Indium hydroxide to oxide decomposition observed in one nanocrystal during in situ transmission electron microscopy studies
Identifieur interne : 000A77 ( Main/Repository ); précédent : 000A76; suivant : 000A78Indium hydroxide to oxide decomposition observed in one nanocrystal during in situ transmission electron microscopy studies
Auteurs : RBID : Pascal:13-0133960Descripteurs français
- Pascal (Inist)
- Oxyde d'indium, Hydroxyde d'indium, Nanocristal, Nanomatériau, Microscopie électronique transmission, Microscopie électronique haute résolution, Résolution spatiale, Etude cas, Faisceau électron, Morphologie cristalline, Effet rayonnement, Irradiation électron, Résolution temporelle, Spectre résolution temporelle, Monocristal, Orientation cristalline, Cinétique, Cristallisation, Diffraction électron sélection aire, Texture, Induction, Transformation Fourier, Fraction volumique, Transformation phase, Retrait, Mécanisme réaction, Nucléation, Mécanisme croissance, Constante vitesse, Taux croissance, Déplacement atomique, Liaison disponible, Substrat indium, In2O3, In, 8107, 6180F, 6470K, 8130H, Bixbyite.
English descriptors
- KwdEn :
- Atomic displacements, Bixbyite, Case study, Crystal morphology, Crystal orientation, Crystallization, Dangling bonds, Electron beams, Electron irradiation, Fourier transformation, Growth mechanism, Growth rate, High resolution electron microscopy, Indium hydroxide, Indium oxide, Induction, Kinetics, Monocrystals, Nanocrystal, Nanostructured materials, Nucleation, Phase transformations, Radiation effects, Rate constant, Reaction mechanism, SAED, Shrinkage, Spatial resolution, Texture, Time resolution, Time resolved spectra, Transmission electron microscopy, Volume fraction.
Abstract
The high-resolution transmission electron microscopy (HR-TEM) is used to study, in situ, spatially resolved decomposition in individual nanocrystals of metal hydroxides and oxyhydroxides. This case study reports on the decomposition of indium hydroxide (c-In(OH)3) to bixbyite-type indium oxide (c-In2O3). The electron beam is focused onto a single cube-shaped In(OH)3 crystal of {100} morphology with ca. 35 nm edge length and a sequence of HR-TEM images was recorded during electron beam irradiation. The frame-by-frame analysis of video sequences allows for the in situ, time-resolved observation of the shape and orientation of the transformed crystals, which in turn enables the evaluation of the kinetics of c-In2O3 crystallization. Supplementary material (video of the transformation) related to this article can be found online at http://dx.doi.org/10,1016/j.jssc.2012.09.022. After irradiation the shape of the parent cube-shaped crystal is preserved, however, its linear dimension (edge) is reduced by the factor 1.20. The corresponding spotted selected area electron diffraction (SAED) pattern representing zone [001] of c-In(OH)3 is transformed to a diffuse strongly textured ring-like pattern of c-In2O3 that indicates the transformed cube is no longer a single crystal but is disintegrated into individual c-In2O3 domains with the size of about 5-10 nm. The induction time of approximately 15 s is estimated from the time-resolved Fourier transforms. The volume fraction of the transformed phase (c-In2O3), calculated from the shrinkage of the parent c-In(OH)3 crystal in the recorded HR-TEM images, is used as a measure of the kinetics of c-In2O3 crystallization within the framework of Avrami-Erofeev formalism. The Avrami exponent of ∼3 is characteristic for a reaction mechanism with fast nucleation at the beginning of the reaction and subsequent three-dimensional growth of nuclei with a constant growth rate. The structural transformation path in reconstructive decomposition of c-In(OH)3 to c-In2O3 is discussed in terms of (i) the displacement of hydrogen atoms that lead to breaking the hydrogen bond between OH groups of [In(OH)6] octahedra and finally to their destabilization and (ii) transformation of the vertices-shared indium-oxygen octahedra in c-In(OH)3 to vertices- and edge-shared octahedra in c-In2O3.
