Electrodeposition of copper into functionalized polypyrrole films
Identifieur interne : 001315 ( Istex/Corpus ); précédent : 001314; suivant : 001316Electrodeposition of copper into functionalized polypyrrole films
Auteurs : Ahmed Zouaoui ; Olivier Stéphan ; Michel Carrier ; Jean-Claude MoutetSource :
- Journal of Electroanalytical Chemistry [ 1572-6657 ] ; 1999.
English descriptors
Abstract
Copper microparticles have been dispersed in anion-exchange polymer films coated on carbon electrodes by oxidative electropolymerization of pyrrole–alkylammonium monomers. Incorporation of copper in polymeric films was effected by impregnation of copper-oxalate anionic complexes followed by an electroreductive precipitation to copper metal, or by electroreduction of polymer coated electrodes immersed in copper–oxalate aqueous solutions. The deposition process was examined by voltammetry. Scanning electron microscopy showed a dispersion of metal particles from 50–100 up to 300 nm, according to the lipophilic character of the polymer, located in a layer near the carbon∣polymer interface. A study of the electrocatalytic activity in the reduction of nitrobenzene to aniline at these materials was performed. The cathodes appeared much more active than bulk copper electrodes.
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DOI: 10.1016/S0022-0728(99)00310-1
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first="Michel" last="Carrier">Michel Carrier</name><affiliation><mods:affiliation>Institut National des Sciences et Techniques Nucléaires, CEA-Saclay, 91191 Gif-sur-Yvette, France</mods:affiliation></affiliation></author><author><name sortKey="Moutet, Jean Claude" sort="Moutet, Jean Claude" uniqKey="Moutet J" first="Jean-Claude" last="Moutet">Jean-Claude Moutet</name><affiliation><mods:affiliation>E-mail: jean-claude.moutet@ujf-grenoble.fr</mods:affiliation></affiliation><affiliation><mods:affiliation>Laboratoire d’Electrochimie Organique et de Photochimie Rédox, UMR CNRS 5630, Université Joseph Fourier Grenoble I, BP 53, 38041 Grenoble Cedex 9, France</mods:affiliation></affiliation></author></titleStmt><publicationStmt><idno type="wicri:source">ISTEX</idno><idno type="RBID">ISTEX:2DE5F8979AAAE687376A593CCB269AF4CAB3E7F6</idno><date when="1999" year="1999">1999</date><idno type="doi">10.1016/S0022-0728(99)00310-1</idno><idno 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Matériaux Electroactifs, UMR CNRS 5588, Université Joseph Fourier Grenoble 1, BP 87, 38402 Saint Martin d’Hères Cedex, France</mods:affiliation></affiliation></author><author><name sortKey="Carrier, Michel" sort="Carrier, Michel" uniqKey="Carrier M" first="Michel" last="Carrier">Michel Carrier</name><affiliation><mods:affiliation>Institut National des Sciences et Techniques Nucléaires, CEA-Saclay, 91191 Gif-sur-Yvette, France</mods:affiliation></affiliation></author><author><name sortKey="Moutet, Jean Claude" sort="Moutet, Jean Claude" uniqKey="Moutet J" first="Jean-Claude" last="Moutet">Jean-Claude Moutet</name><affiliation><mods:affiliation>E-mail: jean-claude.moutet@ujf-grenoble.fr</mods:affiliation></affiliation><affiliation><mods:affiliation>Laboratoire d’Electrochimie Organique et de Photochimie Rédox, UMR CNRS 5630, Université Joseph Fourier Grenoble I, BP 53, 38041 Grenoble Cedex 9, France</mods:affiliation></affiliation></author></analytic><monogr></monogr><series><title level="j">Journal of Electroanalytical Chemistry</title><title level="j" type="abbrev">JEC</title><idno type="ISSN">1572-6657</idno><imprint><publisher>ELSEVIER</publisher><date type="published" when="1999">1999</date><biblScope unit="volume">474</biblScope><biblScope unit="issue">2</biblScope><biblScope unit="page" from="113">113</biblScope><biblScope