Thickness determination of electrochemical titanium oxide (Ti/TiO2) formed in HClO4 solutions

Autores
Filippin, Francisco Angel; Linarez Pérez, Omar Ezequiel; Lopez Teijelo, Manuel; Bonetto, Rita Dominga; Trincavelli, Jorge Carlos; Avalle, Lucia Bernardita
Año de publicación
2014
Idioma
inglés
Tipo de recurso
artículo
Estado
versión publicada
Descripción
Anodic Titanium oxide films were potentiodinamically grown on Ti foil and glass/Ti in 0.010 M HClO4 at 50 mVs−1. The current density-potential curves (j − E) showed that the oxide grows according to the physical model for high-field conduction. However, for final potential (Ef) higher than 1.5 V vs. Ag/AgCl (sat. KCl) the oxygen evolution reaction becomes more significant, and the formation of bubbles prevented or made more difficult the application of in situ techniques for the simultaneous study of the thickness and optical properties of the anodic layer. We developed a method based on electron probe microanalysis (EPMA) to calculate oxide thickness using ex situ ellipsometry as a reference technique. The normalized intensity of the O Kα peaks was measured for anodic oxides corresponding to Ef values from spontaneous oxide up to 50 V, where a linear relationship was observed for a narrower range of final potentials. This behaviour was studied with Monte Carlo simulations. After calibration with ellipsometric results, to take into account sample damage during the electron irradiation, EPMA was applied as a method for thickness determination at Ef ≥ 1.0 V. Once the method was established, ex situ thickness determinations became independent of the preparation method of the oxide layer, which represents a comparative advantage against ex situ ellipsometry.
Fil: Filippin, Francisco Angel. Universidad Nacional de Catamarca; Argentina
Fil: Linarez Pérez, Omar Ezequiel. Consejo Nacional de Investigaciones Científicas y Técnicas. Centro Científico Tecnológico Conicet - Córdoba. Instituto de Investigaciones en Físico-química de Córdoba. Universidad Nacional de Córdoba. Facultad de Ciencias Químicas. Instituto de Investigaciones en Físico-química de Córdoba; Argentina
Fil: Lopez Teijelo, Manuel. Consejo Nacional de Investigaciones Científicas y Técnicas. Centro Científico Tecnológico Conicet - Córdoba. Instituto de Investigaciones en Físico-química de Córdoba. Universidad Nacional de Córdoba. Facultad de Ciencias Químicas. Instituto de Investigaciones en Físico-química de Córdoba; Argentina
Fil: Bonetto, Rita Dominga. Consejo Nacional de Investigaciones Científicas y Técnicas. Centro Científico Tecnológico Conicet - La Plata. Centro de Investigación y Desarrollo en Ciencias Aplicadas "Dr. Jorge J. Ronco". Universidad Nacional de La Plata. Facultad de Ciencias Exactas. Centro de Investigación y Desarrollo en Ciencias Aplicadas; Argentina
Fil: Trincavelli, Jorge Carlos. Consejo Nacional de Investigaciones Científicas y Técnicas. Centro Científico Tecnológico Conicet - Córdoba. Instituto de Física Enrique Gaviola. Universidad Nacional de Córdoba. Instituto de Física Enrique Gaviola; Argentina
Fil: Avalle, Lucia Bernardita. Consejo Nacional de Investigaciones Científicas y Técnicas. Centro Científico Tecnológico Conicet - Córdoba. Instituto de Física Enrique Gaviola. Universidad Nacional de Córdoba. Instituto de Física Enrique Gaviola; Argentina
Materia
Electrochemistry
Ellipsometry
Epma
Oxide Growth
Tio2
Nivel de accesibilidad
acceso abierto
Condiciones de uso
https://creativecommons.org/licenses/by-nc-sa/2.5/ar/
Repositorio
CONICET Digital (CONICET)
Institución
Consejo Nacional de Investigaciones Científicas y Técnicas
OAI Identificador
oai:ri.conicet.gov.ar:11336/31573
Acceder
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oai_identifier_str oai:ri.conicet.gov.ar:11336/31573
network_acronym_str CONICETDig
repository_id_str 3498
network_name_str CONICET Digital (CONICET)