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<record><TEI><teiHeader><fileDesc><titleStmt><title xml:lang="en" level="a">Indium hydroxide to oxide decomposition observed in one nanocrystal during in situ transmission electron microscopy studies</title><author><name sortKey="Miehe, Gerhard" uniqKey="Miehe G">Gerhard Miehe</name><affiliation wicri:level="3"><inist:fA14 i1="01"><s1>Technische Universität Darmstadt, Fachbereich Material- und Geowissenschaften, Petersenstr. 23</s1><s2>64287 Darmstadt</s2><s3>DEU</s3><sZ>1 aut.</sZ><sZ>2 aut.</sZ><sZ>3 aut.</sZ><sZ>4 aut.</sZ></inist:fA14><country>Allemagne</country><placeName><region type="land" nuts="1">Hesse (Land)</region><region type="district" nuts="2">District de Darmstadt</region><settlement type="city">Darmstadt</settlement></placeName></affiliation></author><author><name sortKey="Lauterbach, Stefan" uniqKey="Lauterbach S">Stefan Lauterbach</name><affiliation wicri:level="3"><inist:fA14 i1="01"><s1>Technische Universität Darmstadt, Fachbereich Material- und Geowissenschaften, Petersenstr. 23</s1><s2>64287 Darmstadt</s2><s3>DEU</s3><sZ>1 aut.</sZ><sZ>2 aut.</sZ><sZ>3 aut.</sZ><sZ>4 aut.</sZ></inist:fA14><country>Allemagne</country><placeName><region type="land" nuts="1">Hesse (Land)</region><region type="district" nuts="2">District de Darmstadt</region><settlement type="city">Darmstadt</settlement></placeName></affiliation></author><author><name sortKey="Kleebe, Hans Joachim" uniqKey="Kleebe H">Hans-Joachim Kleebe</name><affiliation wicri:level="3"><inist:fA14 i1="01"><s1>Technische Universität Darmstadt, Fachbereich Material- und Geowissenschaften, Petersenstr. 23</s1><s2>64287 Darmstadt</s2><s3>DEU</s3><sZ>1 aut.</sZ><sZ>2 aut.</sZ><sZ>3 aut.</sZ><sZ>4 aut.</sZ></inist:fA14><country>Allemagne</country><placeName><region type="land" nuts="1">Hesse (Land)</region><region type="district" nuts="2">District de Darmstadt</region><settlement type="city">Darmstadt</settlement></placeName></affiliation></author><author><name sortKey="Gurlo, Aleksander" uniqKey="Gurlo A">Aleksander Gurlo</name><affiliation wicri:level="3"><inist:fA14 i1="01"><s1>Technische Universität Darmstadt, Fachbereich Material- und Geowissenschaften, Petersenstr. 23</s1><s2>64287 Darmstadt</s2><s3>DEU</s3><sZ>1 aut.</sZ><sZ>2 aut.</sZ><sZ>3 aut.</sZ><sZ>4 aut.</sZ></inist:fA14><country>Allemagne</country><placeName><region type="land" nuts="1">Hesse (Land)</region><region type="district" nuts="2">District de Darmstadt</region><settlement type="city">Darmstadt</settlement></placeName></affiliation></author></titleStmt><publicationStmt><idno type="inist">13-0133960</idno><date when="2013">2013</date><idno type="stanalyst">PASCAL 13-0133960 INIST</idno><idno type="RBID">Pascal:13-0133960</idno><idno type="wicri:Area/Main/Corpus">001023</idno><idno type="wicri:Area/Main/Repository">000A77</idno></publicationStmt><seriesStmt><idno type="ISSN">0022-4596</idno><title level="j" type="abbreviated">J. solid state chem. : (Print)</title><title level="j" type="main">Journal of solid state chemistry : (Print)</title></seriesStmt></fileDesc><profileDesc><textClass><keywords