unit="page" to="122">122</biblScope></imprint><idno type="ISSN">1572-6657</idno></series><idno type="istex">2DE5F8979AAAE687376A593CCB269AF4CAB3E7F6</idno><idno type="DOI">10.1016/S0022-0728(99)00310-1</idno><idno type="PII">S0022-0728(99)00310-1</idno></biblStruct></sourceDesc><seriesStmt><idno type="ISSN">1572-6657</idno></seriesStmt></fileDesc><profileDesc><textClass><keywords scheme="KwdEn" xml:lang="en"><term>Copper complexes</term><term>Electrocatalysis</term><term>Functionalized polypyrrole</term><term>Modified electrode</term></keywords></textClass><langUsage><language ident="en">en</language></langUsage></profileDesc></teiHeader><front><div type="abstract" xml:lang="en">Copper microparticles have been dispersed in anion-exchange polymer films coated on carbon electrodes by oxidative electropolymerization of pyrrole–alkylammonium monomers. Incorporation of copper in polymeric films was effected by impregnation of copper-oxalate anionic complexes followed by an electroreductive precipitation to copper metal, or by electroreduction of polymer coated electrodes immersed in copper–oxalate aqueous solutions. The deposition process was examined by voltammetry. Scanning electron microscopy showed a dispersion of metal particles from 50–100 up to 300 nm, according to the lipophilic character of the polymer, located in a layer near the carbon∣polymer interface. A study of the electrocatalytic activity in the reduction of nitrobenzene to aniline at these materials was performed. The cathodes appeared much more active than bulk copper electrodes.</div></front></TEI><istex><corpusName>elsevier</corpusName><author><json:item><name>Ahmed Zouaoui</name><affiliations><json:string>Laboratoire d’Electrochimie Organique et de Photochimie Rédox, UMR CNRS 5630, Université Joseph Fourier Grenoble I, BP 53, 38041 Grenoble Cedex 9, France</json:string></affiliations></json:item><json:item><name>Olivier Stéphan</name><affiliations><json:string>Laboratoire de Spectrométrie Physique, Equipe Matériaux Electroactifs, UMR CNRS 5588, Université Joseph Fourier Grenoble 1, BP 87, 38402 Saint Martin d’Hères Cedex, France</json:string></affiliations></json:item><json:item><name>Michel Carrier</name><affiliations><json:string>Institut National des Sciences et Techniques Nucléaires, CEA-Saclay, 91191 Gif-sur-Yvette, France</json:string></affiliations></json:item><json:item><name>Jean-Claude Moutet</name><affiliations><json:string>E-mail: jean-claude.moutet@ujf-grenoble.fr</json:string><json:string>Laboratoire d’Electrochimie Organique et de Photochimie Rédox, UMR CNRS 5630, Université Joseph Fourier Grenoble I, BP 53, 38041 Grenoble Cedex 9, France</json:string></affiliations></json:item></author><subject><json:item><lang><json:string>eng</json:string></lang><value>Modified electrode</value></json:item><json:item><lang><json:string>eng</json:string></lang><value>Functionalized polypyrrole</value></json:item><json:item><lang><json:string>eng</json:string></lang><value>Electrocatalysis</value></json:item><json:item><lang><json:string>eng</json:string></lang><value>Copper complexes</value></json:item></subject><language><json:string>eng</json:string></language><originalGenre><json:string>Full-length article</json:string></originalGenre><abstract>Copper microparticles have been dispersed in anion-exchange polymer films coated on carbon electrodes by oxidative electropolymerization of pyrrole–alkylammonium monomers. Incorporation of copper in polymeric films was effected by impregnation of copper-oxalate anionic complexes followed by an electroreductive precipitation to copper metal, or by electroreduction of polymer coated electrodes immersed in copper–oxalate aqueous solutions. The deposition process was examined by voltammetry. Scanning electron microscopy showed a dispersion of metal particles from 50–100 up to 300 nm, according to the lipophilic character of the polymer, located in a layer near the carbon∣polymer interface. A study of the electrocatalytic activity in the reduction of nitrobenzene to aniline at these materials was performed. The cathodes appeared much more active than bulk copper electrodes.