Structure and evolved gas analyses (TG/DTA-MS and TG-FTIR) of mer-trichlorotris(thiourea)-indium(III), a precursor for indium sulfide thin films
Identifieur interne : 002476 ( Main/Repository ); précédent : 002475; suivant : 002477Structure and evolved gas analyses (TG/DTA-MS and TG-FTIR) of mer-trichlorotris(thiourea)-indium(III), a precursor for indium sulfide thin films
Auteurs : RBID : Pascal:12-0139138Descripteurs français
- Pascal (Inist)
- Analyse thermique différentielle, Thermogravimétrie, Spectrométrie masse, Méthode couplée, Thiourée, Indium III Complexe, Complexe chloro, Précurseur, Indium Sulfure, Couche mince, Monocristal, Diffraction RX, Analyse gaz, Dégagement gazeux, Analyse thermique, Spectrométrie IR, Transformation Fourier, FT IR, Analyse gaz dégagé, Dépôt par pyrolyse d'aérosol.
English descriptors
- KwdEn :
- Chloro complex, Coupled method, Differential thermal analysis, Evolved gas analysis, Fourier transformation, Gas analysis, Gas release, Indium III Complexes, Indium Sulfides, Infrared spectrometry, Mass spectrometry, Precursor, Single crystal, Spray pyrolysis, Thermal analysis, Thermogravimetry, Thin film, Thiourea, X ray diffraction.
Abstract
The indium complex, mer-trichlorotris(thiourea)-indium(III) (In(tu)3Cl3, 1), crystallized from aqueous solution of InCl3 and SC(NH2)2 (tu) with molar ratio of 1:3, is a single-source precursor for In2S3 films by chemical spray pyrolysis. The structural model of the triclinic crystal 1 (space group P-1 with a = 8.4842(2) Å, b = 10.5174(2) Å, c = 13.1767(2) Å, α = 111.1870(10)°, β = 98.0870(10)°, γ = 97.889(2)°) has been improved by single crystal X-ray diffraction analysis through successful separation of the disordered positions of the asymmetric complex molecule situated on the inversion centre into two spatial arrangements. Thermal decomposition of 1 occurs with very similar mass loss courses till 400 °C in both nitrogen and air, anyhow the DTA curve indicates a gas-phase oxidation with an additional exothermic heat effect at 255 °C in air. Partial or more advanced oxidation of the initially evolved CS2 has taken place in both atmospheres, as its oxidation products, SO2, COS, CO2 are accompanied by the release of NH3, HCl in temperature range of 205-275 °C, while H2NCN and HCN evolve in air. In the third mass loss step, in the temperature interval of 405-750 °C in nitrogen and 405-700 °C in air, two processes, evaporation and oxidation of the solid residues are competing with each other, resulting in final decomposition product of 1 in air In2O3, while also some In2O3 in inert atmosphere beyond the main phase of In2S3 where, in addition considerable extent of loss of indium occurs, probably through volatile dimeric indium chloride species, which could not be detected either by EGA-MS or EGA-FTIR systems of ours. Nevertheless, evolution of HNCS is confirmed by EGA-FTIR, and release of CO2, H2NCN, SO2, and a little HCl is detected at temperatures above 450 °C in both atmospheres.
