Nanocrystalline anatase derived from modified alkoxide mesostructured gel
A sol prepared by chelation of titanium n -butoxide with ethyl acetoacetate (1:1) was slowly hydrolyzed, and the obtained gel was thermally treated in order to produce anatase. Samples were investigated by means of FTIR, XRD, DTA/TG, N 2 adsorption–desorption isotherms, FESEM and HRTEM. It was deter...
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| Veröffentlicht in: | Journal of thermal analysis and calorimetry 2016-05, Vol.124 (2), p.645-655 |
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| creator | Kurajica, S. Minga, I. Mandić, V. Matijašić, G. |
| description | A sol prepared by chelation of titanium
n
-butoxide with ethyl acetoacetate (1:1) was slowly hydrolyzed, and the obtained gel was thermally treated in order to produce anatase. Samples were investigated by means of FTIR, XRD, DTA/TG, N
2
adsorption–desorption isotherms, FESEM and HRTEM. It was determined the modified alkoxide is partially hydrolyzed, leaving small amount of butoxide and ethyl acetoacetate groups attached to titanium. XRD pattern and HRTEM micrograph revealed gel ordering at the mesostructure scale. Observed mesostructure was found to be consisted with inorganic–organic nanoclusters, exhibiting some polydispersity in the size and variations in composition. Thermal decomposition exhibits evaporation of water and butanol, elimination of ethyl acetoacetate and butoxy groups, carbonate removal, anatase crystallization and transformation to rutile, accompanied with oxidation of carbonaceous species. After 2 h at 350 °C pure nanocrystalline anatase crystallites were obtained having average crystallite size of 16.4 nm with majority of exposed {101} facets. |
| doi_str_mv | 10.1007/s10973-015-5188-6 |
| format | Article |
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n
-butoxide with ethyl acetoacetate (1:1) was slowly hydrolyzed, and the obtained gel was thermally treated in order to produce anatase. Samples were investigated by means of FTIR, XRD, DTA/TG, N
2
adsorption–desorption isotherms, FESEM and HRTEM. It was determined the modified alkoxide is partially hydrolyzed, leaving small amount of butoxide and ethyl acetoacetate groups attached to titanium. XRD pattern and HRTEM micrograph revealed gel ordering at the mesostructure scale. Observed mesostructure was found to be consisted with inorganic–organic nanoclusters, exhibiting some polydispersity in the size and variations in composition. Thermal decomposition exhibits evaporation of water and butanol, elimination of ethyl acetoacetate and butoxy groups, carbonate removal, anatase crystallization and transformation to rutile, accompanied with oxidation of carbonaceous species. After 2 h at 350 °C pure nanocrystalline anatase crystallites were obtained having average crystallite size of 16.4 nm with majority of exposed {101} facets.</description><identifier>ISSN: 1388-6150</identifier><identifier>EISSN: 1588-2926</identifier><identifier>EISSN: 1572-8943</identifier><identifier>DOI: 10.1007/s10973-015-5188-6</identifier><language>eng</language><publisher>Dordrecht: Springer Netherlands</publisher><subject>Adsorption ; Alkoxides ; Analytical Chemistry ; Anatase ; Calorimetry ; Carbonates ; Chelation ; Chemistry ; Chemistry and Materials Science ; Crystallites ; Inorganic Chemistry ; Measurement Science and Instrumentation ; Nanocrystals ; Nanostructure ; Physical Chemistry ; Polymer Sciences ; Titanium</subject><ispartof>Journal of thermal analysis and calorimetry, 2016-05, Vol.124 (2), p.645-655</ispartof><rights>Akadémiai Kiadó, Budapest, Hungary 2015</rights><rights>COPYRIGHT 2016 