</abstract><qualityIndicators><score>6.428</score><pdfVersion>1.2</pdfVersion><pdfPageSize>552 x 770 pts</pdfPageSize><refBibsNative>true</refBibsNative><keywordCount>4</keywordCount><abstractCharCount>881</abstractCharCount><pdfWordCount>5685</pdfWordCount><pdfCharCount>33761</pdfCharCount><pdfPageCount>10</pdfPageCount><abstractWordCount>119</abstractWordCount></qualityIndicators><title>Electrodeposition of copper into functionalized polypyrrole films</title><pii><json:string>S0022-0728(99)00310-1</json:string></pii><genre><json:string>research-article</json:string></genre><host><volume>474</volume><pii><json:string>S0022-0728(00)X0103-9</json:string></pii><pages><last>122</last><first>113</first></pages><issn><json:string>1572-6657</json:string></issn><issue>2</issue><genre><json:string>journal</json:string></genre><language><json:string>unknown</json:string></language><title>Journal of Electroanalytical Chemistry</title><publicationDate>1999</publicationDate></host><categories><wos><json:string>CHEMISTRY, ANALYTICAL</json:string><json:string>ELECTROCHEMISTRY</json:string></wos></categories><publicationDate>1999</publicationDate><copyrightDate>1999</copyrightDate><doi><json:string>10.1016/S0022-0728(99)00310-1</json:string></doi><id>2DE5F8979AAAE687376A593CCB269AF4CAB3E7F6</id><score>0.042285845</score><fulltext><json:item><original>true</original><mimetype>application/pdf</mimetype><extension>pdf</extension><uri>https://api.istex.fr/document/2DE5F8979AAAE687376A593CCB269AF4CAB3E7F6/fulltext/pdf</uri></json:item><json:item><original>false</original><mimetype>application/zip</mimetype><extension>zip</extension><uri>https://api.istex.fr/document/2DE5F8979AAAE687376A593CCB269AF4CAB3E7F6/fulltext/zip</uri></json:item><istex:fulltextTEI uri="https://api.istex.fr/document/2DE5F8979AAAE687376A593CCB269AF4CAB3E7F6/fulltext/tei"><teiHeader><fileDesc><titleStmt><title level="a" type="main" xml:lang="en">Electrodeposition of copper into functionalized polypyrrole films</title></titleStmt><publicationStmt><authority>ISTEX</authority><publisher>ELSEVIER</publisher><availability><p>©1999 Elsevier Science S.A.</p></availability><date>1999</date></publicationStmt><notesStmt><note type="content">Fig. 1: Distribution curves of the Cu2+ complexes in a solution containing copper sulfate (1 mM) and sodium oxalate (5 mM).</note><note type="content">Fig. 2: Cyclic voltammetry curves at a glassy carbon disc electrode (3 mm in diameter) for a solution containing 1 mM CuSO4 in 0.1 M Na2SO4: (a) without oxalate; (b) with 5 mM Na2(Ox); ν=0.1 V s−1.</note><note type="content">Fig. 3: Rotating disc (3 mm in diameter) voltammograms recorded on naked carbon (curves a and c) and on carbon∣poly1 (ΓN+=8.5×10−8 mol cm−2) modified electrodes (curves b and d) in a solution containing 1 mM CuSO4 in 0.1 M Na2SO4: (a, b) without oxalate; (c, d) with 5 mM Na2(Ox); ω=600 rev min−1; ν=10 mV s−1.</note><note type="content">Fig. 4: Copper metal anodic stripping waves in clean 0.1 M Na2SO4 electrolyte, following copper deposition in poly1 films by reduction at −0.36 V in Na2SO4 electrolyte containing 1 mM CuSO4 and 5 mM Na2(Ox) using different cathodic charges: (A) 1 mC; (B) 3 mC and (C) 6 mC (ΓN+=6×10−8 mol cm−2); (D) 6 mC in a thicker film (ΓN+=1.2×10−7 mol cm−2); (E) copper on naked carbon, charge passed 6 mC; ν=10 mV s−1; carbon disc electrode 3 mm in diameter.