spelling Thickness determination of electrochemical titanium oxide (Ti/TiO2) formed in HClO4 solutionsFilippin, Francisco AngelLinarez Pérez, Omar EzequielLopez Teijelo, ManuelBonetto, Rita DomingaTrincavelli, Jorge CarlosAvalle, Lucia BernarditaElectrochemistryEllipsometryEpmaOxide GrowthTio2https://purl.org/becyt/ford/1.3https://purl.org/becyt/ford/1Anodic Titanium oxide films were potentiodinamically grown on Ti foil and glass/Ti in 0.010 M HClO4 at 50 mVs−1. The current density-potential curves (j − E) showed that the oxide grows according to the physical model for high-field conduction. However, for final potential (Ef) higher than 1.5 V vs. Ag/AgCl (sat. KCl) the oxygen evolution reaction becomes more significant, and the formation of bubbles prevented or made more difficult the application of in situ techniques for the simultaneous study of the thickness and optical properties of the anodic layer. We developed a method based on electron probe microanalysis (EPMA) to calculate oxide thickness using ex situ ellipsometry as a reference technique. The normalized intensity of the O Kα peaks was measured for anodic oxides corresponding to Ef values from spontaneous oxide up to 50 V, where a linear relationship was observed for a narrower range of final potentials. This behaviour was studied with Monte Carlo simulations. After calibration with ellipsometric results, to take into account sample damage during the electron irradiation, EPMA was applied as a method for thickness determination at Ef ≥ 1.0 V. Once the method was established, ex situ thickness determinations became independent of the preparation method of the oxide layer, which represents a comparative advantage against ex situ ellipsometry.Fil: Filippin, Francisco Angel. Universidad Nacional de Catamarca; ArgentinaFil: Linarez Pérez, Omar Ezequiel. Consejo Nacional de Investigaciones Científicas y Técnicas. Centro Científico Tecnológico Conicet - Córdoba. Instituto de Investigaciones en Físico-química de Córdoba. Universidad Nacional de Córdoba. Facultad de Ciencias Químicas. Instituto de Investigaciones en Físico-química de Córdoba; ArgentinaFil: Lopez Teijelo, Manuel. Consejo Nacional de Investigaciones Científicas y Técnicas. Centro Científico Tecnológico Conicet - Córdoba. Instituto de Investigaciones en Físico-química de Córdoba. Universidad Nacional de Córdoba. Facultad de Ciencias Químicas. Instituto de Investigaciones en Físico-química de Córdoba; ArgentinaFil: Bonetto, Rita Dominga. Consejo Nacional de Investigaciones Científicas y Técnicas. Centro Científico Tecnológico Conicet - La Plata. Centro de Investigación y Desarrollo en Ciencias Aplicadas "Dr. Jorge J. Ronco". Universidad Nacional de La Plata. Facultad de Ciencias Exactas. Centro de Investigación y Desarrollo en Ciencias Aplicadas; ArgentinaFil: Trincavelli, Jorge Carlos. Consejo Nacional de Investigaciones Científicas y Técnicas. Centro Científico Tecnológico Conicet - Córdoba. Instituto de Física Enrique Gaviola. Universidad Nacional de Córdoba. Instituto de Física Enrique Gaviola; ArgentinaFil: Avalle, Lucia Bernardita. Consejo Nacional de Investigaciones Científicas y Técnicas. Centro Científico Tecnológico Conicet - Córdoba. Instituto de Física Enrique Gaviola. Universidad Nacional de Córdoba. Instituto de Física Enrique Gaviola; ArgentinaPergamon-Elsevier Science Ltd.2014-03info:eu-repo/semantics/articleinfo:eu-repo/semantics/publishedVersionhttp://purl.org/coar/resource_type/c_6501info:ar-repo/semantics/articuloapplication/pdfapplication/pdfapplication/pdfapplication/pdfapplication/pdfapplication/pdfapplication/pdfapplication/pdfapplication/pdfapplication/pdfhttp://hdl.handle.net/11336/31573Avalle, Lucia Bernardita; Bonetto, Rita Dominga; Lopez Teijelo, Manuel; Linarez Pérez, Omar Ezequiel; Filippin, Francisco Angel; Trincavelli, Jorge Carlos; et al.; Thickness determination of electrochemical titanium