scheme="KwdEn" xml:lang="en"><term>Atomic displacements</term><term>Bixbyite</term><term>Case study</term><term>Crystal morphology</term><term>Crystal orientation</term><term>Crystallization</term><term>Dangling bonds</term><term>Electron beams</term><term>Electron irradiation</term><term>Fourier transformation</term><term>Growth mechanism</term><term>Growth rate</term><term>High resolution electron microscopy</term><term>Indium hydroxide</term><term>Indium oxide</term><term>Induction</term><term>Kinetics</term><term>Monocrystals</term><term>Nanocrystal</term><term>Nanostructured materials</term><term>Nucleation</term><term>Phase transformations</term><term>Radiation effects</term><term>Rate constant</term><term>Reaction mechanism</term><term>SAED</term><term>Shrinkage</term><term>Spatial resolution</term><term>Texture</term><term>Time resolution</term><term>Time resolved spectra</term><term>Transmission electron microscopy</term><term>Volume fraction</term></keywords><keywords scheme="Pascal" xml:lang="fr"><term>Oxyde d'indium</term><term>Hydroxyde d'indium</term><term>Nanocristal</term><term>Nanomatériau</term><term>Microscopie électronique transmission</term><term>Microscopie électronique haute résolution</term><term>Résolution spatiale</term><term>Etude cas</term><term>Faisceau électron</term><term>Morphologie cristalline</term><term>Effet rayonnement</term><term>Irradiation électron</term><term>Résolution temporelle</term><term>Spectre résolution temporelle</term><term>Monocristal</term><term>Orientation cristalline</term><term>Cinétique</term><term>Cristallisation</term><term>Diffraction électron sélection aire</term><term>Texture</term><term>Induction</term><term>Transformation Fourier</term><term>Fraction volumique</term><term>Transformation phase</term><term>Retrait</term><term>Mécanisme réaction</term><term>Nucléation</term><term>Mécanisme croissance</term><term>Constante vitesse</term><term>Taux croissance</term><term>Déplacement atomique</term><term>Liaison disponible</term><term>Substrat indium</term><term>In2O3</term><term>In</term><term>8107</term><term>6180F</term><term>6470K</term><term>8130H</term><term>Bixbyite</term></keywords></textClass></profileDesc></teiHeader><front><div type="abstract" xml:lang="en">The high-resolution transmission electron microscopy (HR-TEM) is used to study, in situ, spatially resolved decomposition in individual nanocrystals of metal hydroxides and oxyhydroxides. This case study reports on the decomposition of indium hydroxide (c-In(OH)<sub>3</sub>) to bixbyite-type indium oxide (c-In<sub>2</sub>O<sub>3</sub>). The electron beam is focused onto a single cube-shaped In(OH)<sub>3</sub> crystal of {100} morphology with ca. 35 nm edge length and a sequence of HR-TEM images was recorded during electron beam irradiation. The frame-by-frame analysis of video sequences allows for the in situ, time-resolved observation of the shape and orientation of the transformed crystals, which in turn enables the evaluation of the kinetics of c-In<sub>2</sub>O<sub>3</sub> crystallization. Supplementary material (video