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<record><TEI><teiHeader><fileDesc><titleStmt><title xml:lang="en" level="a">Structure and evolved gas analyses (TG/DTA-MS and TG-FTIR) of mer-trichlorotris(thiourea)-indium(III), a precursor for indium sulfide thin films</title><author><name sortKey="Otto, Kairi" uniqKey="Otto K">Kairi Otto</name><affiliation wicri:level="1"><inist:fA14 i1="01"><s1>Department of Materials Science, Tallinn University of Technology, Ehitajate tee 5</s1><s2>Tallinn 19086</s2><s3>EST</s3><sZ>1 aut.</sZ><sZ>4 aut.</sZ><sZ>5 aut.</sZ></inist:fA14><country>Estonie</country><wicri:noRegion>Tallinn 19086</wicri:noRegion></affiliation></author><author><name sortKey="Bombicz, Petra" uniqKey="Bombicz P">Petra Bombicz</name><affiliation wicri:level="1"><inist:fA14 i1="02"><s1>Institute of Structural Chemistry, Chemical Research Center, Hungarian Academy of Sciences, POB 17</s1><s2>Budapest 1525</s2><s3>HUN</s3><sZ>2 aut.</sZ></inist:fA14><country>Hongrie</country><placeName><settlement type="city">Budapest</settlement><region nuts="2">Hongrie centrale</region></placeName></affiliation></author><author><name sortKey="Madarasz, J Nos" uniqKey="Madarasz J">J Nos Madarasz</name><affiliation wicri:level="1"><inist:fA14 i1="03"><s1>Department of Inorganic and Analytical Chemistry, Budapest University of Technology and Economics, Szt. Gellért tér 4</s1><s2>Budapest 1521</s2><s3>HUN</s3><sZ>3 aut.</sZ><sZ>6 aut.</sZ></inist:fA14><country>Hongrie</country><placeName><settlement type="city">Budapest</settlement><region nuts="2">Hongrie centrale</region></placeName></affiliation></author><author><name sortKey="Oja Acik, Ilona" uniqKey="Oja Acik I">Ilona Oja Acik</name><affiliation wicri:level="1"><inist:fA14 i1="01"><s1>Department of Materials Science, Tallinn University of Technology, Ehitajate tee 5</s1><s2>Tallinn 19086</s2><s3>EST</s3><sZ>1 aut.</sZ><sZ>4 aut.</sZ><sZ>5 aut.</sZ></inist:fA14><country>Estonie</country><wicri:noRegion>Tallinn 19086</wicri:noRegion></affiliation></author><author><name sortKey="Krunks, Malle" uniqKey="Krunks M">Malle Krunks</name><affiliation wicri:level="1"><inist:fA14 i1="01"><s1>Department of Materials Science, Tallinn University of Technology, Ehitajate tee 5</s1><s2>Tallinn 19086</s2><s3>EST</s3><sZ>1 aut.</sZ><sZ>4 aut.</sZ><sZ>5 aut.</sZ></inist:fA14><country>Estonie</country><wicri:noRegion>Tallinn 19086</wicri:noRegion></affiliation></author><author><name sortKey="Pokol, Gy Rgy" uniqKey="Pokol G">Gy Rgy Pokol</name><affiliation wicri:level="1"><inist:fA14 i1="03"><s1>Department of Inorganic and Analytical Chemistry, Budapest University of Technology and Economics, Szt. Gellért tér 4</s1><s2>Budapest 1521</s2><s3>HUN</s3><sZ>3 aut.</sZ><sZ>6 aut.