oxide (Ti/TiO2) formed in HClO4 solutions; Pergamon-Elsevier Science Ltd.; Electrochimica Acta; 129; 3-2014; 266-2750013-4686CONICET DigitalCONICETenginfo:eu-repo/semantics/altIdentifier/doi/10.1016/j.electacta.2014.02.086info:eu-repo/semantics/altIdentifier/url/http://www.sciencedirect.com/science/article/pii/S0013468614004009info:eu-repo/semantics/openAccesshttps://creativecommons.org/licenses/by-nc-sa/2.5/ar/reponame:CONICET Digital (CONICET)instname:Consejo Nacional de Investigaciones Científicas y Técnicas2025-09-29T10:37:32Zoai:ri.conicet.gov.ar:11336/31573instacron: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:34982025-09-29 10:37:32.67CONICET Digital (CONICET) - Consejo Nacional de Investigaciones Científicas y Técnicasfalse
dc.title.none.fl_str_mv Thickness determination of electrochemical titanium oxide (Ti/TiO2) formed in HClO4 solutions
title Thickness determination of electrochemical titanium oxide (Ti/TiO2) formed in HClO4 solutions
spellingShingle Thickness determination of electrochemical titanium oxide (Ti/TiO2) formed in HClO4 solutions
Filippin, Francisco Angel
Electrochemistry
Ellipsometry
Epma
Oxide Growth
Tio2
title_short Thickness determination of electrochemical titanium oxide (Ti/TiO2) formed in HClO4 solutions
title_full Thickness determination of electrochemical titanium oxide (Ti/TiO2) formed in HClO4 solutions
title_fullStr Thickness determination of electrochemical titanium oxide (Ti/TiO2) formed in HClO4 solutions
title_full_unstemmed Thickness determination of electrochemical titanium oxide (Ti/TiO2) formed in HClO4 solutions
title_sort Thickness determination of electrochemical titanium oxide (Ti/TiO2) formed in HClO4 solutions
dc.creator.none.fl_str_mv Filippin, Francisco Angel
Linarez Pérez, Omar Ezequiel
Lopez Teijelo, Manuel
Bonetto, Rita Dominga
Trincavelli, Jorge Carlos
Avalle, Lucia Bernardita
author Filippin, Francisco Angel
author_facet Filippin, Francisco Angel
Linarez Pérez, Omar Ezequiel
Lopez Teijelo, Manuel
Bonetto, Rita Dominga
Trincavelli, Jorge Carlos
Avalle, Lucia Bernardita
author_role author
author2 Linarez Pérez, Omar Ezequiel
Lopez Teijelo, Manuel
Bonetto, Rita Dominga
Trincavelli, Jorge Carlos
Avalle, Lucia Bernardita
author2_role author
author
author
author
author
dc.subject.none.fl_str_mv Electrochemistry
Ellipsometry
Epma
Oxide Growth
Tio2
topic Electrochemistry
Ellipsometry
Epma
Oxide Growth
Tio2
purl_subject.fl_str_mv https://purl.org/becyt/ford/1.3
https://purl.org/becyt/ford/1
dc.description.none.fl_txt_mv Anodic Titanium oxide films were potentiodinamically grown on Ti foil and glass/Ti in 0.010 M HClO4 at 50 mVs−1. The current density-potential curves (j − E) showed that the oxide grows according to the physical model for high-field conduction. However, for final potential (Ef) higher than 1.5 V vs. Ag/AgCl (sat. KCl) the oxygen evolution reaction becomes more significant, and the formation of bubbles prevented or made more difficult the application of in situ techniques for the simultaneous study of the thickness and optical properties of the anodic layer. We developed a method based on electron probe microanalysis (EPMA) to calculate oxide thickness using ex situ ellipsometry as a reference technique. The normalized intensity of the O Kα peaks was measured for anodic oxides corresponding to Ef values from spontaneous oxide up to 50 V, where a linear relationship was observed for a narrower range of final potentials. This behaviour was studied with Monte Carlo simulations. After calibration with ellipsometric results, to take into account sample damage during the electron irradiation, EPMA was applied as a method for thickness determination at Ef ≥ 1.0 V. Once the method was established, ex situ thickness determinations became independent of the preparation method of the oxide layer, which represents a comparative advantage against ex situ ellipsometry.
