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
CONICET Digital (CONICET)
Institución
Consejo Nacional de Investigaciones Científicas y Técnicas
OAI Identificador
oai:ri.conicet.gov.ar:11336/227863

id CONICETDig_c26fdb07adecb1371bab8d8108fc95c6
oai_identifier_str oai:ri.conicet.gov.ar:11336/227863
network_acronym_str CONICETDig
repository_id_str 3498
network_name_str CONICET Digital (CONICET)
spelling 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
_version_ 1846083341070106624
score 13.22299