</note><note type="content">Fig. 5: Cyclic voltammetry curves (curves a: 1st cycle; curves b: 2nd cycle) in (A, C) 0.1 M LiClO4 and (B) 0.4 M H2SO4 electrolyte for copper metal dissolution from 10×10×4 mm carbon felt electrodes coated with poly1; (A) copper incorporation by the ion-exchange procedure (see the text) in a film containing 1.2×10−6 mol of alkylammonium units; (B) copper incorporation by electroreduction of the modified electrode (0.9×10−6 mol of alkylammonium units) in copper–oxalate media (see the text); (C) copper dissolution from a naked 10×10×4 mm carbon felt electrode after copper deposition in the same conditions as in (B), charge passed 1 C; ν=10 mV s−1.</note><note type="content">Fig. 6: Cyclic voltammetry curves in Na2SO4 electrolyte (curves a: 1st cycle; curves b: 2nd cycle) for copper metal dissolution from 10×10×4 mm carbon felt electrodes modified with poly2 films (1.2×10−6 mol of alkylammonium units) in which copper has been deposited using the ion-exchange procedure: (A) 1 incorporation, and (B) 3 incorporations of metal (see text); ν=10 mV s−1.</note><note type="content">Fig. 7: SEM micrographs of (A) surface, and (B, C) cross-section of a poly1 film (ΓN+=2.5×10−7 mol cm−2) after incorporation of copper microparticles by direct electroreduction in copper–oxalate media (charge passed 200 mC cm−2; 10−6 mol cm−2 of copper).</note><note type="content">Fig. 8: SEM micrographs of copper microparticles deposited in poly2 films by direct electroreduction in copper–oxalate media using different cathodic charges: (A) 100 mC cm−2 (5×10−7 mol cm−2 of copper; ΓN+=2×10−7 mol cm−2); (B) 200 mC cm−2 (10−6 mol cm−2 of copper; ΓN+=2.6×10−7 mol cm−2)</note><note type="content">Fig. 9: SEM micrograph of copper microparticles electrodeposited using the ion-exchange/electroreduction procedure (performed twice) in poly1 coated on carbon felt.</note><note type="content">Table 1: Hydrogenation of nitrobenzenea at C∣poly1–Cu and C∣poly2–Cu modified electrodes</note></notesStmt><sourceDesc><biblStruct type="inbook"><analytic><title level="a" type="main" xml:lang="en">Electrodeposition of copper into functionalized polypyrrole films</title><author xml:id="author-1"><persName><forename type="first">Ahmed</forename><surname>Zouaoui</surname></persName><note type="biography">Permanent address: Institut de Chimie Industrielle, Université Ferhat Abbas, Sétif, Algérie.</note><affiliation>Permanent address: Institut de Chimie Industrielle, Université Ferhat Abbas, Sétif, Algérie.</affiliation><affiliation>Laboratoire d’Electrochimie Organique et de Photochimie Rédox, UMR CNRS 5630, Université Joseph Fourier Grenoble I, BP 53, 38041 Grenoble Cedex 9, France</affiliation></author><author xml:id="author-2"><persName><forename type="first">Olivier</forename><surname>Stéphan</surname></persName><affiliation>Laboratoire de Spectrométrie Physique, Equipe Matériaux Electroactifs, UMR CNRS 5588, Université Joseph Fourier Grenoble 1, BP 87, 38402 Saint Martin d’Hères Cedex, France</affiliation></author><author xml:id="author-3"><persName><forename type="first">Michel</forename><surname>Carrier</surname></persName><affiliation>Institut National des Sciences et Techniques Nucléaires, CEA-Saclay, 91191 Gif-sur-Yvette, France</affiliation></author><author xml:id="author-4"><persName><forename type="first">Jean-Claude</forename><surname>Moutet</surname></persName><email>jean-claude.moutet@ujf-grenoble.fr</email><note type="correspondence"><p>Corresponding author. Fax: +33-04-76514267</p></note><affiliation>Laboratoire d’Electrochimie Organique et de Photochimie Rédox, UMR CNRS 5630, Université Joseph Fourier Grenoble I, BP 53, 38041 Grenoble Cedex 9, France</affiliation></author></analytic><monogr><title level="j">Journal of Electroanalytical Chemistry</title><title