Upscaling the urea method synthesis of CoAl layered double hydroxides
- Autores
- Jaramillo Hernández, Camilo; Oestreicher, Víctor; Mizrahi, Martin Daniel; Abellán, Gonzalo
- Año de publicación
- 2023
- Idioma
- inglés
- Tipo de recurso
- artículo
- Estado
- versión publicada
- Descripción
- Research on two-dimensional materials is one of the most relevant fields in materials science. Layered double hydroxides (LDHs), a versatile class of anionic clays, exhibit great potential in photocatalysis, energy storage and conversion, and environmental applications. However, its implementation in real-life devices requires the development of efficient and reproducible large-scale synthesis processes. Unfortunately, reliable methods that allow for the production of large quantities of two-dimensional LDHs with well-defined morphologies and high crystallinity are very scarce. In this work, we carry out a scale-up of the urea-based CoAl-LDH synthesis method. We thoroughly study the effects of the mass scale-up (25-fold: up to 375 mM) and the volumetric scale-up (20-fold: up to 2 L). For this, we use a combination of several structural (XRD, TGA, and N2 and CO2 isotherms), microscopic (SEM, TEM, and AFM), magnetic (SQUID), and spectroscopic techniques (ATR-FTIR, UV–vis, XPS, ICP-MS, and XANES-EXAFS). In the case of the volumetric scale-up, a reduction of 45% in the lateral dimensions of the crystals (from 3.7 to 2.0 µm) is observed as the reaction volume increases. This fact is related to modified heating processes affecting the alkalinization rates and, concomitantly, the precipitation, even under recrystallization at high temperatures. In contrast, for the tenfold mass scale-up, similar morphological features were observed and assigned to changes in nucleation and growth. However, at higher concentrations, simonkolleite-like Co-based layered hydroxide impurities are formed, indicating a phase competition during the precipitation related to the thermodynamic stability of the growing phases. Overall, this work demonstrates that it is possible to upscale the synthesis of high-quality hexagonal CoAl-LDH in a reproducible manner. It highlights the most critical synthesis aspects that must be controlled and provides various fingerprints to trace the quality of these materials. These results will contribute to bringing the use of these 2D layered materials closer to reality in different applications of interest.
Fil: Jaramillo Hernández, Camilo. Universidad de Valencia. Instituto de Ciencia Molecular.;
Fil: Oestreicher, Víctor. Universidad de Valencia. Instituto de Ciencia Molecular.;
Fil: Mizrahi, Martin Daniel. Universidad Nacional de La Plata. Facultad de Ingeniería. Departamento de Ciencias Básicas; Argentina. Consejo Nacional de Investigaciones Científicas y Técnicas. Centro Científico Tecnológico Conicet - La Plata. Instituto de Investigaciones Fisicoquímicas Teóricas y Aplicadas. Universidad Nacional de La Plata. Facultad de Ciencias Exactas. Instituto de Investigaciones Fisicoquímicas Teóricas y Aplicadas; Argentina
Fil: Abellán, Gonzalo. Universidad de Valencia. Instituto de Ciencia Molecular.; - Materia
-
CoAl LDH
UPSCALING PROCESS
STRUCTURAL STUDY
XAS - Nivel de accesibilidad
- acceso abierto
- Condiciones de uso
- https://creativecommons.org/licenses/by/2.5/ar/
- Repositorio
- Institución
- Consejo Nacional de Investigaciones Científicas y Técnicas
- OAI Identificador
- oai:ri.conicet.gov.ar:11336/227863
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Upscaling the urea method synthesis of CoAl layered double hydroxidesJaramillo Hernández, CamiloOestreicher, VíctorMizrahi, Martin DanielAbellán, GonzaloCoAl LDHUPSCALING PROCESSSTRUCTURAL STUDYXAShttps://purl.org/becyt/ford/1.4https://purl.org/becyt/ford/1Research on two-dimensional materials is one of the most relevant fields in materials science. Layered double hydroxides (LDHs), a versatile class of anionic clays, exhibit great potential in photocatalysis, energy storage and conversion, and environmental applications. However, its implementation in real-life devices requires the development of efficient and reproducible large-scale synthesis