Springer</rights><lds50>peer_reviewed</lds50><woscitedreferencessubscribed>false</woscitedreferencessubscribed><citedby>FETCH-LOGICAL-c431t-c2dcad4a0fdc53baadca06d51c6cf62778d0207b1c0b3f9a7e909171f440641a3</citedby><cites>FETCH-LOGICAL-c431t-c2dcad4a0fdc53baadca06d51c6cf62778d0207b1c0b3f9a7e909171f440641a3</cites></display><links><openurl>$$Topenurl_article</openurl><openurlfulltext>$$Topenurlfull_article</openurlfulltext><thumbnail>$$Tsyndetics_thumb_exl</thumbnail><linktopdf>$$Uhttps://link.springer.com/content/pdf/10.1007/s10973-015-5188-6$$EPDF$$P50$$Gspringer$$H</linktopdf><linktohtml>$$Uhttps://link.springer.com/10.1007/s10973-015-5188-6$$EHTML$$P50$$Gspringer$$H</linktohtml><link.rule.ids>314,780,784,27924,27925,41488,42557,51319</link.rule.ids></links><search><creatorcontrib>Kurajica, S.</creatorcontrib><creatorcontrib>Minga, I.</creatorcontrib><creatorcontrib>Mandić, V.</creatorcontrib><creatorcontrib>Matijašić, G.</creatorcontrib><title>Nanocrystalline anatase derived from modified alkoxide mesostructured gel</title><title>Journal of thermal analysis and calorimetry</title><addtitle>J Therm Anal Calorim</addtitle><description>A sol prepared by chelation of titanium
n
-butoxide with ethyl acetoacetate (1:1) was slowly hydrolyzed, and the obtained gel was thermally treated in order to produce anatase. Samples were investigated by means of FTIR, XRD, DTA/TG, N
2
adsorption–desorption isotherms, FESEM and HRTEM. It was determined the modified alkoxide is partially hydrolyzed, leaving small amount of butoxide and ethyl acetoacetate groups attached to titanium. XRD pattern and HRTEM micrograph revealed gel ordering at the mesostructure scale. Observed mesostructure was found to be consisted with inorganic–organic nanoclusters, exhibiting some polydispersity in the size and variations in composition. Thermal decomposition exhibits evaporation of water and butanol, elimination of ethyl acetoacetate and butoxy groups, carbonate removal, anatase crystallization and transformation to rutile, accompanied with oxidation of carbonaceous species. After 2 h at 350 °C pure nanocrystalline anatase crystallites were obtained having average crystallite size of 16.4 nm with majority of exposed {101} facets.</description><subject>Adsorption</subject><subject>Alkoxides</subject><subject>Analytical Chemistry</subject><subject>Anatase</subject><subject>Calorimetry</subject><subject>Carbonates</subject><subject>Chelation</subject><subject>Chemistry</subject><subject>Chemistry and Materials Science</subject><subject>Crystallites</subject><subject>Inorganic Chemistry</subject><subject>Measurement Science and Instrumentation</subject><subject>Nanocrystals</subject><subject>Nanostructure</subject><subject>Physical Chemistry</subject><subject>Polymer Sciences</subject><subject>Titanium</subject><issn>1388-6150</issn><issn>1588-2926</issn><issn>1572-8943</issn><fulltext>true</fulltext><rsrctype>article</rsrctype><creationdate>2016</creationdate><recordtype>article</recordtype><recordid>eNp9kc1O3TAQRiPUSlDKA7DLsl2EzjhxnCwRaumVEEj9WVtz7fGVaRJT26ng7eurdMOm8sIzn87xwl9VXSJcIYD6lBBG1TaAspE4DE1_Up2hLIMYRf-mzO0xRAmn1buUHgFgHAHPqt09LcHEl5RpmvzCNS2UKXFtOfo_bGsXw1zPwXrny0bTr_DsLdczp5ByXE1eY8kPPL2v3jqaEl_8u8-rn18-_7j52tw93O5uru8a07WYGyOsIdsROGtkuycqK_RWoumN64VSgwUBao8G9q0bSfEIIyp0XQd9h9SeVx-2d59i-L1yynr2yfA00cJhTRoHIWWrWikKerWhB5pY-8WFHMmUY3n2JizsfMmvu24QQz8qKMLHV0JhMj_nA60p6d33b69Z3FgTQ0qRnX6Kfqb4ohH0sRO9daJLJ_rYie6LIzYnFXY5cNSPYY1L-a7_SH8BFu2PEw</recordid><startdate>20160501</startdate><enddate>20160501</enddate><creator>Kurajica, S.</creator><creator>Minga, I.</creator><creator>Mandić, V.</creator><creator>Matijašić, G.</creator><general>Springer Netherlands</general><general>Springer</general><scope>AAYXX</scope><scope>CITATION</scope><scope>ISR</scope><scope>7SR</scope><scope>7U5</scope><scope>8BQ</scope><scope>8FD</scope><scope>JG9</scope><scope>L7M</scope></search><sort><creationdate>20160501</creationdate><title>Nanocrystalline anatase derived from modified alkoxide mesostructured gel</title><author>Kurajica, S. ; Minga, I. ; Mandić, V. ; Matijašić, G.