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MFI crystal and film growth and defects evolution: Revealed by high resolution electron microscopy: [Crecimiento de películas y cristales de MFI y evolución de defectos; revelado por microscopía electrónica de alta resolución]
Luleå University of Technology, Department of Engineering Sciences and Mathematics, Material Science.ORCID iD: 0000-0001-8663-6584
Luleå University of Technology, Department of Engineering Sciences and Mathematics, Material Science.ORCID iD: 0000-0003-4582-0902
Luleå University of Technology, Department of Civil, Environmental and Natural Resources Engineering, Chemical Engineering.ORCID iD: 0000-0002-7477-4960
Luleå University of Technology, Department of Engineering Sciences and Mathematics, Material Science.ORCID iD: 0000-0003-4888-6237
2022 (English)In: Boletín de la Sociedad Espanola de Ceramica y Vidrio, ISSN 0366-3175, E-ISSN 2173-0431, Vol. 61, no 5, p. 439-452Article in journal (Refereed) Published
Abstract [en]

Mechanism of MFI film growth from seed crystals and evolution of defects during the film growth were investigated. The hydrothermal growth of colloidal silicalite-1 crystals of 50 nm on silicon substrate was used to reveal the MFI film formation mechanism at different time intervals using high resolution-transmission electron microscopy (HR-TEM) and extreme high resolution-scanning electron microscopy (XHR-SEM). It was found that the MFI seeds started to grow in the early stages of hydrothermal treatment from 50 nm to 75 nm in size and connect to the crystals in the vicinity, showing the onset of film formation. The film growth mechanism was led by the sub-colloidal particles in the synthesis solution arriving at the crystal surfaces contributing to the film growth. A continuous film with a thickness of 100 nm was formed after 12 h of hydrothermal treatment containing pinhole defects. Pinhole defects disappeared after 24 h of hydrothermal treatment with a film thickness of 200 nm and grain boundaries thickness of 2 nm were formed. Furthermore, mesoporous defects were found in the grains of the film, which appeared due to the film growth by sub-colloidal particles of synthesis solution. The growth rate of the MFI film was calculated to 0.007 (μm/h) and compared with the crystal growth inside the synthesis solution.

Abstract [es]

Se investigó el mecanismo de crecimiento de películas de MFI a partir de cristales semilla y la evolución de los defectos durante el crecimiento de dichas películas. La síntesis hidrotérmica a partir de cristales coloidales de silicalita-1 de 50 nm sobre sustrato de silicio se utilizó para revelar el mecanismo de formación de la película de MFI en diferentes intervalos de tiempo, utilizando microscopía electrónica de transmisión de alta resolución (HR-TEM) y microscopía electrónica de barrido de extrema alta resolución (XHR-SEM). Se observó que las semillas de MFI comenzaron a crecer en las primeras etapas del tratamiento hidrotérmico de 50 a 75 nm de tamaño y se conectaron a los cristales en las cercanías, evidenciando el inicio de la formación de la película. El mecanismo de crecimiento fue dirigido por las partículas subcoloidales en la solución de síntesis que llegaron a las superficies de los cristales, contribuyendo al crecimiento de la película. Se formó una película continua con un espesor de 100 nm después de 12 h de tratamiento hidrotérmico que contenía orificios. Estos desaparecieron después de 24 h de este mismo tratamiento, habiendo alcanzado un espesor de película de 200 nm, y se formaron límites de grano de 2 nm. Además, se encontraron defectos mesoporosos que aparecieron debido al crecimiento de la película a partir de partículas subcoloidales presentes en la solución de síntesis. La tasa de crecimiento de la película de MFI se calculó en 0,007 (μm/h) y se comparó con el crecimiento de cristales dentro de la solución de síntesis.

Place, publisher, year, edition, pages
Elsevier, 2022. Vol. 61, no 5, p. 439-452
Keywords [en]
MFI film, Electron microscopy, Crystal, Nanoparticle
Keywords [es]
Película Mordenite Framework Inverted, Microscopía electrónica, Cristal, Nanopartícula
National Category
Chemical Process Engineering
Research subject
Engineering Materials; Chemical Technology
Identifiers
URN: urn:nbn:se:ltu:diva-85863DOI: 10.1016/j.bsecv.2021.03.002Scopus ID: 2-s2.0-85104518488OAI: oai:DiVA.org:ltu-85863DiVA, id: diva2:1571073
Funder
Swedish Research Council Formas, 2016-01099Swedish Research Council, 2018-04407
Note

Validerad;2022;Nivå 2;2022-11-30 (sofila)

Available from: 2021-06-22 Created: 2021-06-22 Last updated: 2023-09-05Bibliographically approved

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Nabavi, Mohammad SadeghMouzon, JohanneZhou, MingAkhtar, Farid

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