{"id":{"repo_id":"uiuc","oai_identifier":"oai:www.ideals.illinois.edu:2142/70388"},"canonical_url":"https://search.dev.ndltd.org/etd/uiuc/oai:www.ideals.illinois.edu:2142/70388","repository":{"repo_id":"uiuc","name":"University of Illinois - Urbana-Champaign","base_url":"https://www.ideals.illinois.edu/oai-pmh"},"display":{"title":"Multinuclear NMR Investigations of Sol-Gel Systems","abstract":"The inorganic polymeric materials known as oxide glasses are normally prepared by the fusion of refractory oxides, followed by rapid cooling to avoid devitrification. A topic of current interest in materials research is the preparation of oxide glasses by the hydrolysis and polymerization of metal alkoxides in solution to form a gel, which may then be fired to form a glass. This so-called sol-gel process represents the synthesis of an inorganic polymer in a manner analogous to that in which organic polymers have traditionally been prepared.","abstract_html":"The inorganic polymeric materials known as oxide glasses are normally prepared by the fusion of refractory oxides, followed by rapid cooling to avoid devitrification. A topic of current interest in materials research is the preparation of oxide glasses by the hydrolysis and polymerization of metal alkoxides in solution to form a gel, which may then be fired to form a glass. This so-called sol-gel process represents the synthesis of an inorganic polymer in a manner analogous to that in which organic polymers have traditionally been prepared.","abstract_has_math":false,"creators":["Irwin, Alan Dale"],"institution":"University of Illinois at Urbana-Champaign","degree_name":"Ph.D.","degree_level":"Dissertation","degree_discipline":"Chemistry","degree_department":null,"school":null,"contributors":["Jonas, Jiri"],"advisors":[],"committee_chairs":[],"committee_members":[],"year":2014,"date_issued":"2014-12-15T23:19:06Z","date_published":"2014-12-15T23:19:06Z","updated_at":"2026-07-22T22:26:02Z","subjects":["Chemistry, Analytical"],"languages":[],"rights":[],"rights_urls":[],"identifier_entries":[{"key":"dc:identifier","label":"Identifier","values":["(UMI)AAI8803078"],"render_values":[{"text":"(UMI)AAI8803078","href":null,"code":true}]}]},"links":{"outbound_url":"http://hdl.handle.net/2142/70388","outbound_label":"Handle","outbound_source":"dc:identifier"},"metadata_groups":[{"id":"people","label":"People","entries":[{"key":"dc:contributor","label":"Contributor","values":["Jonas, Jiri"]},{"key":"dc:creator","label":"Author","values":["Irwin, Alan Dale"]}]},{"id":"academic_context","label":"Academic Context","entries":[{"key":"dc:date","label":"Dc Date","values":["2014-12-15T23:19:06Z","10000-01-01","1987"]},{"key":"dc:type","label":"Dc Type","values":["text"]},{"key":"thesis:degree_discipline","label":"Discipline","values":["Chemistry"]},{"key":"thesis:degree_level","label":"Degree Level","values":["Dissertation"]},{"key":"thesis:degree_name","label":"Degree Name","values":["Ph.D."]},{"key":"thesis:institution_name","label":"Thesis Institution Name","values":["University of Illinois at Urbana-Champaign"]}]},{"id":"subjects_keywords","label":"Subjects and Keywords","entries":[{"key":"dc:subject","label":"Dc Subject","values":["Chemistry, Analytical"]}]},{"id":"identifiers","label":"Identifiers","entries":[{"key":"dc:identifier","label":"Identifier","values":["http://hdl.handle.net/2142/70388","(UMI)AAI8803078"]}]},{"id":"additional","label":"Additional Metadata","entries":[{"key":"dc:description","label":"Description","values":["The inorganic polymeric materials known as oxide glasses are normally prepared by the fusion of refractory oxides, followed by rapid cooling to avoid devitrification. A topic of current interest in materials research is the preparation of oxide glasses by the hydrolysis and polymerization of metal alkoxides in solution to form a gel, which may then be fired to form a glass. This so-called sol-gel process represents the synthesis of an inorganic polymer in a manner analogous to that in which organic polymers have traditionally been prepared.","Much work has been and continues to be done toward preparing specific materials by the sol-gel process, and toward determining the physical characteristics of sol-gel derived materials. However, there remains a great need for basic understanding of the chemistry involved. The effects of processing variables such as starting reagents, temperature, pressure, pH, etc. cannot be optimally controlled or exploited without a knowledge of the chemistry of polymer-forming metal alkoxide systems.","Recent advances in instrumentation and methods have made pulse Fourier transform nuclear magnetic resonance (NMR) spectroscopy a powerful technique for studying the chemistry of inorganic oxide systems in both the liquid and solid states. This thesis describes the application of these NMR techniques to the sol-gel systems SiO$\\sb2$, B$\\sb2$O$\\sb3$-SiO$\\sb2$, Al$\\sb2$O$\\sb3$-SiO$\\sb2$ and Na$\\sb2$O-Al$\\sb2$O$\\sb3$-SiO$\\sb2$.","It