Hybrid Organic−Inorganic Xerogel Access to Meso- and Microporous Silica by Thermal and Chemical Treatment
Hybrid xerogels of general formula (O)1,5Si−C⋮C−(CH2) n −C⋮C−Si(O)1,5 were prepared by sol−gel polycondensation in THF of the corresponding precursors (H3CO)3Si−C⋮C−(CH2) n −C⋮C−Si(OCH3)3, without catalyst. Treatment of the hybrid xerogels was with methanol and water in the presence of 2.0% of ammon...
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| Veröffentlicht in: | Chemistry of materials 1999-02, Vol.11 (2), p.281-291 |
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| creator | Boury, Bruno Chevalier, Pierre Corriu, Robert J. P Delord, Pierre Moreau, Joel J. E Chiman, Michel Wong |
| description | Hybrid xerogels of general formula (O)1,5Si−C⋮C−(CH2) n −C⋮C−Si(O)1,5 were prepared by sol−gel polycondensation in THF of the corresponding precursors (H3CO)3Si−C⋮C−(CH2) n −C⋮C−Si(OCH3)3, without catalyst. Treatment of the hybrid xerogels was with methanol and water in the presence of 2.0% of ammonium fluoride as catalyst. For 2 < n < 4, elimination of the organic spacer was quantitatively achieved and the organic spacer was recovered in high yield. For n = 5, 6, and 8, increasing the length of the spacer results in a decreasing efficiency of this chemical treatment. Thermal oxidation at 600−680 °C of the hybrid xerogels was also performed and elimination of the organic spacer was obtained in all the cases. Mesoporous silica with a narrow pore-size distribution was obtained by chemical treatment of the xerogel with n = 2−4. Microporous silica was obtained by thermal treatment of the xerogel at 680 °C. All the materials were characterized by SAXS, BET, and spectroscopy analysis. |
| doi_str_mv | 10.1021/cm980519i |
| format | Article |
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P ; Delord, Pierre ; Moreau, Joel J. E ; Chiman, Michel Wong</creator><creatorcontrib>Boury, Bruno ; Chevalier, Pierre ; Corriu, Robert J. P ; Delord, Pierre ; Moreau, Joel J. E ; Chiman, Michel Wong</creatorcontrib><description>Hybrid xerogels of general formula (O)1,5Si−C⋮C−(CH2) n −C⋮C−Si(O)1,5 were prepared by sol−gel polycondensation in THF of the corresponding precursors (H3CO)3Si−C⋮C−(CH2) n −C⋮C−Si(OCH3)3, without catalyst. Treatment of the hybrid xerogels was with methanol and water in the presence of 2.0% of ammonium fluoride as catalyst. For 2 < n < 4, elimination of the organic spacer was quantitatively achieved and the organic spacer was recovered in high yield. For n = 5, 6, and 8, increasing the length of the spacer results in a decreasing efficiency of this chemical treatment. Thermal oxidation at 600−680 °C of the hybrid xerogels was also performed and elimination of the organic spacer was obtained in all the cases. Mesoporous silica with a narrow pore-size distribution was obtained by chemical treatment of the xerogel with n = 2−4. Microporous silica was obtained by thermal treatment of the xerogel at 680 °C. All the materials were characterized by SAXS, BET, and spectroscopy analysis.