Novel high-temperature phase and crystal structure evolution of CsCuBr3 halide identified by neutron powder diffraction

Autores
Abia, Carmen; Lopez, Carlos Alberto; Gainza, Javier; Rodrigues, João Elias F. S.; Fernández Díaz, María Teresa; Céspedes, Eva; Martínez, José Luis; Alonso, José Antonio
Año de publicación
2023
Idioma
inglés
Tipo de recurso
artículo
Estado
versión publicada
Descripción
The search for novel lead-free materials with potential optoelectronic applications is a main research topic nowadays for an environment-friendly energy transition. Based on promising all-inorganic CsPbBr3 perovskite, we tested here the substitution of toxic Pb2+ with Cu2+ and explored the understudied CsCuBr3 halide. We present a mechanically-synthesized CsCuBr3 specimen obtained by ball milling, consisting of a well-crystallized and pure sample. Calorimetric measurements revealed a thermal event suggesting a structural phase transition around 422 K, immediately below the decomposition of the sample due to Br loss. A detailed structural analysis was carried out using neutron powder diffraction data from 20 to 420 K, focusing on the evolution of the orthorhombic phase (space-group: C2221) up to 400 K; this crystal arrangement consists of dimer units of face-sharing [CuBr6] octahedra containing Cu–Cu dimers with conspicuously short distances that account for the magnetic coupling between Cu2+ spins described before. Additionally, at 420 K, we identified a novel high-temperature phase as described in the hexagonal P6522 space group, where infinite chains of [CuBr4] square-planar units were observed. An additional study considering the Debye model was carried out, providing information on the relative Cs–Br and Cu–Br chemical bonds. From diffuse reflectance UV-Vis measurements, an optical gap of ∼1.8 eV was estimated for the orthorhombic phase at room temperature. Magnetic measurements indicate that the effective magnetization behavior versus temperature appears close to linear and seems to extrapolate to zero (smaller than 10−5 μB/Cu atom) at temperatures above 420 K, coinciding with onset of phase transition.
Fil: Abia, Carmen. Instituto de Ciencia de Materiales de Madrid; España
Fil: Lopez, Carlos Alberto. Universidad Nacional de San Luis. Facultad de Química, Bioquímica y Farmacia. Área Química General e Inorgánica; Argentina. Consejo Nacional de Investigaciones Científicas y Técnicas. Centro Científico Tecnológico Conicet - San Luis. Instituto de Investigaciones en Tecnología Química. Universidad Nacional de San Luis. Facultad de Química, Bioquímica y Farmacia. Instituto de Investigaciones en Tecnología Química; Argentina. Instituto de Ciencia de Materiales de Madrid; España
Fil: Gainza, Javier. Instituto de Ciencia de Materiales de Madrid; España
Fil: Rodrigues, João Elias F. S.. European Synchrotron Radiation Facility; Francia
Fil: Fernández Díaz, María Teresa. Institut Laue Langevin; Francia
Fil: Céspedes, Eva. Instituto de Ciencia de Materiales de Madrid; España
Fil: Martínez, José Luis. Instituto de Ciencia de Materiales de Madrid; España
Fil: Alonso, José Antonio. Instituto de Ciencia de Materiales de Madrid; España
Materia
High-temperature
Nivel de accesibilidad
acceso abierto
Condiciones de uso
https://creativecommons.org/licenses/by-nc/2.5/ar/
Repositorio
CONICET Digital (CONICET)
Institución
Consejo Nacional de Investigaciones Científicas y Técnicas
OAI Identificador
oai:ri.conicet.gov.ar:11336/232192

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repository_id_str 3498
network_name_str CONICET Digital (CONICET)
spelling Novel high-temperature phase and crystal structure evolution of CsCuBr3 halide identified by neutron powder diffractionAbia, CarmenLopez, Carlos AlbertoGainza, JavierRodrigues, João Elias F. S.Fernández Díaz, María TeresaCéspedes, EvaMartínez, José LuisAlonso, José AntonioHigh-temperaturehttps://purl.org/becyt/ford/1.4https://purl.org/becyt/ford/1The search for novel lead-free materials with potential optoelectronic applications is a main research topic nowadays for an environment-friendly energy transition. Based on promising all-inorganic CsPbBr3 perovskite, we tested here the substitution of toxic Pb2+ with Cu2+ and explored the understudied CsCuBr3 halide. We present a mechanically-synthesized CsCuBr3 specimen obtained by ball milling, consisting of a well-crystallized and pure sample. Calorimetric measurements revealed a thermal event suggesting a structural phase transition around 422 K, immediately below the decomposition of