</sZ></inist:fA14><country>Hongrie</country><placeName><settlement type="city">Budapest</settlement><region nuts="2">Hongrie centrale</region></placeName></affiliation></author></titleStmt><publicationStmt><idno type="inist">12-0139138</idno><date when="2011">2011</date><idno type="stanalyst">PASCAL 12-0139138 INIST</idno><idno type="RBID">Pascal:12-0139138</idno><idno type="wicri:Area/Main/Corpus">002018</idno><idno type="wicri:Area/Main/Repository">002476</idno></publicationStmt><seriesStmt><idno type="ISSN">1388-6150</idno><title level="j" type="abbreviated">J. therm. anal. calorim.</title><title level="j" type="main">Journal of thermal analysis and calorimetry</title></seriesStmt></fileDesc><profileDesc><textClass><keywords scheme="KwdEn" xml:lang="en"><term>Chloro complex</term><term>Coupled method</term><term>Differential thermal analysis</term><term>Evolved gas analysis</term><term>Fourier transformation</term><term>Gas analysis</term><term>Gas release</term><term>Indium III Complexes</term><term>Indium Sulfides</term><term>Infrared spectrometry</term><term>Mass spectrometry</term><term>Precursor</term><term>Single crystal</term><term>Spray pyrolysis</term><term>Thermal analysis</term><term>Thermogravimetry</term><term>Thin film</term><term>Thiourea</term><term>X ray diffraction</term></keywords><keywords scheme="Pascal" xml:lang="fr"><term>Analyse thermique différentielle</term><term>Thermogravimétrie</term><term>Spectrométrie masse</term><term>Méthode couplée</term><term>Thiourée</term><term>Indium III Complexe</term><term>Complexe chloro</term><term>Précurseur</term><term>Indium Sulfure</term><term>Couche mince</term><term>Monocristal</term><term>Diffraction RX</term><term>Analyse gaz</term><term>Dégagement gazeux</term><term>Analyse thermique</term><term>Spectrométrie IR</term><term>Transformation Fourier</term><term>FT IR</term><term>Analyse gaz dégagé</term><term>Dépôt par pyrolyse d'aérosol</term></keywords></textClass></profileDesc></teiHeader><front><div type="abstract" xml:lang="en">The indium complex, mer-trichlorotris(thiourea)-indium(III) (In(tu)<sub>3</sub>Cl<sub>3</sub>, 1), crystallized from aqueous solution of InCl<sub>3</sub> and SC(NH<sub>2</sub>)<sub>2</sub> (tu) with molar ratio of 1:3, is a single-source precursor for In<sub>2</sub>S<sub>3</sub> films by chemical spray pyrolysis. The structural model of the triclinic crystal 1 (space group P-1 with a = 8.4842(2) Å, b = 10.5174(2) Å, c = 13.1767(2) Å, α = 111.1870(10)°, β = 98.0870(10)°, γ = 97.889(2)°) has been improved by single crystal X-ray diffraction analysis through successful separation of the disordered positions of the asymmetric complex molecule situated on the inversion centre into two spatial arrangements. Thermal decomposition of 1 occurs with very similar mass loss courses till 400 °C in both nitrogen and air, anyhow the DTA curve indicates a gas-phase oxidation with an additional exothermic heat effect at 255 °C in air. Partial or more advanced oxidation of the initially evolved CS<sub>2</sub> has taken place in both atmospheres, as its oxidation products, SO<sub>2</sub>, COS, CO<sub>2</sub> are accompanied by the release of NH<sub>3</sub>, HCl in temperature range of 205-275 °C, while H<sub>2</sub>NCN and HCN evolve in