level="j" type="abbrev">JEC</title><idno type="pISSN">1572-6657</idno><idno type="PII">S0022-0728(00)X0103-9</idno><imprint><publisher>ELSEVIER</publisher><date type="published" when="1999"></date><biblScope unit="volume">474</biblScope><biblScope unit="issue">2</biblScope><biblScope unit="page" from="113">113</biblScope><biblScope unit="page" to="122">122</biblScope></imprint></monogr><idno type="istex">2DE5F8979AAAE687376A593CCB269AF4CAB3E7F6</idno><idno type="DOI">10.1016/S0022-0728(99)00310-1</idno><idno type="PII">S0022-0728(99)00310-1</idno></biblStruct></sourceDesc></fileDesc><profileDesc><creation><date>1999</date></creation><langUsage><language ident="en">en</language></langUsage><abstract xml:lang="en"><p>Copper microparticles have been dispersed in anion-exchange polymer films coated on carbon electrodes by oxidative electropolymerization of pyrrole–alkylammonium monomers. Incorporation of copper in polymeric films was effected by impregnation of copper-oxalate anionic complexes followed by an electroreductive precipitation to copper metal, or by electroreduction of polymer coated electrodes immersed in copper–oxalate aqueous solutions. The deposition process was examined by voltammetry. Scanning electron microscopy showed a dispersion of metal particles from 50–100 up to 300 nm, according to the lipophilic character of the polymer, located in a layer near the carbon∣polymer interface. A study of the electrocatalytic activity in the reduction of nitrobenzene to aniline at these materials was performed. The cathodes appeared much more active than bulk copper electrodes.</p></abstract><textClass xml:lang="en"><keywords scheme="keyword"><list><head>Keywords</head><item><term>Modified electrode</term></item><item><term>Functionalized polypyrrole</term></item><item><term>Electrocatalysis</term></item><item><term>Copper complexes</term></item></list></keywords></textClass></profileDesc><revisionDesc><change when="1999-06-14">Modified</change><change when="1999">Published</change></revisionDesc></teiHeader></istex:fulltextTEI><json:item><original>false</original><mimetype>text/plain</mimetype><extension>txt</extension><uri>https://api.istex.fr/document/2DE5F8979AAAE687376A593CCB269AF4CAB3E7F6/fulltext/txt</uri></json:item></fulltext><metadata><istex:metadataXml wicri:clean="Elsevier, elements deleted: ce:floats; body; tail"><istex:xmlDeclaration>version="1.0" encoding="utf-8"</istex:xmlDeclaration><istex:docType PUBLIC="-//ES//DTD journal article DTD version 4.5.2//EN//XML" URI="art452.dtd" name="istex:docType"><istex:entity SYSTEM="fx1" NDATA="IMAGE" name="fx1"></istex:entity><istex:entity SYSTEM="gr1" NDATA="IMAGE" name="gr1"></istex:entity><istex:entity SYSTEM="gr2" NDATA="IMAGE" name="gr2"></istex:entity><istex:entity SYSTEM="gr3" NDATA="IMAGE" name="gr3"></istex:entity><istex:entity SYSTEM="gr4" NDATA="IMAGE" name="gr4"></istex:entity><istex:entity SYSTEM="gr5" NDATA="IMAGE" name="gr5"></istex:entity><istex:entity SYSTEM="gr6" NDATA="IMAGE" name="gr6"></istex:entity><istex:entity SYSTEM="gr7" NDATA="IMAGE" name="gr7"></istex:entity><istex:entity SYSTEM="gr8" NDATA="IMAGE" name="gr8"></istex:entity><istex:entity SYSTEM="gr9" NDATA="IMAGE" name="gr9"></istex:entity></istex:docType><istex:document><converted-article version="4.5.2" docsubtype="fla" xml:lang="en"><item-info><jid>JEC</jid><aid>8363</aid><ce:pii>S0022-0728(99)00310-1</ce:pii><ce:doi>10.1016/S0022-0728(99)00310-1</ce:doi><ce:copyright type="full-transfer" year="1999">Elsevier Science S.A.