of the transformation) related to this article can be found online at http://dx.doi.org/10,1016/j.jssc.2012.09.022. After irradiation the shape of the parent cube-shaped crystal is preserved, however, its linear dimension (edge) is reduced by the factor 1.20. The corresponding spotted selected area electron diffraction (SAED) pattern representing zone [001] of c-In(OH)<sub>3</sub> is transformed to a diffuse strongly textured ring-like pattern of c-In<sub>2</sub>O<sub>3</sub> that indicates the transformed cube is no longer a single crystal but is disintegrated into individual c-In<sub>2</sub>O<sub>3</sub> domains with the size of about 5-10 nm. The induction time of approximately 15 s is estimated from the time-resolved Fourier transforms. The volume fraction of the transformed phase (c-In<sub>2</sub>O<sub>3</sub>), calculated from the shrinkage of the parent c-In(OH)<sub>3</sub> crystal in the recorded HR-TEM images, is used as a measure of the kinetics of c-In<sub>2</sub>O<sub>3</sub> crystallization within the framework of Avrami-Erofeev formalism. The Avrami exponent of ∼3 is characteristic for a reaction mechanism with fast nucleation at the beginning of the reaction and subsequent three-dimensional growth of nuclei with a constant growth rate. The structural transformation path in reconstructive decomposition of c-In(OH)<sub>3</sub> to c-In<sub>2</sub>O<sub>3</sub> is discussed in terms of (i) the displacement of hydrogen atoms that lead to breaking the hydrogen bond between OH groups of [In(OH)<sub>6</sub>] octahedra and finally to their destabilization and (ii) transformation of the vertices-shared indium-oxygen octahedra in c-In(OH)<sub>3</sub> to vertices- and edge-shared octahedra in c-In<sub>2</sub>O<sub>3</sub>.</div></front></TEI><inist><standard h6="B"><pA><fA01 i1="01" i2="1"><s0>0022-4596</s0></fA01><fA02 i1="01"><s0>JSSCBI</s0></fA02><fA03 i2="1"><s0>J. solid state chem. : (Print)</s0></fA03><fA05><s2>198</s2></fA05><fA08 i1="01" i2="1" l="ENG"><s1>Indium hydroxide to oxide decomposition observed in one nanocrystal during in situ transmission electron microscopy studies</s1></fA08><fA11 i1="01" i2="1"><s1>MIEHE (Gerhard)</s1></fA11><fA11 i1="02" i2="1"><s1>LAUTERBACH (Stefan)</s1></fA11><fA11 i1="03" i2="1"><s1>KLEEBE (Hans-Joachim)</s1></fA11><fA11 i1="04" i2="1"><s1>GURLO (Aleksander)</s1></fA11><fA14 i1="01"><s1>Technische Universität Darmstadt, Fachbereich Material- und Geowissenschaften, Petersenstr. 23</s1><s2>64287 Darmstadt</s2><s3>DEU</s3><sZ>1 aut.</sZ><sZ>2 aut.</sZ><sZ>3 aut.</sZ><sZ>4 aut.</sZ></fA14><fA20><s1>364-370</s1></fA20><fA21><s1>2013</s1></fA21><fA23 i1="01"><s0>ENG</s0></fA23><fA43 i1="01"><s1>INIST</s1><s2>14677</s2><s5>354000503720600530</s5></fA43><fA44><s0>0000</s0><s1>© 2013 INIST-CNRS. All rights reserved.</s1></fA44><fA45><s0>30 ref.