the sample due to Br loss. A detailed structural analysis was carried out using neutron powder diffraction data from 20 to 420 K, focusing on the evolution of the orthorhombic phase (space-group: C2221) up to 400 K; this crystal arrangement consists of dimer units of face-sharing [CuBr6] octahedra containing Cu–Cu dimers with conspicuously short distances that account for the magnetic coupling between Cu2+ spins described before. Additionally, at 420 K, we identified a novel high-temperature phase as described in the hexagonal P6522 space group, where infinite chains of [CuBr4] square-planar units were observed. An additional study considering the Debye model was carried out, providing information on the relative Cs–Br and Cu–Br chemical bonds. From diffuse reflectance UV-Vis measurements, an optical gap of ∼1.8 eV was estimated for the orthorhombic phase at room temperature. Magnetic measurements indicate that the effective magnetization behavior versus temperature appears close to linear and seems to extrapolate to zero (smaller than 10−5 μB/Cu atom) at temperatures above 420 K, coinciding with onset of phase transition.Fil: Abia, Carmen. Instituto de Ciencia de Materiales de Madrid; EspañaFil: Lopez, Carlos Alberto. Universidad Nacional de San Luis. Facultad de Química, Bioquímica y Farmacia. Área Química General e Inorgánica; Argentina. Consejo Nacional de Investigaciones Científicas y Técnicas. Centro Científico Tecnológico Conicet - San Luis. Instituto de Investigaciones en Tecnología Química. Universidad Nacional de San Luis. Facultad de Química, Bioquímica y Farmacia. Instituto de Investigaciones en Tecnología Química; Argentina. Instituto de Ciencia de Materiales de Madrid; EspañaFil: Gainza, Javier. Instituto de Ciencia de Materiales de Madrid; EspañaFil: Rodrigues, João Elias F. S.. European Synchrotron Radiation Facility; FranciaFil: Fernández Díaz, María Teresa. Institut Laue Langevin; FranciaFil: Céspedes, Eva. Instituto de Ciencia de Materiales de Madrid; EspañaFil: Martínez, José Luis. Instituto de Ciencia de Materiales de Madrid; EspañaFil: Alonso, José Antonio. Instituto de Ciencia de Materiales de Madrid; EspañaRoyal Society of Chemistry2023-05info:eu-repo/semantics/articleinfo:eu-repo/semantics/publishedVersionhttp://purl.org/coar/resource_type/c_6501info:ar-repo/semantics/articuloapplication/pdfapplication/pdfhttp://hdl.handle.net/11336/232192Abia, Carmen; Lopez, Carlos Alberto; Gainza, Javier; Rodrigues, João Elias F. S.; Fernández Díaz, María Teresa; et al.; Novel high-temperature phase and crystal structure evolution of CsCuBr3 halide identified by neutron powder diffraction; Royal Society of Chemistry; CrystEngComm; 25; 31; 5-2023; 4417-44261466-8033CONICET DigitalCONICETenginfo:eu-repo/semantics/altIdentifier/doi/10.1039/d3ce00432einfo:eu-repo/semantics/altIdentifier/url/https://pubs.rsc.org/en/content/articlelanding/2023/ce/d3ce00432einfo:eu-repo/semantics/openAccesshttps://creativecommons.org/licenses/by-nc/2.5/ar/reponame:CONICET Digital (CONICET)instname:Consejo Nacional de Investigaciones Científicas y Técnicas2025-10-22T11:40:41Zoai:ri.conicet.gov.ar:11336/232192instacron: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:34982025-10-22 11:40:42.059CONICET Digital (CONICET) - Consejo Nacional de Investigaciones Científicas y Técnicasfalse
dc.title.none.fl_str_mv Novel high-temperature phase and crystal structure evolution of CsCuBr3 halide identified by neutron powder diffraction
title Novel high-temperature phase and crystal structure evolution of CsCuBr3 halide identified by neutron powder diffraction
spellingShingle Novel high-temperature phase and crystal structure evolution of CsCuBr3 halide identified by neutron powder diffraction
Abia, Carmen
High-temperature
title_short Novel high-temperature phase and crystal structure evolution of CsCuBr3 halide identified by neutron powder diffraction
title_full Novel high-temperature phase and crystal structure evolution of CsCuBr3 halide identified by neutron powder diffraction
title_fullStr Novel high-temperature phase and crystal structure evolution of CsCuBr3 halide identified by neutron powder diffraction
title_full_unstemmed Novel high-temperature phase and crystal structure evolution of CsCuBr3 halide identified by neutron powder diffraction
title_sort Novel high-temperature phase and crystal structure evolution of CsCuBr3 halide identified by neutron powder diffraction
dc.creator.none.fl_str_mv Abia, Carmen
Lopez, Carlos Alberto
Gainza, Javier
Rodrigues, João Elias F. S.