</ce:copyright></item-info><head><ce:title>Electrodeposition of copper into functionalized polypyrrole films</ce:title><ce:author-group><ce:author><ce:given-name>Ahmed</ce:given-name><ce:surname>Zouaoui</ce:surname><ce:cross-ref refid="FN1"><ce:sup>1</ce:sup></ce:cross-ref><ce:cross-ref refid="AFF1"><ce:sup>a</ce:sup></ce:cross-ref></ce:author><ce:author><ce:given-name>Olivier</ce:given-name><ce:surname>Stéphan</ce:surname><ce:cross-ref refid="AFF2"><ce:sup>b</ce:sup></ce:cross-ref></ce:author><ce:author><ce:given-name>Michel</ce:given-name><ce:surname>Carrier</ce:surname><ce:cross-ref refid="AFF3"><ce:sup>c</ce:sup></ce:cross-ref></ce:author><ce:author><ce:given-name>Jean-Claude</ce:given-name><ce:surname>Moutet</ce:surname><ce:cross-ref refid="AFF1"><ce:sup>a</ce:sup></ce:cross-ref><ce:cross-ref refid="CORR1">*</ce:cross-ref><ce:e-address>jean-claude.moutet@ujf-grenoble.fr</ce:e-address></ce:author><ce:affiliation id="AFF1"><ce:label>a</ce:label><ce:textfn>Laboratoire d’Electrochimie Organique et de Photochimie Rédox, UMR CNRS 5630, Université Joseph Fourier Grenoble I, BP 53, 38041 Grenoble Cedex 9, France</ce:textfn></ce:affiliation><ce:affiliation id="AFF2"><ce:label>b</ce:label><ce:textfn>Laboratoire de Spectrométrie Physique, Equipe Matériaux Electroactifs, UMR CNRS 5588, Université Joseph Fourier Grenoble 1, BP 87, 38402 Saint Martin d’Hères Cedex, France</ce:textfn></ce:affiliation><ce:affiliation id="AFF3"><ce:label>c</ce:label><ce:textfn>Institut National des Sciences et Techniques Nucléaires, CEA-Saclay, 91191 Gif-sur-Yvette, France</ce:textfn></ce:affiliation><ce:correspondence id="CORR1"><ce:label>*</ce:label><ce:text>Corresponding author. Fax: +33-04-76514267</ce:text></ce:correspondence><ce:footnote id="FN1"><ce:label>1</ce:label><ce:note-para>Permanent address: Institut de Chimie Industrielle, Université Ferhat Abbas, Sétif, Algérie.</ce:note-para></ce:footnote></ce:author-group><ce:date-received day="23" month="2" year="1999"></ce:date-received><ce:date-revised day="14" month="6" year="1999"></ce:date-revised><ce:date-accepted day="6" month="7" year="1999"></ce:date-accepted><ce:abstract><ce:section-title>Abstract</ce:section-title><ce:abstract-sec><ce:simple-para>Copper microparticles have been dispersed in anion-exchange polymer films coated on carbon electrodes by oxidative electropolymerization of pyrrole–alkylammonium monomers. Incorporation of copper in polymeric films was effected by impregnation of copper-oxalate anionic complexes followed by an electroreductive precipitation to copper metal, or by electroreduction of polymer coated electrodes immersed in copper–oxalate aqueous solutions. The deposition process was examined by voltammetry. Scanning electron microscopy showed a dispersion of metal particles from 50–100 up to 300 nm, according to the lipophilic character of the polymer, located in a layer near the carbon<ce:hsp sp="0.25"></ce:hsp>∣<ce:hsp sp="0.25"></ce:hsp>polymer interface. A study of the electrocatalytic activity in the reduction of nitrobenzene to aniline at these materials was performed. The cathodes appeared much more active than bulk copper electrodes.</ce:simple-para></ce:abstract-sec></ce:abstract><ce:keywords class="keyword"><ce:section-title>Keywords</ce:section-title><ce:keyword><ce:text>Modified electrode</ce:text></ce:keyword><ce:keyword><ce:text>Functionalized polypyrrole</ce:text></ce:keyword><ce:keyword><ce:text>Electrocatalysis</ce:text></ce:keyword><ce:keyword><ce:text>Copper complexes</ce:text></ce:keyword></ce:keywords></head></converted-article></istex:document></istex:metadataXml><mods version="3.6"><titleInfo lang="en"><title>Electrodeposition of copper into functionalized polypyrrole films</title></titleInfo><titleInfo type="alternative" lang="en" contentType="CDATA"><title>Electrodeposition of copper into functionalized polypyrrole films</title></titleInfo><name type="personal"><namePart type="given">Ahmed</namePart><namePart type="family">Zouaoui</namePart><affiliation>Laboratoire d’Electrochimie Organique et de Photochimie Rédox, UMR CNRS 5630, Université Joseph Fourier Grenoble I, BP 53, 38041 Grenoble Cedex 9, France</affiliation><description>Permanent address: Institut de Chimie Industrielle, Université Ferhat Abbas, Sétif, Algérie.