processes. Unfortunately, reliable methods that allow for the production of large quantities of two-dimensional LDHs with well-defined morphologies and high crystallinity are very scarce. In this work, we carry out a scale-up of the urea-based CoAl-LDH synthesis method. We thoroughly study the effects of the mass scale-up (25-fold: up to 375 mM) and the volumetric scale-up (20-fold: up to 2 L). For this, we use a combination of several structural (XRD, TGA, and N2 and CO2 isotherms), microscopic (SEM, TEM, and AFM), magnetic (SQUID), and spectroscopic techniques (ATR-FTIR, UV–vis, XPS, ICP-MS, and XANES-EXAFS). In the case of the volumetric scale-up, a reduction of 45% in the lateral dimensions of the crystals (from 3.7 to 2.0 µm) is observed as the reaction volume increases. This fact is related to modified heating processes affecting the alkalinization rates and, concomitantly, the precipitation, even under recrystallization at high temperatures. In contrast, for the tenfold mass scale-up, similar morphological features were observed and assigned to changes in nucleation and growth. However, at higher concentrations, simonkolleite-like Co-based layered hydroxide impurities are formed, indicating a phase competition during the precipitation related to the thermodynamic stability of the growing phases. Overall, this work demonstrates that it is possible to upscale the synthesis of high-quality hexagonal CoAl-LDH in a reproducible manner. It highlights the most critical synthesis aspects that must be controlled and provides various fingerprints to trace the quality of these materials. These results will contribute to bringing the use of these 2D layered materials closer to reality in different applications of interest.Fil: Jaramillo Hernández, Camilo. Universidad de Valencia. Instituto de Ciencia Molecular.;Fil: Oestreicher, Víctor. Universidad de Valencia. Instituto de Ciencia Molecular.;Fil: Mizrahi, Martin Daniel. Universidad Nacional de La Plata. Facultad de Ingeniería. Departamento de Ciencias Básicas; Argentina. Consejo Nacional de Investigaciones Científicas y Técnicas. Centro Científico Tecnológico Conicet - La Plata. Instituto de Investigaciones Fisicoquímicas Teóricas y Aplicadas. Universidad Nacional de La Plata. Facultad de Ciencias Exactas. Instituto de Investigaciones Fisicoquímicas Teóricas y Aplicadas; ArgentinaFil: Abellán, Gonzalo. Universidad de Valencia. Instituto de Ciencia Molecular.;Beilstein Institute for the Advancement of Chemical Sciences2023-09info:eu-repo/semantics/articleinfo:eu-repo/semantics/publishedVersionhttp://purl.org/coar/resource_type/c_6501info:ar-repo/semantics/articuloapplication/pdfapplication/pdfhttp://hdl.handle.net/11336/227863Jaramillo Hernández, Camilo; Oestreicher, Víctor; Mizrahi, Martin Daniel; Abellán, Gonzalo; Upscaling the urea method synthesis of CoAl layered double hydroxides; Beilstein Institute for the Advancement of Chemical Sciences; Beilstein Journal of Nanotechnology; 14; 9-2023; 927-9382190-4286CONICET DigitalCONICETenginfo:eu-repo/semantics/altIdentifier/url/https://www.beilstein-journals.org/bjnano/articles/14/76info:eu-repo/semantics/altIdentifier/doi/10.3762/bjnano.14.76info:eu-repo/semantics/openAccesshttps://creativecommons.org/licenses/by/2.5/ar/reponame:CONICET Digital (CONICET)instname:Consejo Nacional de Investigaciones Científicas y Técnicas2025-10-15T15:19:13Zoai:ri.conicet.gov.ar:11336/227863instacron:CONICETInstitucionalhttp://ri.conicet.gov.ar/Organismo científico-tecnológicoNo correspondehttp://ri.conicet.gov.ar/oai/requestdasensio@conicet.gov.ar; lcarlino@conicet.gov.arArgentinaNo correspondeNo correspondeNo correspondeopendoar:34982025-10-15 15:19:13.639CONICET Digital (CONICET) - Consejo Nacional de Investigaciones Científicas y Técnicasfalse |
dc.title.none.fl_str_mv |
Upscaling the urea method synthesis of CoAl layered double hydroxides |
title |
Upscaling the urea method synthesis of CoAl layered double hydroxides |
spellingShingle |
Upscaling the urea method synthesis of CoAl layered double hydroxides Jaramillo Hernández, Camilo CoAl LDH UPSCALING PROCESS STRUCTURAL STUDY XAS |
title_short |
Upscaling the urea method synthesis of CoAl layered double hydroxides |