</s0></fA45><fA47 i1="01" i2="1"><s0>13-0133960</s0></fA47><fA60><s1>P</s1></fA60><fA61><s0>A</s0></fA61><fA64 i1="01" i2="1"><s0>Journal of solid state chemistry : (Print)</s0></fA64><fA66 i1="01"><s0>NLD</s0></fA66><fC01 i1="01" l="ENG"><s0>The high-resolution transmission electron microscopy (HR-TEM) is used to study, in situ, spatially resolved decomposition in individual nanocrystals of metal hydroxides and oxyhydroxides. This case study reports on the decomposition of indium hydroxide (c-In(OH)<sub>3</sub>) to bixbyite-type indium oxide (c-In<sub>2</sub>O<sub>3</sub>). The electron beam is focused onto a single cube-shaped In(OH)<sub>3</sub> crystal of {100} morphology with ca. 35 nm edge length and a sequence of HR-TEM images was recorded during electron beam irradiation. The frame-by-frame analysis of video sequences allows for the in situ, time-resolved observation of the shape and orientation of the transformed crystals, which in turn enables the evaluation of the kinetics of c-In<sub>2</sub>O<sub>3</sub> crystallization. Supplementary material (video of the transformation) related to this article can be found online at http://dx.doi.org/10,1016/j.jssc.2012.09.022. After irradiation the shape of the parent cube-shaped crystal is preserved, however, its linear dimension (edge) is reduced by the factor 1.20. The corresponding spotted selected area electron diffraction (SAED) pattern representing zone [001] of c-In(OH)<sub>3</sub> is transformed to a diffuse strongly textured ring-like pattern of c-In<sub>2</sub>O<sub>3</sub> that indicates the transformed cube is no longer a single crystal but is disintegrated into individual c-In<sub>2</sub>O<sub>3</sub> domains with the size of about 5-10 nm. The induction time of approximately 15 s is estimated from the time-resolved Fourier transforms. The volume fraction of the transformed phase (c-In<sub>2</sub>O<sub>3</sub>), calculated from the shrinkage of the parent c-In(OH)<sub>3</sub> crystal in the recorded HR-TEM images, is used as a measure of the kinetics of c-In<sub>2</sub>O<sub>3</sub> crystallization within the framework of Avrami-Erofeev formalism. The Avrami exponent of ∼3 is characteristic for a reaction mechanism with fast nucleation at the beginning of the reaction and subsequent three-dimensional growth of nuclei with a constant growth rate. The structural transformation path in reconstructive decomposition of c-In(OH)<sub>3</sub> to c-In<sub>2</sub>O<sub>3</sub> is discussed in terms of (i) the displacement of hydrogen atoms that lead to breaking the hydrogen bond between OH groups of [In(OH)<sub>6</sub>] octahedra and finally to their destabilization and (ii) transformation of the vertices-shared indium-oxygen octahedra in c-In(OH)<sub>3</sub> to vertices- and edge-shared octahedra in c-In<sub>2</sub>O<sub>3</sub>.</s0></fC01><fC02 i1="01" i2="3"><s0>001B80A07Z</s0></fC02><fC02 i1="02" i2="3"><s0>001B60A80F</s0></fC02><fC02 i1="03" i2="3"><s0>001B60D70K</s0></fC02><fC02 i1="04" i2="3"><s0>001B80A30H</s0></fC02><fC03 i1="01" i2="X" l="FRE"><s0>Oxyde d'indium</s0><s5>01</s5></fC03><fC03 i1="01" i2="X" l="ENG"><s0>Indium oxide</s0><s5>01</s5></fC03><fC03 i1="01" i2="X" l="SPA"><s0>Indio óxido</s0><s5>01</s5></fC03><fC03 i1="02" i2="X" l="FRE"><s0>Hydroxyde d'indium</s0><s5>02</s5></fC03><fC03 i1="02" i2="X" 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l="ENG"><s0>SAED</s0><s5>32</s5></fC03><fC03 