air. In the third mass loss step, in the temperature interval of 405-750 °C in nitrogen and 405-700 °C in air, two processes, evaporation and oxidation of the solid residues are competing with each other, resulting in final decomposition product of 1 in air In<sub>2</sub>O<sub>3</sub>, while also some In<sub>2</sub>O<sub>3</sub> in inert atmosphere beyond the main phase of In<sub>2</sub>S<sub>3</sub> where, in addition considerable extent of loss of indium occurs, probably through volatile dimeric indium chloride species, which could not be detected either by EGA-MS or EGA-FTIR systems of ours. Nevertheless, evolution of HNCS is confirmed by EGA-FTIR, and release of CO<sub>2</sub>, H<sub>2</sub>NCN, SO<sub>2</sub>, and a little HCl is detected at temperatures above 450 °C in both atmospheres.</div></front></TEI><inist><standard h6="B"><pA><fA01 i1="01" i2="1"><s0>1388-6150</s0></fA01><fA03 i2="1"><s0>J. therm. anal. calorim.</s0></fA03><fA05><s2>105</s2></fA05><fA06><s2>1</s2></fA06><fA08 i1="01" i2="1" l="ENG"><s1>Structure and evolved gas analyses (TG/DTA-MS and TG-FTIR) of mer-trichlorotris(thiourea)-indium(III), a precursor for indium sulfide thin films</s1></fA08><fA11 i1="01" i2="1"><s1>OTTO (Kairi)</s1></fA11><fA11 i1="02" i2="1"><s1>BOMBICZ (Petra)</s1></fA11><fA11 i1="03" i2="1"><s1>MADARASZ (János)</s1></fA11><fA11 i1="04" i2="1"><s1>OJA ACIK (Ilona)</s1></fA11><fA11 i1="05" i2="1"><s1>KRUNKS (Malle)</s1></fA11><fA11 i1="06" i2="1"><s1>POKOL (György)</s1></fA11><fA14 i1="01"><s1>Department of Materials Science, Tallinn University of Technology, Ehitajate tee 5</s1><s2>Tallinn 19086</s2><s3>EST</s3><sZ>1 aut.</sZ><sZ>4 aut.</sZ><sZ>5 aut.</sZ></fA14><fA14 i1="02"><s1>Institute of Structural Chemistry, Chemical Research Center, Hungarian Academy of Sciences, POB 17</s1><s2>Budapest 1525</s2><s3>HUN</s3><sZ>2 aut.</sZ></fA14><fA14 i1="03"><s1>Department of Inorganic and Analytical Chemistry, Budapest University of Technology and Economics, Szt. Gellért tér 4</s1><s2>Budapest 1521</s2><s3>HUN</s3><sZ>3 aut.</sZ><sZ>6 aut.</sZ></fA14><fA20><s1>83-91</s1></fA20><fA21><s1>2011</s1></fA21><fA23 i1="01"><s0>ENG</s0></fA23><fA43 i1="01"><s1>INIST</s1><s2>6367</s2><s5>354000190451120090</s5></fA43><fA44><s0>0000</s0><s1>© 2012 INIST-CNRS. All rights reserved.</s1></fA44><fA45><s0>27 ref.</s0></fA45><fA47 i1="01" i2="1"><s0>12-0139138</s0></fA47><fA60><s1>P</s1></fA60><fA61><s0>A</s0></fA61><fA64 i1="01" i2="1"><s0>Journal of thermal analysis and calorimetry</s0></fA64><fA66 i1="01"><s0>NLD</s0></fA66><fC01 i1="01" l="ENG"><s0>The indium complex, mer-trichlorotris(thiourea)-indium(III) (In(tu)<sub>3</sub>Cl<sub>3</sub>, 1), crystallized from aqueous solution of InCl<sub>3</sub> and SC(NH<sub>2</sub>)<sub>2</sub> (tu) with molar ratio of 1:3, is a single-source precursor for In<sub>2</sub>S<sub>3</sub> films by chemical spray pyrolysis. The structural model of the triclinic crystal 1 (space group P-1 with a = 8.4842(2) Å, b = 10.5174(2) Å, c = 13.1767(2) Å, α = 111.1870(10)°, β = 98.0870(10)°, γ = 97.889(2)°) has been improved by single crystal X-ray diffraction analysis through successful separation of the disordered positions of the asymmetric complex molecule situated on the inversion centre into two spatial arrangements. Thermal decomposition of 1 occurs with very similar mass loss courses till 400 °C in both nitrogen and air, anyhow the DTA curve indicates a gas-phase oxidation with an additional exothermic heat effect at 255 °C in air. Partial or more advanced oxidation of the initially evolved CS<sub>2</sub> has taken place in both atmospheres, as its oxidation products, SO<sub>2</sub>, COS, CO<sub>2</sub> are accompanied by the release of NH<sub>3</sub>, HCl in temperature range of 205-275 °C, while H<sub>2</sub>NCN and HCN evolve in air. In the third mass loss step, in the temperature interval of 405-750 °C in nitrogen and 405-700 °C in air, two processes, evaporation and oxidation of the solid residues are competing with each other, resulting in final decomposition product of 1 in air In<sub>2</sub>O<sub>3</sub>, while also some In<sub>2</sub>O<sub>3</sub> in inert atmosphere beyond the main phase of In<sub>2</sub>S<sub>3</sub> where, in addition considerable extent of loss of indium occurs, probably through volatile dimeric indium chloride species, which could not be detected either by EGA-MS or EGA-FTIR systems of ours. Nevertheless, evolution of HNCS is confirmed by EGA-FTIR, and release of CO<sub>2</sub>, H<sub>2</sub>NCN, SO<sub>2</sub>, and a little HCl is detected at temperatures above 450 °C in both atmospheres.</s0></fC01><fC02 i1="01" i2="X"><s0>001C02B04</s0></fC02><fC03 i1="01" i2="X" l="FRE"><s0>Analyse thermique différentielle</s0><s5>01</s5></fC03><fC03 i1="01" i2="X" l="ENG"><s0>Differential thermal analysis</s0><s5>01</s5></fC03><fC03 i1="01" i2="X" l="SPA"><s0>Análisis térmico diferencial</s0><s5>01</s5></fC03><fC03 i1="02" i2="X" l="FRE"><s0>Thermogravimétrie</s0><s5>02</s5></fC03><fC03 i1="02" i2="X" l="ENG"><s0>Thermogravimetry</s0><s5>02</s5></fC03><fC03 i1="02" i2="X" l="SPA"><s0>Termogravimetría</s0><s5>02</s5></fC03><fC03 i1="03" i2="X" l="FRE"><s0>Spectrométrie masse</s0><s5>03</s5></fC03><fC03 i1="03" i2="X" l="ENG"><s0>Mass spectrometry</s0><s5>03</s5></fC03><fC03 i1="03" i2="X" l="SPA"><s0>Espectrometría masa</s0><s5>03</s5></fC03><fC03 i1="04" i2="X" l="FRE"><s0>Méthode couplée</s0><s5>04</s5></fC03><fC03 i1="04" i2="X" l="ENG"><s0>Coupled method</s0><s5>04</s5></fC03><fC03 i1="04" i2="X" l="SPA"><s0>Método acoplado</s0><s5>04</s5></fC03><fC03 i1="05" i2="X" l="FRE"><s0>Thiourée</s0><s5>05</s5></fC03><fC03 i1="05" i2="X" l="ENG"><s0>Thiourea</s0><s5>05</s5></fC03><fC03 i1="05" i2="X" l="SPA"><s0>Tiourea</s0><s5>05</s5></fC03><fC03 i1="06" i2="X" l="FRE"><s0>Indium III Complexe</s0><s2>NC</s2><s2>NA</s2><s5>06</s5></fC03><fC03 i1="06" i2="X" l="ENG"><s0>Indium III Complexes</s0><s2>NC</s2><s2>NA</s2><s5>06</s5></fC03><fC03 i1="06" i2="X" l="SPA"><s0>Indio III