title_full |
Upscaling the urea method synthesis of CoAl layered double hydroxides |
title_fullStr |
Upscaling the urea method synthesis of CoAl layered double hydroxides |
title_full_unstemmed |
Upscaling the urea method synthesis of CoAl layered double hydroxides |
title_sort |
Upscaling the urea method synthesis of CoAl layered double hydroxides |
dc.creator.none.fl_str_mv |
Jaramillo Hernández, Camilo Oestreicher, Víctor Mizrahi, Martin Daniel Abellán, Gonzalo |
author |
Jaramillo Hernández, Camilo |
author_facet |
Jaramillo Hernández, Camilo Oestreicher, Víctor Mizrahi, Martin Daniel Abellán, Gonzalo |
author_role |
author |
author2 |
Oestreicher, Víctor Mizrahi, Martin Daniel Abellán, Gonzalo |
author2_role |
author author author |
dc.subject.none.fl_str_mv |
CoAl LDH UPSCALING PROCESS STRUCTURAL STUDY XAS |
topic |
CoAl LDH UPSCALING PROCESS STRUCTURAL STUDY XAS |
purl_subject.fl_str_mv |
https://purl.org/becyt/ford/1.4 https://purl.org/becyt/ford/1 |
dc.description.none.fl_txt_mv |
Research on two-dimensional materials is one of the most relevant fields in materials science. Layered double hydroxides (LDHs), a versatile class of anionic clays, exhibit great potential in photocatalysis, energy storage and conversion, and environmental applications. However, its implementation in real-life devices requires the development of efficient and reproducible large-scale synthesis processes. Unfortunately, reliable methods that allow for the production of large quantities of two-dimensional LDHs with well-defined morphologies and high crystallinity are very scarce. In this work, we carry out a scale-up of the urea-based CoAl-LDH synthesis method. We thoroughly study the effects of the mass scale-up (25-fold: up to 375 mM) and the volumetric scale-up (20-fold: up to 2 L). For this, we use a combination of several structural (XRD, TGA, and N2 and CO2 isotherms), microscopic (SEM, TEM, and AFM), magnetic (SQUID), and spectroscopic techniques (ATR-FTIR, UV–vis, XPS, ICP-MS, and XANES-EXAFS). In the case of the volumetric scale-up, a reduction of 45% in the lateral dimensions of the crystals (from 3.7 to 2.0 µm) is observed as the reaction volume increases. This fact is related to modified heating processes affecting the alkalinization rates and, concomitantly, the precipitation, even under recrystallization at high temperatures. In contrast, for the tenfold mass scale-up, similar morphological features were observed and assigned to changes in nucleation and growth. However, at higher concentrations, simonkolleite-like Co-based layered hydroxide impurities are formed, indicating a phase competition during the precipitation related to the thermodynamic stability of the growing phases. Overall, this work demonstrates that it is possible to upscale the synthesis of high-quality hexagonal CoAl-LDH in a reproducible manner. It highlights the most critical synthesis aspects that must be controlled and provides various fingerprints to trace the quality of these materials. These results will contribute to bringing the use of these 2D layered materials closer to reality in different applications of interest. Fil: Jaramillo Hernández, Camilo. Universidad de Valencia. Instituto de Ciencia Molecular.; Fil: Oestreicher, Víctor. Universidad de Valencia. Instituto de Ciencia Molecular.; Fil: Mizrahi, Martin Daniel. Universidad Nacional de La Plata. Facultad de Ingeniería. Departamento de Ciencias Básicas; Argentina. Consejo Nacional de Investigaciones Científicas y Técnicas. Centro Científico Tecnológico Conicet - La Plata. Instituto de Investigaciones Fisicoquímicas Teóricas y Aplicadas. Universidad Nacional de La Plata. Facultad de Ciencias Exactas. Instituto de Investigaciones Fisicoquímicas Teóricas y Aplicadas; Argentina Fil: Abellán, Gonzalo. Universidad de Valencia. Instituto de Ciencia Molecular.; |
description |