</author></sort><facets><frbrtype>5</frbrtype><frbrgroupid>cdi_FETCH-LOGICAL-c431t-c2dcad4a0fdc53baadca06d51c6cf62778d0207b1c0b3f9a7e909171f440641a3</frbrgroupid><rsrctype>articles</rsrctype><prefilter>articles</prefilter><language>eng</language><creationdate>2016</creationdate><topic>Adsorption</topic><topic>Alkoxides</topic><topic>Analytical Chemistry</topic><topic>Anatase</topic><topic>Calorimetry</topic><topic>Carbonates</topic><topic>Chelation</topic><topic>Chemistry</topic><topic>Chemistry and Materials Science</topic><topic>Crystallites</topic><topic>Inorganic Chemistry</topic><topic>Measurement Science and Instrumentation</topic><topic>Nanocrystals</topic><topic>Nanostructure</topic><topic>Physical Chemistry</topic><topic>Polymer Sciences</topic><topic>Titanium</topic><toplevel>peer_reviewed</toplevel><toplevel>online_resources</toplevel><creatorcontrib>Kurajica, S.</creatorcontrib><creatorcontrib>Minga, I.</creatorcontrib><creatorcontrib>Mandić, V.</creatorcontrib><creatorcontrib>Matijašić, G.</creatorcontrib><collection>CrossRef</collection><collection>Gale In Context: Science</collection><collection>Engineered Materials Abstracts</collection><collection>Solid State and Superconductivity Abstracts</collection><collection>METADEX</collection><collection>Technology Research Database</collection><collection>Materials Research Database</collection><collection>Advanced Technologies Database with Aerospace</collection><jtitle>Journal of thermal analysis and calorimetry</jtitle></facets><delivery><delcategory>Remote Search Resource</delcategory><fulltext>fulltext</fulltext></delivery><addata><au>Kurajica, S.</au><au>Minga, I.</au><au>Mandić, V.</au><au>Matijašić, G.</au><format>journal</format><genre>article</genre><ristype>JOUR</ristype><atitle>Nanocrystalline anatase derived from modified alkoxide mesostructured gel</atitle><jtitle>Journal of thermal analysis and calorimetry</jtitle><stitle>J Therm Anal Calorim</stitle><date>2016-05-01</date><risdate>2016</risdate><volume>124</volume><issue>2</issue><spage>645</spage><epage>655</epage><pages>645-655</pages><issn>1388-6150</issn><eissn>1588-2926</eissn><eissn>1572-8943</eissn><abstract>A sol prepared by chelation of titanium
n
-butoxide with ethyl acetoacetate (1:1) was slowly hydrolyzed, and the obtained gel was thermally treated in order to produce anatase. Samples were investigated by means of FTIR, XRD, DTA/TG, N
2
adsorption–desorption isotherms, FESEM and HRTEM. It was determined the modified alkoxide is partially hydrolyzed, leaving small amount of butoxide and ethyl acetoacetate groups attached to titanium. XRD pattern and HRTEM micrograph revealed gel ordering at the mesostructure scale. Observed mesostructure was found to be consisted with inorganic–organic nanoclusters, exhibiting some polydispersity in the size and variations in composition. Thermal decomposition exhibits evaporation of water and butanol, elimination of ethyl acetoacetate and butoxy groups, carbonate removal, anatase crystallization and transformation to rutile, accompanied with oxidation of carbonaceous species. After 2 h at 350 °C pure nanocrystalline anatase crystallites were obtained having average crystallite size of 16.4 nm with majority of exposed {101} facets.</abstract><cop>Dordrecht</cop><pub>Springer Netherlands</pub><doi>10.1007/s10973-015-5188-6</doi><tpages>11</tpages></addata></record> |
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| subjects | Adsorption Alkoxides Analytical Chemistry Anatase Calorimetry Carbonates Chelation Chemistry Chemistry and Materials Science Crystallites Inorganic Chemistry Measurement Science and Instrumentation Nanocrystals Nanostructure Physical Chemistry Polymer Sciences Titanium |
| title | Nanocrystalline anatase derived from modified alkoxide mesostructured gel |
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