Fil: Filippin, Francisco Angel. Universidad Nacional de Catamarca; Argentina
Fil: Linarez Pérez, Omar Ezequiel. Consejo Nacional de Investigaciones Científicas y Técnicas. Centro Científico Tecnológico Conicet - Córdoba. Instituto de Investigaciones en Físico-química de Córdoba. Universidad Nacional de Córdoba. Facultad de Ciencias Químicas. Instituto de Investigaciones en Físico-química de Córdoba; Argentina
Fil: Lopez Teijelo, Manuel. Consejo Nacional de Investigaciones Científicas y Técnicas. Centro Científico Tecnológico Conicet - Córdoba. Instituto de Investigaciones en Físico-química de Córdoba. Universidad Nacional de Córdoba. Facultad de Ciencias Químicas. Instituto de Investigaciones en Físico-química de Córdoba; Argentina
Fil: Bonetto, Rita Dominga. Consejo Nacional de Investigaciones Científicas y Técnicas. Centro Científico Tecnológico Conicet - La Plata. Centro de Investigación y Desarrollo en Ciencias Aplicadas "Dr. Jorge J. Ronco". Universidad Nacional de La Plata. Facultad de Ciencias Exactas. Centro de Investigación y Desarrollo en Ciencias Aplicadas; Argentina
Fil: Trincavelli, Jorge Carlos. Consejo Nacional de Investigaciones Científicas y Técnicas. Centro Científico Tecnológico Conicet - Córdoba. Instituto de Física Enrique Gaviola. Universidad Nacional de Córdoba. Instituto de Física Enrique Gaviola; Argentina
Fil: Avalle, Lucia Bernardita. Consejo Nacional de Investigaciones Científicas y Técnicas. Centro Científico Tecnológico Conicet - Córdoba. Instituto de Física Enrique Gaviola. Universidad Nacional de Córdoba. Instituto de Física Enrique Gaviola; Argentina
description Anodic Titanium oxide films were potentiodinamically grown on Ti foil and glass/Ti in 0.010 M HClO4 at 50 mVs−1. The current density-potential curves (j − E) showed that the oxide grows according to the physical model for high-field conduction. However, for final potential (Ef) higher than 1.5 V vs. Ag/AgCl (sat. KCl) the oxygen evolution reaction becomes more significant, and the formation of bubbles prevented or made more difficult the application of in situ techniques for the simultaneous study of the thickness and optical properties of the anodic layer. We developed a method based on electron probe microanalysis (EPMA) to calculate oxide thickness using ex situ ellipsometry as a reference technique. The normalized intensity of the O Kα peaks was measured for anodic oxides corresponding to Ef values from spontaneous oxide up to 50 V, where a linear relationship was observed for a narrower range of final potentials. This behaviour was studied with Monte Carlo simulations. After calibration with ellipsometric results, to take into account sample damage during the electron irradiation, EPMA was applied as a method for thickness determination at Ef ≥ 1.0 V. Once the method was established, ex situ thickness determinations became independent of the preparation method of the oxide layer, which represents a comparative advantage against ex situ ellipsometry.
publishDate 2014
dc.date.none.fl_str_mv 2014-03
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/11336/31573
Avalle, Lucia Bernardita; Bonetto, Rita Dominga; Lopez Teijelo, Manuel; Linarez Pérez, Omar Ezequiel; Filippin, Francisco Angel; Trincavelli, Jorge Carlos; et al.; Thickness determination of electrochemical titanium oxide (Ti/TiO2) formed in HClO4 solutions; Pergamon-Elsevier Science Ltd.; Electrochimica Acta; 129; 3-2014; 266-275
0013-4686
CONICET Digital
CONICET
url http://hdl.handle.net/11336/31573
identifier_str_mv Avalle, Lucia Bernardita; Bonetto, Rita Dominga; Lopez Teijelo, Manuel; Linarez Pérez, Omar Ezequiel; Filippin, Francisco Angel; Trincavelli, Jorge Carlos; et al.; Thickness determination of electrochemical titanium oxide (Ti/TiO2) formed in HClO4 solutions; Pergamon-Elsevier Science Ltd.; Electrochimica Acta; 129; 3-2014; 266-275
0013-4686
CONICET Digital
CONICET
dc.language.none.fl_str_mv eng
language eng
dc.relation.none.fl_str_mv info:eu-repo/semantics/altIdentifier/doi/10.1016/j.electacta.2014.02.086
info:eu-repo/semantics/altIdentifier/url/http://www.sciencedirect.com/science/article/pii/S0013468614004009
dc.rights.none.fl_str_mv info:eu-repo/semantics/openAccess
https://creativecommons.org/licenses/by-nc-sa/2.5/ar/
eu_rights_str_mv openAccess
rights_invalid_str_mv https://creativecommons.org/licenses/by-nc-sa/2.5/ar/
dc.format.none.fl_str_mv application/pdf
application/pdf
application/pdf
application/pdf
application/pdf
application/pdf
application/pdf
application/pdf
application/pdf
application/pdf
dc.publisher.none.fl_str_mv Pergamon-Elsevier Science Ltd.
publisher.none.fl_str_mv Pergamon-Elsevier Science Ltd.
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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score 13.070432

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