</description><role><roleTerm type="text">author</roleTerm></role></name><name type="personal"><namePart type="given">Olivier</namePart><namePart type="family">Stéphan</namePart><affiliation>Laboratoire de Spectrométrie Physique, Equipe Matériaux Electroactifs, UMR CNRS 5588, Université Joseph Fourier Grenoble 1, BP 87, 38402 Saint Martin d’Hères Cedex, France</affiliation><role><roleTerm type="text">author</roleTerm></role></name><name type="personal"><namePart type="given">Michel</namePart><namePart type="family">Carrier</namePart><affiliation>Institut National des Sciences et Techniques Nucléaires, CEA-Saclay, 91191 Gif-sur-Yvette, France</affiliation><role><roleTerm type="text">author</roleTerm></role></name><name type="personal"><namePart type="given">Jean-Claude</namePart><namePart type="family">Moutet</namePart><affiliation>E-mail: jean-claude.moutet@ujf-grenoble.fr</affiliation><affiliation>Laboratoire d’Electrochimie Organique et de Photochimie Rédox, UMR CNRS 5630, Université Joseph Fourier Grenoble I, BP 53, 38041 Grenoble Cedex 9, France</affiliation><description>Corresponding author. Fax: +33-04-76514267</description><role><roleTerm type="text">author</roleTerm></role></name><typeOfResource>text</typeOfResource><genre type="research-article" displayLabel="Full-length article"></genre><originInfo><publisher>ELSEVIER</publisher><dateIssued encoding="w3cdtf">1999</dateIssued><dateModified encoding="w3cdtf">1999-06-14</dateModified><copyrightDate encoding="w3cdtf">1999</copyrightDate></originInfo><language><languageTerm type="code" authority="iso639-2b">eng</languageTerm><languageTerm type="code" authority="rfc3066">en</languageTerm></language><physicalDescription><internetMediaType>text/html</internetMediaType></physicalDescription><abstract lang="en">Copper microparticles have been dispersed in anion-exchange polymer films coated on carbon electrodes by oxidative electropolymerization of pyrrole–alkylammonium monomers. Incorporation of copper in polymeric films was effected by impregnation of copper-oxalate anionic complexes followed by an electroreductive precipitation to copper metal, or by electroreduction of polymer coated electrodes immersed in copper–oxalate aqueous solutions. The deposition process was examined by voltammetry. Scanning electron microscopy showed a dispersion of metal particles from 50–100 up to 300 nm, according to the lipophilic character of the polymer, located in a layer near the carbon∣polymer interface. A study of the electrocatalytic activity in the reduction of nitrobenzene to aniline at these materials was performed. The cathodes appeared much more active than bulk copper electrodes.</abstract><note type="content">Fig. 1: Distribution curves of the Cu2+ complexes in a solution containing copper sulfate (1 mM) and sodium oxalate (5 mM).</note><note type="content">Fig. 2: Cyclic voltammetry curves at a glassy carbon disc electrode (3 mm in diameter) for a solution containing 1 mM CuSO4 in 0.1 M Na2SO4: (a) without oxalate; (b) with 5 mM Na2(Ox); ν=0.1 V s−1.</note><note type="content">Fig. 3: Rotating disc (3 mm in diameter) voltammograms recorded on naked carbon (curves a and c) and on carbon∣poly1 (ΓN+=8.5×10−8 mol cm−2) modified electrodes (curves b and d) in a solution containing 1 mM CuSO4 in 0.1 M Na2SO4: (a, b) without oxalate; (c, d) with 5 mM Na2(Ox); ω=600 rev min−1; ν=10 mV s−1.