Complejo</s0><s2>NC</s2><s2>NA</s2><s5>06</s5></fC03><fC03 i1="07" i2="X" l="FRE"><s0>Complexe chloro</s0><s5>07</s5></fC03><fC03 i1="07" i2="X" l="ENG"><s0>Chloro complex</s0><s5>07</s5></fC03><fC03 i1="07" i2="X" l="SPA"><s0>Complejo cloro</s0><s5>07</s5></fC03><fC03 i1="08" i2="X" l="FRE"><s0>Précurseur</s0><s5>08</s5></fC03><fC03 i1="08" i2="X" l="ENG"><s0>Precursor</s0><s5>08</s5></fC03><fC03 i1="08" i2="X" l="SPA"><s0>Precursor</s0><s5>08</s5></fC03><fC03 i1="09" i2="X" l="FRE"><s0>Indium Sulfure</s0><s2>NC</s2><s2>NA</s2><s5>09</s5></fC03><fC03 i1="09" i2="X" l="ENG"><s0>Indium Sulfides</s0><s2>NC</s2><s2>NA</s2><s5>09</s5></fC03><fC03 i1="09" i2="X" l="SPA"><s0>Indio Sulfuro</s0><s2>NC</s2><s2>NA</s2><s5>09</s5></fC03><fC03 i1="10" i2="X" l="FRE"><s0>Couche mince</s0><s5>10</s5></fC03><fC03 i1="10" i2="X" l="ENG"><s0>Thin film</s0><s5>10</s5></fC03><fC03 i1="10" i2="X" l="SPA"><s0>Capa fina</s0><s5>10</s5></fC03><fC03 i1="11" i2="X" l="FRE"><s0>Monocristal</s0><s5>12</s5></fC03><fC03 i1="11" i2="X" l="ENG"><s0>Single crystal</s0><s5>12</s5></fC03><fC03 i1="11" i2="X" l="SPA"><s0>Monocristal</s0><s5>12</s5></fC03><fC03 i1="12" i2="X" l="FRE"><s0>Diffraction RX</s0><s5>13</s5></fC03><fC03 i1="12" i2="X" l="ENG"><s0>X ray diffraction</s0><s5>13</s5></fC03><fC03 i1="12" i2="X" l="SPA"><s0>Difracción RX</s0><s5>13</s5></fC03><fC03 i1="13" i2="X" l="FRE"><s0>Analyse gaz</s0><s5>32</s5></fC03><fC03 i1="13" i2="X" l="ENG"><s0>Gas analysis</s0><s5>32</s5></fC03><fC03 i1="13" i2="X" l="SPA"><s0>Análisis gas</s0><s5>32</s5></fC03><fC03 i1="14" i2="X" l="FRE"><s0>Dégagement gazeux</s0><s5>33</s5></fC03><fC03 i1="14" i2="X" l="ENG"><s0>Gas release</s0><s5>33</s5></fC03><fC03 i1="14" i2="X" l="SPA"><s0>Desprendimiento gaseoso</s0><s5>33</s5></fC03><fC03 i1="15" i2="X" l="FRE"><s0>Analyse thermique</s0><s5>34</s5></fC03><fC03 i1="15" i2="X" l="ENG"><s0>Thermal analysis</s0><s5>34</s5></fC03><fC03 i1="15" i2="X" l="SPA"><s0>Análisis térmico</s0><s5>34</s5></fC03><fC03 i1="16" i2="X" l="FRE"><s0>Spectrométrie IR</s0><s5>35</s5></fC03><fC03 i1="16" i2="X" l="ENG"><s0>Infrared spectrometry</s0><s5>35</s5></fC03><fC03 i1="16" i2="X" l="SPA"><s0>Espectrometría IR</s0><s5>35</s5></fC03><fC03 i1="17" i2="X" l="FRE"><s0>Transformation Fourier</s0><s5>36</s5></fC03><fC03 i1="17" i2="X" l="ENG"><s0>Fourier transformation</s0><s5>36</s5></fC03><fC03 i1="17" i2="X" l="SPA"><s0>Transformación Fourier</s0><s5>36</s5></fC03><fC03 i1="18" i2="X" l="FRE"><s0>FT IR</s0><s4>INC</s4><s5>76</s5></fC03><fC03 i1="19" i2="X" l="FRE"><s0>Analyse gaz dégagé</s0><s4>CD</s4><s5>96</s5></fC03><fC03 i1="19" i2="X" l="ENG"><s0>Evolved gas analysis</s0><s4>CD</s4><s5>96</s5></fC03><fC03 i1="20" i2="X" l="FRE"><s0>Dépôt par pyrolyse d'aérosol</s0><s4>CD</s4><s5>97</s5></fC03><fC03 i1="20" i2="X" l="ENG"><s0>Spray pyrolysis</s0><s4>CD</s4><s5>97</s5></fC03><fN21><s1>107</s1></fN21></pA></standard></inist></record>Pour manipuler ce document sous Unix (Dilib)
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