is demonstrated that in the borosilicate system, borosiloxane bonds do not result from co-polymerization in the sol; rather they are formed during heat treatment above 150$\\sp\\circ$C, after water has been driven out. The degree of cross-linking in SiO$\\sb2$ gels prepared under different catalytic conditions is monitored during heat treatment. While the initial gels vary greatly in their degree of cross-linking, the products after heating to 800$\\sp\\circ$C are very similar. In aluminosilicate gels, aluminosiloxy bonds are formed by the time of gelation, the aluminum occupying tetrahedral (AlO$\\sb4$) $\\sp-$ sites which are charge balanced by octahedral cationic aluminum species. The addition of sodium as a counter ion enables the octahedral aluminum to convert to (AlO$\\sb4$) $\\sp-$. The aluminum environment is also shown to be dependent on the type of aluminum starting alkoxide employed.","Made available in DSpace on 2014-12-15T23:19:06Z (GMT). No. of bitstreams: 1 8803078.pdf: 2956024 bytes, checksum: a895c62e900fbd63174135b6a18598f6 (MD5) Previous issue date: 1987","Embargo set by: Seth Robbins for item 70554 Lift date: Forever Reason: Restricted to the U of I community idenfinitely during batch ingest of legacy ETDs","Restricted to the U of I community idenfinitely during batch ingest of legacy ETDs","U of I Only","102 p.","Thesis (Ph.D.)--University of Illinois at Urbana-Champaign, 1987."]},{"key":"dc:title","label":"Title","values":["Multinuclear NMR Investigations of Sol-Gel Systems"]}]}],"canonical_facts":{"dc:contributor":["Jonas, Jiri"],"dc:creator":["Irwin, Alan Dale"],"dc:date":["2014-12-15T23:19:06Z","10000-01-01","1987"],"dc:description":["The inorganic polymeric materials known as oxide glasses are normally prepared by the fusion of refractory oxides, followed by rapid cooling to avoid devitrification. A topic of current interest in materials research is the preparation of oxide glasses by the hydrolysis and polymerization of metal alkoxides in solution to form a gel, which may then be fired to form a glass. This so-called sol-gel process represents the synthesis of an inorganic polymer in a manner analogous to that in which organic polymers have traditionally been prepared.","Much work has been and continues to be done toward preparing specific materials by the sol-gel process, and toward determining the physical characteristics of sol-gel derived materials. However, there remains a great need for basic understanding of the chemistry involved. The effects of processing variables such as starting reagents, temperature, pressure, pH, etc. cannot be optimally controlled or exploited without a knowledge of the chemistry of polymer-forming metal alkoxide systems.","Recent advances in instrumentation and methods have made pulse Fourier transform nuclear magnetic resonance (NMR) spectroscopy a powerful technique for studying the chemistry of inorganic oxide systems in both the liquid and solid states. This thesis describes the application of these NMR techniques to the sol-gel systems SiO$\\sb2$, B$\\sb2$O$\\sb3$-SiO$\\sb2$, Al$\\sb2$O$\\sb3$-SiO$\\sb2$ and Na$\\sb2$O-Al$\\sb2$O$\\sb3$-SiO$\\sb2$.","It is demonstrated that in the borosilicate system, borosiloxane bonds do not result from co-polymerization in the sol; rather they are formed during heat treatment above 150$\\sp\\circ$C, after water has been driven out. The degree of cross-linking in SiO$\\sb2$ gels prepared under different catalytic conditions is monitored during heat treatment. While the initial gels vary greatly in their degree of cross-linking, the products after heating to 800$\\sp\\circ$C are very similar. In aluminosilicate gels, aluminosiloxy bonds are formed by the time of gelation, the aluminum occupying tetrahedral (AlO$\\sb4$) $\\sp-$ sites which are charge balanced by octahedral cationic aluminum species. The addition of sodium as a counter ion enables the octahedral aluminum to convert to (AlO$\\sb4$) $\\sp-$. The aluminum environment is also shown to be dependent on the type of aluminum starting alkoxide employed.","Made available in DSpace on 2014-12-15T23:19:06Z (GMT). No. of bitstreams: 1 8803078.pdf: 2956024 bytes, checksum: a895c62e900fbd63174135b6a18598f6 (MD5) Previous issue date: 1987","Embargo set by: Seth Robbins for item 70554 Lift date: Forever Reason: Restricted to the U of I community idenfinitely during batch ingest of legacy ETDs","Restricted to the U of I community idenfinitely during batch ingest of legacy ETDs","U of I Only","102 p.","Thesis (Ph.D.)--University of Illinois at Urbana-Champaign, 1987."],"dc:identifier":["http://hdl.handle.net/2142/70388","(UMI)AAI8803078"],"dc:subject":["Chemistry, Analytical"],"dc:title":["Multinuclear NMR Investigations of Sol-Gel Systems"],"dc:type":["text"],"thesis:degree_discipline":["Chemistry"],"thesis:degree_level":["Dissertation"],"thesis:degree_name":["Ph.D."],"thesis:institution_name":["University of Illinois at Urbana-Champaign"]},"updated_at":"2026-07-22T22:26:02Z"}