</description><identifier>ISSN: 0897-4756</identifier><identifier>EISSN: 1520-5002</identifier><identifier>DOI: 10.1021/cm980519i</identifier><language>eng</language><publisher>Washington, DC: American Chemical Society</publisher><subject>Chemistry ; Colloidal gels. Colloidal sols ; Colloidal state and disperse state ; Exact sciences and technology ; General and physical chemistry</subject><ispartof>Chemistry of materials, 1999-02, Vol.11 (2), p.281-291</ispartof><rights>Copyright © 1999 American Chemical Society</rights><rights>1999 INIST-CNRS</rights><lds50>peer_reviewed</lds50><woscitedreferencessubscribed>false</woscitedreferencessubscribed><citedby>FETCH-LOGICAL-a390t-e2901abd713e19d40bbd95eee29c24ee68cac1969546c6b869a40a9410a2f3c43</citedby><cites>FETCH-LOGICAL-a390t-e2901abd713e19d40bbd95eee29c24ee68cac1969546c6b869a40a9410a2f3c43</cites></display><links><openurl>$$Topenurl_article</openurl><openurlfulltext>$$Topenurlfull_article</openurlfulltext><thumbnail>$$Tsyndetics_thumb_exl</thumbnail><linktopdf>$$Uhttps://pubs.acs.org/doi/pdf/10.1021/cm980519i$$EPDF$$P50$$Gacs$$H</linktopdf><linktohtml>$$Uhttps://pubs.acs.org/doi/10.1021/cm980519i$$EHTML$$P50$$Gacs$$H</linktohtml><link.rule.ids>314,780,784,2765,27076,27924,27925,56738,56788</link.rule.ids><backlink>$$Uhttp://pascal-francis.inist.fr/vibad/index.php?action=getRecordDetail&idt=1802350$$DView record in Pascal Francis$$Hfree_for_read</backlink></links><search><creatorcontrib>Boury, Bruno</creatorcontrib><creatorcontrib>Chevalier, Pierre</creatorcontrib><creatorcontrib>Corriu, Robert J. P</creatorcontrib><creatorcontrib>Delord, Pierre</creatorcontrib><creatorcontrib>Moreau, Joel J. E</creatorcontrib><creatorcontrib>Chiman, Michel Wong</creatorcontrib><title>Hybrid Organic−Inorganic Xerogel Access to Meso- and Microporous Silica by Thermal and Chemical Treatment</title><title>Chemistry of materials</title><addtitle>Chem. Mater</addtitle><description>Hybrid xerogels of general formula (O)1,5Si−C⋮C−(CH2) n −C⋮C−Si(O)1,5 were prepared by sol−gel polycondensation in THF of the corresponding precursors (H3CO)3Si−C⋮C−(CH2) n −C⋮C−Si(OCH3)3, without catalyst. Treatment of the hybrid xerogels was with methanol and water in the presence of 2.0% of ammonium fluoride as catalyst. For 2 < n < 4, elimination of the organic spacer was quantitatively achieved and the organic spacer was recovered in high yield. For n = 5, 6, and 8, increasing the length of the spacer results in a decreasing efficiency of this chemical treatment. Thermal oxidation at 600−680 °C of the hybrid xerogels was also performed and elimination of the organic spacer was obtained in all the cases. Mesoporous silica with a narrow pore-size distribution was obtained by chemical treatment of the xerogel with n = 2−4. Microporous silica was obtained by thermal treatment of the xerogel at 680 °C. All the materials were characterized by SAXS, BET, and spectroscopy analysis.</description><subject>Chemistry</subject><subject>Colloidal gels. Colloidal sols</subject><subject>Colloidal state and disperse state</subject><subject>Exact sciences and technology</subject><subject>General and physical chemistry</subject><issn>0897-4756</issn><issn>1520-5002</issn><fulltext>true</fulltext><rsrctype>article</rsrctype><creationdate>1999</creationdate><recordtype>article</recordtype><recordid>eNptkEtOAzEMhiMEEuWx4AZZwILFgDPvLKsKKNACEkViF3kybgmdR5UMEr0Ba47ISQgMgg0rW_Zn-_fP2IGAEwGhONW1zCER0mywgUhCCBKAcJMNIJdZEGdJus12nHsGEB7PB2w5XhfWlPzWLrAx-uPt_bJp-5w_km0XVPGh1uQc71o-JdcGHJuST4227aq17Yvj96YyGnmx5rMnsjVW38ToiWpfrvjMEnY1Nd0e25pj5Wj_J-6yh_Oz2WgcTG4vLkfDSYCRhC6gUILAosxEREKWMRRFKRMiX9dhTJTmGrWQqUziVKdFnkqMAWUsAMN5pONolx33e71E5yzN1cqaGu1aCVBfLqlflzx72LMrdF7s3GKjjfsbyCGMEvBY0GPGdfT620a7VGkWZYma3d2rUXg1GYvrG5V6_qjnUTv13L7Yxj_8z_lPMpiDdQ</recordid><startdate>19990215</startdate><enddate>19990215</enddate><creator>Boury, Bruno</creator><creator>Chevalier, Pierre</creator><creator>Corriu, Robert J. 