i1="20" i2="3" l="FRE"><s0>Texture</s0><s5>33</s5></fC03><fC03 i1="20" i2="3" l="ENG"><s0>Texture</s0><s5>33</s5></fC03><fC03 i1="21" i2="3" l="FRE"><s0>Induction</s0><s5>34</s5></fC03><fC03 i1="21" i2="3" l="ENG"><s0>Induction</s0><s5>34</s5></fC03><fC03 i1="22" i2="3" l="FRE"><s0>Transformation Fourier</s0><s5>35</s5></fC03><fC03 i1="22" i2="3" l="ENG"><s0>Fourier transformation</s0><s5>35</s5></fC03><fC03 i1="23" i2="X" l="FRE"><s0>Fraction volumique</s0><s5>36</s5></fC03><fC03 i1="23" i2="X" l="ENG"><s0>Volume fraction</s0><s5>36</s5></fC03><fC03 i1="23" i2="X" l="SPA"><s0>Fracción volumétrica</s0><s5>36</s5></fC03><fC03 i1="24" i2="3" l="FRE"><s0>Transformation phase</s0><s5>37</s5></fC03><fC03 i1="24" i2="3" l="ENG"><s0>Phase transformations</s0><s5>37</s5></fC03><fC03 i1="25" i2="3" l="FRE"><s0>Retrait</s0><s5>38</s5></fC03><fC03 i1="25" i2="3" l="ENG"><s0>Shrinkage</s0><s5>38</s5></fC03><fC03 i1="26" i2="X" l="FRE"><s0>Mécanisme réaction</s0><s5>39</s5></fC03><fC03 i1="26" i2="X" l="ENG"><s0>Reaction mechanism</s0><s5>39</s5></fC03><fC03 i1="26" i2="X" l="SPA"><s0>Mecanismo reacción</s0><s5>39</s5></fC03><fC03 i1="27" i2="3" l="FRE"><s0>Nucléation</s0><s5>40</s5></fC03><fC03 i1="27" i2="3" l="ENG"><s0>Nucleation</s0><s5>40</s5></fC03><fC03 i1="28" i2="X" l="FRE"><s0>Mécanisme croissance</s0><s5>41</s5></fC03><fC03 i1="28" i2="X" l="ENG"><s0>Growth mechanism</s0><s5>41</s5></fC03><fC03 i1="28" i2="X" l="SPA"><s0>Mecanismo crecimiento</s0><s5>41</s5></fC03><fC03 i1="29" i2="X" l="FRE"><s0>Constante vitesse</s0><s5>42</s5></fC03><fC03 i1="29" i2="X" l="ENG"><s0>Rate constant</s0><s5>42</s5></fC03><fC03 i1="29" i2="X" l="SPA"><s0>Constante velocidad</s0><s5>42</s5></fC03><fC03 i1="30" i2="3" l="FRE"><s0>Taux croissance</s0><s5>43</s5></fC03><fC03 i1="30" i2="3" l="ENG"><s0>Growth rate</s0><s5>43</s5></fC03><fC03 i1="31" i2="3" l="FRE"><s0>Déplacement atomique</s0><s5>44</s5></fC03><fC03 i1="31" i2="3" l="ENG"><s0>Atomic displacements</s0><s5>44</s5></fC03><fC03 i1="32" i2="3" l="FRE"><s0>Liaison disponible</s0><s5>45</s5></fC03><fC03 i1="32" i2="3" l="ENG"><s0>Dangling bonds</s0><s5>45</s5></fC03><fC03 i1="33" i2="3" l="FRE"><s0>Substrat indium</s0><s4>INC</s4><s5>46</s5></fC03><fC03 i1="34" i2="3" l="FRE"><s0>In2O3</s0><s4>INC</s4><s5>47</s5></fC03><fC03 i1="35" i2="3" l="FRE"><s0>In</s0><s4>INC</s4><s5>48</s5></fC03><fC03 i1="36" i2="3" l="FRE"><s0>8107</s0><s4>INC</s4><s5>71</s5></fC03><fC03 i1="37" i2="3" l="FRE"><s0>6180F</s0><s4>INC</s4><s5>72</s5></fC03><fC03 i1="38" i2="3" l="FRE"><s0>6470K</s0><s4>INC</s4><s5>73</s5></fC03><fC03 i1="39" i2="3" l="FRE"><s0>8130H</s0><s4>INC</s4><s5>74</s5></fC03><fC03 i1="40" i2="3" l="FRE"><s0>Bixbyite</s0><s4>CD</s4><s5>96</s5></fC03><fC03 i1="40" i2="3" l="ENG"><s0>Bixbyite</s0><s4>CD</s4><s5>96</s5></fC03><fC03 i1="40" i2="3" l="SPA"><s0>Bixbyita</s0><s4>CD</s4><s5>96</s5></fC03><fN21><s1>105</s1></fN21><fN44 i1="01"><s1>OTO</s1></fN44><fN82><s1>OTO</s1></fN82></pA></standard></inist></record>Pour manipuler ce document sous Unix (Dilib)
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