Fernández Díaz, María Teresa
Céspedes, Eva
Martínez, José Luis
Alonso, José Antonio
author Abia, Carmen
author_facet Abia, Carmen
Lopez, Carlos Alberto
Gainza, Javier
Rodrigues, João Elias F. S.
Fernández Díaz, María Teresa
Céspedes, Eva
Martínez, José Luis
Alonso, José Antonio
author_role author
author2 Lopez, Carlos Alberto
Gainza, Javier
Rodrigues, João Elias F. S.
Fernández Díaz, María Teresa
Céspedes, Eva
Martínez, José Luis
Alonso, José Antonio
author2_role author
author
author
author
author
author
author
dc.subject.none.fl_str_mv High-temperature
topic High-temperature
purl_subject.fl_str_mv https://purl.org/becyt/ford/1.4
https://purl.org/becyt/ford/1
dc.description.none.fl_txt_mv The search for novel lead-free materials with potential optoelectronic applications is a main research topic nowadays for an environment-friendly energy transition. Based on promising all-inorganic CsPbBr3 perovskite, we tested here the substitution of toxic Pb2+ with Cu2+ and explored the understudied CsCuBr3 halide. We present a mechanically-synthesized CsCuBr3 specimen obtained by ball milling, consisting of a well-crystallized and pure sample. Calorimetric measurements revealed a thermal event suggesting a structural phase transition around 422 K, immediately below the decomposition of the sample due to Br loss. A detailed structural analysis was carried out using neutron powder diffraction data from 20 to 420 K, focusing on the evolution of the orthorhombic phase (space-group: C2221) up to 400 K; this crystal arrangement consists of dimer units of face-sharing [CuBr6] octahedra containing Cu–Cu dimers with conspicuously short distances that account for the magnetic coupling between Cu2+ spins described before. Additionally, at 420 K, we identified a novel high-temperature phase as described in the hexagonal P6522 space group, where infinite chains of [CuBr4] square-planar units were observed. An additional study considering the Debye model was carried out, providing information on the relative Cs–Br and Cu–Br chemical bonds. From diffuse reflectance UV-Vis measurements, an optical gap of ∼1.8 eV was estimated for the orthorhombic phase at room temperature. Magnetic measurements indicate that the effective magnetization behavior versus temperature appears close to linear and seems to extrapolate to zero (smaller than 10−5 μB/Cu atom) at temperatures above 420 K, coinciding with onset of phase transition.
