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Batch and Flow Synthesis of CeO(2) Nanomaterials Using Solid-State Microwave Generators

Microwave-assisted synthesis in combination with flow synthesis offers an interesting approach to develop faster and more sustainable procedures for the preparation of homogeneous nanomaterials. Recently, solid-state generators of microwaves appeared as a tool with improved control over power and fr...

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Autores principales: Rodríguez-Carrillo, Cristina, Torres García, Juan, Benítez, Miriam, El Haskouri, Jamal, Amorós, Pedro, Ros-Lis, Jose V.
Formato: Online Artículo Texto
Lenguaje:English
Publicado: MDPI 2022
Materias:
Acceso en línea:https://www.ncbi.nlm.nih.gov/pmc/articles/PMC9101767/
https://www.ncbi.nlm.nih.gov/pubmed/35566060
http://dx.doi.org/10.3390/molecules27092712
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author Rodríguez-Carrillo, Cristina
Torres García, Juan
Benítez, Miriam
El Haskouri, Jamal
Amorós, Pedro
Ros-Lis, Jose V.
author_facet Rodríguez-Carrillo, Cristina
Torres García, Juan
Benítez, Miriam
El Haskouri, Jamal
Amorós, Pedro
Ros-Lis, Jose V.
author_sort Rodríguez-Carrillo, Cristina
collection PubMed
description Microwave-assisted synthesis in combination with flow synthesis offers an interesting approach to develop faster and more sustainable procedures for the preparation of homogeneous nanomaterials. Recently, solid-state generators of microwaves appeared as a tool with improved control over power and frequency. Cerium oxide, despite its excellent catalytic activity, has not been prepared before using solid-state generators or microwave-assisted flow chemistry. We report a procedure for the preparation of nanoparticulated CeO(2) (around 4 nm) under 2.45 GHz microwaves in only 30 s. The materials are further calcined at 800 °C to increase particle size, with a better defined particle size and crystallinity. The procedure was tested in batch at pH 11 and 12 and diverse potencies, and the products were characterized by TEM, XRD, DLS, and N(2) adsorption–desorption isotherms. The materials were similar at the diverse pH values and potencies. XRD confirms the crystallinity of the CeO(2) material with a fluorite-like structure. They are composed of particles around 40 nm that aggregate as structures of around 100 nm. The procedure was successfully adapted to flow synthesis, obtaining materials with structure and properties equivalent to batch synthesis. The batch and flow materials offer peroxidase properties, opening the door for their use as ROS scavengers.
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spelling pubmed-91017672022-05-14 Batch and Flow Synthesis of CeO(2) Nanomaterials Using Solid-State Microwave Generators Rodríguez-Carrillo, Cristina Torres García, Juan Benítez, Miriam El Haskouri, Jamal Amorós, Pedro Ros-Lis, Jose V. Molecules Article Microwave-assisted synthesis in combination with flow synthesis offers an interesting approach to develop faster and more sustainable procedures for the preparation of homogeneous nanomaterials. Recently, solid-state generators of microwaves appeared as a tool with improved control over power and frequency. Cerium oxide, despite its excellent catalytic activity, has not been prepared before using solid-state generators or microwave-assisted flow chemistry. We report a procedure for the preparation of nanoparticulated CeO(2) (around 4 nm) under 2.45 GHz microwaves in only 30 s. The materials are further calcined at 800 °C to increase particle size, with a better defined particle size and crystallinity. The procedure was tested in batch at pH 11 and 12 and diverse potencies, and the products were characterized by TEM, XRD, DLS, and N(2) adsorption–desorption isotherms. The materials were similar at the diverse pH values and potencies. XRD confirms the crystallinity of the CeO(2) material with a fluorite-like structure. They are composed of particles around 40 nm that aggregate as structures of around 100 nm. The procedure was successfully adapted to flow synthesis, obtaining materials with structure and properties equivalent to batch synthesis. The batch and flow materials offer peroxidase properties, opening the door for their use as ROS scavengers. MDPI 2022-04-22 /pmc/articles/PMC9101767/ /pubmed/35566060 http://dx.doi.org/10.3390/molecules27092712 Text en © 2022 by the authors. https://creativecommons.org/licenses/by/4.0/Licensee MDPI, Basel, Switzerland. This article is an open access article distributed under the terms and conditions of the Creative Commons Attribution (CC BY) license (https://creativecommons.org/licenses/by/4.0/).
spellingShingle Article
Rodríguez-Carrillo, Cristina
Torres García, Juan
Benítez, Miriam
El Haskouri, Jamal
Amorós, Pedro
Ros-Lis, Jose V.
Batch and Flow Synthesis of CeO(2) Nanomaterials Using Solid-State Microwave Generators
title Batch and Flow Synthesis of CeO(2) Nanomaterials Using Solid-State Microwave Generators
title_full Batch and Flow Synthesis of CeO(2) Nanomaterials Using Solid-State Microwave Generators
title_fullStr Batch and Flow Synthesis of CeO(2) Nanomaterials Using Solid-State Microwave Generators
title_full_unstemmed Batch and Flow Synthesis of CeO(2) Nanomaterials Using Solid-State Microwave Generators
title_short Batch and Flow Synthesis of CeO(2) Nanomaterials Using Solid-State Microwave Generators
title_sort batch and flow synthesis of ceo(2) nanomaterials using solid-state microwave generators
topic Article
url https://www.ncbi.nlm.nih.gov/pmc/articles/PMC9101767/
https://www.ncbi.nlm.nih.gov/pubmed/35566060
http://dx.doi.org/10.3390/molecules27092712
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