission electron microscopy (STEM), combined with analytical STEM and electron tomography (ET), for the evaluation of the thermal stability of hollow Pt nanospheres under vacuum and high-pressure hydrogen environments. Spherical Pt hollow nanospheres (HNSs) with an average diameter of 15 and 34 nm were synthesized by a galvanic replacement-based procedure using either steep or continuous addition of Pt salts during synthesis. The as-synthesized HNSs exhibit complex 3D structures with shells of a few nm constituted by small Pt nanoparticles and marked by the presence of open channels. The thermal stability of Pt-based HNSs under TEM vacuum and 1 bar of hydrogen flow is reported by considering microstructural changes, e.g., the build-up of a continuous shell and its evolution until HNSs collapse at elevated temperatures (>500 °C). Experimental findings are discussed considering fundamental phenomenological issues, i.e., NP faceting, NP diffusion, and subsequent NP sintering, with respect to the behavior of the systems investigated. |
| format | Article |
| id | doaj-art-9b23e077a2df4ef394568f68f3241d0c |
| institution | DOAJ |
| issn | 1420-3049 |
| language | English |
| publishDate | 2025-02-01 |
| publisher | MDPI AG |
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| series | Molecules |
| spelling | doaj-art-9b23e077a2df4ef394568f68f3241d0c2025-08-20T02:44:39ZengMDPI AGMolecules1420-30492025-02-0130479210.3390/molecules30040792Insights on Morphology and Thermal Stability of Hollow Pt Nanospheres by In Situ Environmental TEMJosephine Rezkallah0Xavier Sauvage1Bernhard Witulski2Simona Moldovan3Univ Rouen Normandie, INSA Rouen Normandie, CNRS, Normandie Univ, GPM UMR 6634, 76000 Rouen, FranceUniv Rouen Normandie, INSA Rouen Normandie, CNRS, Normandie Univ, GPM UMR 6634, 76000 Rouen, FranceLaboratoire de Chimie Moléculaire et Thio-Organique (LCMT), CNRS UMR 6507, ENSICAEN, Université de Caen, Normandie Univ, 6 Bd. Maréchal Juin, 14050 Caen, FranceUniv Rouen Normandie, INSA Rouen Normandie, CNRS, Normandie Univ, GPM UMR 6634, 76000 Rouen, FranceThe fields of catalysis and energy storage nowadays quote the use of nanomaterials with well-defined size, morphology, chemical composition, and thermal stability in the high-temperature range and under harsh conditions of reactions. We present herein an approach based on in situ environmental scanning transmission electron microscopy (STEM), combined with analytical STEM and electron tomography (ET), for the evaluation of the thermal stability of hollow Pt nanospheres under vacuum and high-pressure hydrogen environments. Spherical Pt hollow nanospheres (HNSs) with an average diameter of 15 and 34 nm were synthesized by a galvanic replacement-based procedure using either steep or continuous addition of Pt salts during synthesis. The as-synthesized HNSs exhibit complex 3D structures with shells of a few nm constituted by small Pt nanoparticles and marked by the presence of open channels. The thermal stability of Pt-based HNSs under TEM vacuum and 1 bar of hydrogen flow is reported by considering microstructural changes, e.g., the build-up of a continuous shell and its evolution until HNSs collapse at elevated temperatures (>500 °C). Experimental findings are discussed considering fundamental phenomenological issues, i.e., NP faceting, NP diffusion, and subsequent NP sintering, with respect to the behavior of the systems investigated.https://www.mdpi.com/1420-3049/30/4/792Pt hollow nanospheresin situ environmental TEMgalvanic replacement synthesiselectron tomographycatalysts |
| spellingShingle | Josephine Rezkallah Xavier Sauvage Bernhard Witulski Simona Moldovan Insights on Morphology and Thermal Stability of Hollow Pt Nanospheres by In Situ Environmental TEM Molecules Pt hollow nanospheres in situ environmental TEM galvanic replacement synthesis electron tomography catalysts |
| title | Insights on Morphology and Thermal Stability of Hollow Pt Nanospheres by In Situ Environmental TEM |
| title_full | Insights on Morphology and Thermal Stability of Hollow Pt Nanospheres by In Situ Environmental TEM |
| title_fullStr | Insights on Morphology and Thermal Stability of Hollow Pt Nanospheres by In Situ Environmental TEM |
| title_full_unstemmed | Insights on Morphology and Thermal Stability of Hollow Pt Nanospheres by In Situ Environmental TEM |
| title_short | Insights on Morphology and Thermal Stability of Hollow Pt Nanospheres by In Situ Environmental TEM |
| title_sort | insights on morphology and thermal stability of hollow pt nanospheres by in situ environmental tem |
| topic | Pt hollow nanospheres in situ environmental TEM galvanic replacement synthesis electron tomography catalysts |
| url | https://www.mdpi.com/1420-3049/30/4/792 |
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