Fil: Abia, Carmen. Instituto de Ciencia de Materiales de Madrid; España
Fil: Lopez, Carlos Alberto. Universidad Nacional de San Luis. Facultad de Química, Bioquímica y Farmacia. Área Química General e Inorgánica; Argentina. Consejo Nacional de Investigaciones Científicas y Técnicas. Centro Científico Tecnológico Conicet - San Luis. Instituto de Investigaciones en Tecnología Química. Universidad Nacional de San Luis. Facultad de Química, Bioquímica y Farmacia. Instituto de Investigaciones en Tecnología Química; Argentina. Instituto de Ciencia de Materiales de Madrid; España
Fil: Gainza, Javier. Instituto de Ciencia de Materiales de Madrid; España
Fil: Rodrigues, João Elias F. S.. European Synchrotron Radiation Facility; Francia
Fil: Fernández Díaz, María Teresa. Institut Laue Langevin; Francia
Fil: Céspedes, Eva. Instituto de Ciencia de Materiales de Madrid; España
Fil: Martínez, José Luis. Instituto de Ciencia de Materiales de Madrid; España
Fil: Alonso, José Antonio. Instituto de Ciencia de Materiales de Madrid; España
description The search for novel lead-free materials with potential optoelectronic applications is a main research topic nowadays for an environment-friendly energy transition. Based on promising all-inorganic CsPbBr3 perovskite, we tested here the substitution of toxic Pb2+ with Cu2+ and explored the understudied CsCuBr3 halide. We present a mechanically-synthesized CsCuBr3 specimen obtained by ball milling, consisting of a well-crystallized and pure sample. Calorimetric measurements revealed a thermal event suggesting a structural phase transition around 422 K, immediately below the decomposition of the sample due to Br loss. A detailed structural analysis was carried out using neutron powder diffraction data from 20 to 420 K, focusing on the evolution of the orthorhombic phase (space-group: C2221) up to 400 K; this crystal arrangement consists of dimer units of face-sharing [CuBr6] octahedra containing Cu–Cu dimers with conspicuously short distances that account for the magnetic coupling between Cu2+ spins described before. Additionally, at 420 K, we identified a novel high-temperature phase as described in the hexagonal P6522 space group, where infinite chains of [CuBr4] square-planar units were observed. An additional study considering the Debye model was carried out, providing information on the relative Cs–Br and Cu–Br chemical bonds. From diffuse reflectance UV-Vis measurements, an optical gap of ∼1.8 eV was estimated for the orthorhombic phase at room temperature. Magnetic measurements indicate that the effective magnetization behavior versus temperature appears close to linear and seems to extrapolate to zero (smaller than 10−5 μB/Cu atom) at temperatures above 420 K, coinciding with onset of phase transition.
publishDate 2023
dc.date.none.fl_str_mv 2023-05
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/11336/232192
Abia, Carmen; Lopez, Carlos Alberto; Gainza, Javier; Rodrigues, João Elias F. S.; Fernández Díaz, María Teresa; et al.; Novel high-temperature phase and crystal structure evolution of CsCuBr3 halide identified by neutron powder diffraction; Royal Society of Chemistry; CrystEngComm; 25; 31; 5-2023; 4417-4426
1466-8033
CONICET Digital
CONICET
url http://hdl.handle.net/11336/232192
identifier_str_mv Abia, Carmen; Lopez, Carlos Alberto; Gainza, Javier; Rodrigues, João Elias F. S.; Fernández Díaz, María Teresa; et al.; Novel high-temperature phase and crystal structure evolution of CsCuBr3 halide identified by neutron powder diffraction; Royal Society of Chemistry; CrystEngComm; 25; 31; 5-2023; 4417-4426
1466-8033
CONICET Digital
CONICET
dc.language.none.fl_str_mv eng
language eng
dc.relation.none.fl_str_mv info:eu-repo/semantics/altIdentifier/doi/10.1039/d3ce00432e
info:eu-repo/semantics/altIdentifier/url/https://pubs.rsc.org/en/content/articlelanding/2023/ce/d3ce00432e
dc.rights.none.fl_str_mv info:eu-repo/semantics/openAccess
https://creativecommons.org/licenses/by-nc/2.5/ar/
eu_rights_str_mv openAccess
rights_invalid_str_mv https://creativecommons.org/licenses/by-nc/2.5/ar/
dc.format.none.fl_str_mv application/pdf
application/pdf
dc.publisher.none.fl_str_mv Royal Society of Chemistry
publisher.none.fl_str_mv Royal Society of Chemistry
dc.source.none.fl_str_mv reponame:CONICET Digital (CONICET)
instname:Consejo Nacional de Investigaciones Científicas y Técnicas
reponame_str CONICET Digital (CONICET)
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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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