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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Main Authors: Josephine Rezkallah, Xavier Sauvage, Bernhard Witulski, Simona Moldovan
Format: Article
Language:English
Published: MDPI AG 2025-02-01
Series:Molecules
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Online Access:https://www.mdpi.com/1420-3049/30/4/792
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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.
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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
work_keys_str_mv AT josephinerezkallah insightsonmorphologyandthermalstabilityofhollowptnanospheresbyinsituenvironmentaltem
AT xaviersauvage insightsonmorphologyandthermalstabilityofhollowptnanospheresbyinsituenvironmentaltem
AT bernhardwitulski insightsonmorphologyandthermalstabilityofhollowptnanospheresbyinsituenvironmentaltem
AT simonamoldovan insightsonmorphologyandthermalstabilityofhollowptnanospheresbyinsituenvironmentaltem