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Colloidal sols</topic><topic>Colloidal state and disperse state</topic><topic>Exact sciences and technology</topic><topic>General and physical chemistry</topic><toplevel>peer_reviewed</toplevel><toplevel>online_resources</toplevel><creatorcontrib>Boury, Bruno</creatorcontrib><creatorcontrib>Chevalier, Pierre</creatorcontrib><creatorcontrib>Corriu, Robert J. P</creatorcontrib><creatorcontrib>Delord, Pierre</creatorcontrib><creatorcontrib>Moreau, Joel J. E</creatorcontrib><creatorcontrib>Chiman, Michel Wong</creatorcontrib><collection>Istex</collection><collection>Pascal-Francis</collection><collection>CrossRef</collection><jtitle>Chemistry of materials</jtitle></facets><delivery><delcategory>Remote Search Resource</delcategory><fulltext>fulltext</fulltext></delivery><addata><au>Boury, Bruno</au><au>Chevalier, Pierre</au><au>Corriu, Robert J. P</au><au>Delord, Pierre</au><au>Moreau, Joel J. E</au><au>Chiman, Michel Wong</au><format>journal</format><genre>article</genre><ristype>JOUR</ristype><atitle>Hybrid Organic−Inorganic Xerogel Access to Meso- and Microporous Silica by Thermal and Chemical Treatment</atitle><jtitle>Chemistry of materials</jtitle><addtitle>Chem. Mater</addtitle><date>1999-02-15</date><risdate>1999</risdate><volume>11</volume><issue>2</issue><spage>281</spage><epage>291</epage><pages>281-291</pages><issn>0897-4756</issn><eissn>1520-5002</eissn><abstract>Hybrid xerogels of general formula (O)1,5Si−C⋮C−(CH2) n −C⋮C−Si(O)1,5 were prepared by sol−gel polycondensation in THF of the corresponding precursors (H3CO)3Si−C⋮C−(CH2) n −C⋮C−Si(OCH3)3, without catalyst. Treatment of the hybrid xerogels was with methanol and water in the presence of 2.0% of ammonium fluoride as catalyst. For 2 < n < 4, elimination of the organic spacer was quantitatively achieved and the organic spacer was recovered in high yield. For n = 5, 6, and 8, increasing the length of the spacer results in a decreasing efficiency of this chemical treatment. Thermal oxidation at 600−680 °C of the hybrid xerogels was also performed and elimination of the organic spacer was obtained in all the cases. Mesoporous silica with a narrow pore-size distribution was obtained by chemical treatment of the xerogel with n = 2−4. Microporous silica was obtained by thermal treatment of the xerogel at 680 °C. All the materials were characterized by SAXS, BET, and spectroscopy analysis.</abstract><cop>Washington, DC</cop><pub>American Chemical Society</pub><doi>10.1021/cm980519i</doi><tpages>11</tpages></addata></record> |
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| ispartof | Chemistry of materials, 1999-02, Vol.11 (2), p.281-291 |
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| language | eng |
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| source | ACS Publications |
| subjects | Chemistry Colloidal gels. Colloidal sols Colloidal state and disperse state Exact sciences and technology General and physical chemistry |
| title | Hybrid Organic−Inorganic Xerogel Access to Meso- and Microporous Silica by Thermal and Chemical Treatment |
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