</note><note type="content">Fig. 4: Copper metal anodic stripping waves in clean 0.1 M Na2SO4 electrolyte, following copper deposition in poly1 films by reduction at −0.36 V in Na2SO4 electrolyte containing 1 mM CuSO4 and 5 mM Na2(Ox) using different cathodic charges: (A) 1 mC; (B) 3 mC and (C) 6 mC (ΓN+=6×10−8 mol cm−2); (D) 6 mC in a thicker film (ΓN+=1.2×10−7 mol cm−2); (E) copper on naked carbon, charge passed 6 mC; ν=10 mV s−1; carbon disc electrode 3 mm in diameter.</note><note type="content">Fig. 5: Cyclic voltammetry curves (curves a: 1st cycle; curves b: 2nd cycle) in (A, C) 0.1 M LiClO4 and (B) 0.4 M H2SO4 electrolyte for copper metal dissolution from 10×10×4 mm carbon felt electrodes coated with poly1; (A) copper incorporation by the ion-exchange procedure (see the text) in a film containing 1.2×10−6 mol of alkylammonium units; (B) copper incorporation by electroreduction of the modified electrode (0.9×10−6 mol of alkylammonium units) in copper–oxalate media (see the text); (C) copper dissolution from a naked 10×10×4 mm carbon felt electrode after copper deposition in the same conditions as in (B), charge passed 1 C; ν=10 mV s−1.</note><note type="content">Fig. 6: Cyclic voltammetry curves in Na2SO4 electrolyte (curves a: 1st cycle; curves b: 2nd cycle) for copper metal dissolution from 10×10×4 mm carbon felt electrodes modified with poly2 films (1.2×10−6 mol of alkylammonium units) in which copper has been deposited using the ion-exchange procedure: (A) 1 incorporation, and (B) 3 incorporations of metal (see text); ν=10 mV s−1.</note><note type="content">Fig. 7: SEM micrographs of (A) surface, and (B, C) cross-section of a poly1 film (ΓN+=2.5×10−7 mol cm−2) after incorporation of copper microparticles by direct electroreduction in copper–oxalate media (charge passed 200 mC cm−2; 10−6 mol cm−2 of copper).</note><note type="content">Fig. 8: SEM micrographs of copper microparticles deposited in poly2 films by direct electroreduction in copper–oxalate media using different cathodic charges: (A) 100 mC cm−2 (5×10−7 mol cm−2 of copper; ΓN+=2×10−7 mol cm−2); (B) 200 mC cm−2 (10−6 mol cm−2 of copper; ΓN+=2.6×10−7 mol cm−2)</note><note type="content">Fig. 9: SEM micrograph of copper microparticles electrodeposited using the ion-exchange/electroreduction procedure (performed twice) in poly1 coated on carbon felt.</note><note type="content">Table 1: Hydrogenation of nitrobenzenea at C∣poly1–Cu and C∣poly2–Cu modified electrodes</note><subject lang="en"><genre>Keywords</genre><topic>Modified electrode</topic><topic>Functionalized polypyrrole</topic><topic>Electrocatalysis</topic><topic>Copper complexes</topic></subject><relatedItem type="host"><titleInfo><title>Journal of Electroanalytical Chemistry</title></titleInfo><titleInfo type="abbreviated"><title>JEC</title></titleInfo><genre type="journal">journal</genre><originInfo><dateIssued encoding="w3cdtf">19990927</dateIssued></originInfo><identifier type="ISSN">1572-6657</identifier><identifier type="PII">S0022-0728(00)X0103-9</identifier><part><date>19990927</date><detail type="volume"><number>474</number><caption>vol.</caption></detail><detail type="issue"><number>2</number><caption>no.</caption></detail><extent unit="issue pages"><start>101</start><end>201</end></extent><extent unit="pages"><start>113</start><end>122</end></extent></part></relatedItem><identifier type="istex">2DE5F8979AAAE687376A593CCB269AF4CAB3E7F6</identifier><identifier type="DOI">10.1016/S0022-0728(99)00310-1</identifier><identifier type="PII">S0022-0728(99)00310-1</identifier><accessCondition type="use and reproduction" contentType="copyright">©1999 Elsevier Science S.A.</accessCondition><recordInfo><recordContentSource>ELSEVIER</recordContentSource><recordOrigin>Elsevier Science S.A., ©1999</recordOrigin></recordInfo></mods></metadata><serie></serie></istex></record>Pour manipuler ce document sous Unix (Dilib)
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