Research on two-dimensional materials is one of the most relevant fields in materials science. Layered double hydroxides (LDHs), a versatile class of anionic clays, exhibit great potential in photocatalysis, energy storage and conversion, and environmental applications. However, its implementation in real-life devices requires the development of efficient and reproducible large-scale synthesis processes. Unfortunately, reliable methods that allow for the production of large quantities of two-dimensional LDHs with well-defined morphologies and high crystallinity are very scarce. In this work, we carry out a scale-up of the urea-based CoAl-LDH synthesis method. We thoroughly study the effects of the mass scale-up (25-fold: up to 375 mM) and the volumetric scale-up (20-fold: up to 2 L). For this, we use a combination of several structural (XRD, TGA, and N2 and CO2 isotherms), microscopic (SEM, TEM, and AFM), magnetic (SQUID), and spectroscopic techniques (ATR-FTIR, UV–vis, XPS, ICP-MS, and XANES-EXAFS). In the case of the volumetric scale-up, a reduction of 45% in the lateral dimensions of the crystals (from 3.7 to 2.0 µm) is observed as the reaction volume increases. This fact is related to modified heating processes affecting the alkalinization rates and, concomitantly, the precipitation, even under recrystallization at high temperatures. In contrast, for the tenfold mass scale-up, similar morphological features were observed and assigned to changes in nucleation and growth. However, at higher concentrations, simonkolleite-like Co-based layered hydroxide impurities are formed, indicating a phase competition during the precipitation related to the thermodynamic stability of the growing phases. Overall, this work demonstrates that it is possible to upscale the synthesis of high-quality hexagonal CoAl-LDH in a reproducible manner. It highlights the most critical synthesis aspects that must be controlled and provides various fingerprints to trace the quality of these materials. These results will contribute to bringing the use of these 2D layered materials closer to reality in different applications of interest. |
publishDate |
2023 |
dc.date.none.fl_str_mv |
2023-09 |
dc.type.none.fl_str_mv |
info:eu-repo/semantics/article info:eu-repo/semantics/publishedVersion http://purl.org/coar/resource_type/c_6501 info:ar-repo/semantics/articulo |
format |
article |
status_str |
publishedVersion |
dc.identifier.none.fl_str_mv |
http://hdl.handle.net/11336/227863 Jaramillo Hernández, Camilo; Oestreicher, Víctor; Mizrahi, Martin Daniel; Abellán, Gonzalo; Upscaling the urea method synthesis of CoAl layered double hydroxides; Beilstein Institute for the Advancement of Chemical Sciences; Beilstein Journal of Nanotechnology; 14; 9-2023; 927-938 2190-4286 CONICET Digital CONICET |
url |
http://hdl.handle.net/11336/227863 |
identifier_str_mv |
Jaramillo Hernández, Camilo; Oestreicher, Víctor; Mizrahi, Martin Daniel; Abellán, Gonzalo; Upscaling the urea method synthesis of CoAl layered double hydroxides; Beilstein Institute for the Advancement of Chemical Sciences; Beilstein Journal of Nanotechnology; 14; 9-2023; 927-938 2190-4286 CONICET Digital CONICET |
dc.language.none.fl_str_mv |
eng |
language |
eng |
dc.relation.none.fl_str_mv |
info:eu-repo/semantics/altIdentifier/url/https://www.beilstein-journals.org/bjnano/articles/14/76 info:eu-repo/semantics/altIdentifier/doi/10.3762/bjnano.14.76 |
dc.rights.none.fl_str_mv |
info:eu-repo/semantics/openAccess https://creativecommons.org/licenses/by/2.5/ar/ |
eu_rights_str_mv |
openAccess |
rights_invalid_str_mv |
https://creativecommons.org/licenses/by/2.5/ar/ |
dc.format.none.fl_str_mv |
application/pdf application/pdf |
dc.publisher.none.fl_str_mv |
Beilstein Institute for the Advancement of Chemical Sciences |
publisher.none.fl_str_mv |
Beilstein Institute for the Advancement of Chemical Sciences |
dc.source.none.fl_str_mv |
reponame:CONICET Digital (CONICET) instname:Consejo Nacional de Investigaciones Científicas y Técnicas |
reponame_str |
CONICET Digital (CONICET) |
collection |
CONICET Digital (CONICET) |
instname_str |
Consejo Nacional de Investigaciones Científicas y Técnicas |
repository.name.fl_str_mv |
CONICET Digital (CONICET) - Consejo Nacional de Investigaciones Científicas y Técnicas |
repository.mail.fl_str_mv |
dasensio@conicet.gov.ar; lcarlino@conicet.gov.ar |
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1846083341070106624 |
score |
13.22299 |