Colloidal sol/gel processing of ultra-low expansion TiO2/SiO2 glasses

Zaide Deng, Else Breval, Carlo G. Pantano

Research output: Contribution to journalArticle

26 Citations (Scopus)

Abstract

A series of titania-silica glasses with 0-9% TiO2 were fabricated using a sol/gel process. The sol was prepared by dispersing colloidal silica fume in an aqueous solution of titania which was synthesized through the acid-catalyzed hydrolysis of titanium isopropoxide. The sols gelled in 2-4 days, and then were dried for 6-8 days. The dry gels were sintered at 1450-1500°C to produce clear, dense, microstructure-free glasses. The gels underwent a total shrinkage of ∼50% to yield glass rods about 50 mm long and 5 mm in diameter, or glass discs about 4 cm in diameter and 5 mm thick. The drying step was most critical in the production of crack-free specimens. In the gel, the transmission electron microscope (TEM) revealed the presence of 1-5 nm rutile microcrystallites uniformly distributed within a network of colloidal silica particles. After sintering to 1450-1500°C, though, a dense, transparent, microstructure-free glass was created. Fourier transform infrared spectroscopy (FTIR) verified the formation of an amorphous solid-solution of titania and silica after sintering. The thermal expansion of the glasses was measured using a differential dilatometer. The average linear coefficients of thermal expansion (CTE @ 25-675°C) varied between +5 × 10-7 and -0.2 × 10-7°C-1 in the range 0 to 9% TiO2. The glass with 7.2% TiO2 exhibited a zero thermal expansion coefficient at 150-210°C. The hysteresis in CTE on heating and cooling was of the order of 0.01-0.02 ppm.

Original languageEnglish (US)
Pages (from-to)364-370
Number of pages7
JournalJournal of Non-Crystalline Solids
Volume100
Issue number1-3
DOIs
StatePublished - Mar 1988

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Sol-gels
gels
Glass
expansion
glass
titanium
Processing
Titanium
Thermal expansion
thermal expansion
Gels
Polymethyl Methacrylate
Sols
silicon dioxide
Silicon Dioxide
sintering
Sintering
Silica
fumes
microstructure

All Science Journal Classification (ASJC) codes

  • Electronic, Optical and Magnetic Materials
  • Ceramics and Composites
  • Condensed Matter Physics
  • Materials Chemistry

Cite this

Deng, Zaide ; Breval, Else ; Pantano, Carlo G. / Colloidal sol/gel processing of ultra-low expansion TiO2/SiO2 glasses. In: Journal of Non-Crystalline Solids. 1988 ; Vol. 100, No. 1-3. pp. 364-370.
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abstract = "A series of titania-silica glasses with 0-9{\%} TiO2 were fabricated using a sol/gel process. The sol was prepared by dispersing colloidal silica fume in an aqueous solution of titania which was synthesized through the acid-catalyzed hydrolysis of titanium isopropoxide. The sols gelled in 2-4 days, and then were dried for 6-8 days. The dry gels were sintered at 1450-1500°C to produce clear, dense, microstructure-free glasses. The gels underwent a total shrinkage of ∼50{\%} to yield glass rods about 50 mm long and 5 mm in diameter, or glass discs about 4 cm in diameter and 5 mm thick. The drying step was most critical in the production of crack-free specimens. In the gel, the transmission electron microscope (TEM) revealed the presence of 1-5 nm rutile microcrystallites uniformly distributed within a network of colloidal silica particles. After sintering to 1450-1500°C, though, a dense, transparent, microstructure-free glass was created. Fourier transform infrared spectroscopy (FTIR) verified the formation of an amorphous solid-solution of titania and silica after sintering. The thermal expansion of the glasses was measured using a differential dilatometer. The average linear coefficients of thermal expansion (CTE @ 25-675°C) varied between +5 × 10-7 and -0.2 × 10-7°C-1 in the range 0 to 9{\%} TiO2. The glass with 7.2{\%} TiO2 exhibited a zero thermal expansion coefficient at 150-210°C. The hysteresis in CTE on heating and cooling was of the order of 0.01-0.02 ppm.",
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Colloidal sol/gel processing of ultra-low expansion TiO2/SiO2 glasses. / Deng, Zaide; Breval, Else; Pantano, Carlo G.

In: Journal of Non-Crystalline Solids, Vol. 100, No. 1-3, 03.1988, p. 364-370.

Research output: Contribution to journalArticle

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N2 - A series of titania-silica glasses with 0-9% TiO2 were fabricated using a sol/gel process. The sol was prepared by dispersing colloidal silica fume in an aqueous solution of titania which was synthesized through the acid-catalyzed hydrolysis of titanium isopropoxide. The sols gelled in 2-4 days, and then were dried for 6-8 days. The dry gels were sintered at 1450-1500°C to produce clear, dense, microstructure-free glasses. The gels underwent a total shrinkage of ∼50% to yield glass rods about 50 mm long and 5 mm in diameter, or glass discs about 4 cm in diameter and 5 mm thick. The drying step was most critical in the production of crack-free specimens. In the gel, the transmission electron microscope (TEM) revealed the presence of 1-5 nm rutile microcrystallites uniformly distributed within a network of colloidal silica particles. After sintering to 1450-1500°C, though, a dense, transparent, microstructure-free glass was created. Fourier transform infrared spectroscopy (FTIR) verified the formation of an amorphous solid-solution of titania and silica after sintering. The thermal expansion of the glasses was measured using a differential dilatometer. The average linear coefficients of thermal expansion (CTE @ 25-675°C) varied between +5 × 10-7 and -0.2 × 10-7°C-1 in the range 0 to 9% TiO2. The glass with 7.2% TiO2 exhibited a zero thermal expansion coefficient at 150-210°C. The hysteresis in CTE on heating and cooling was of the order of 0.01-0.02 ppm.

AB - A series of titania-silica glasses with 0-9% TiO2 were fabricated using a sol/gel process. The sol was prepared by dispersing colloidal silica fume in an aqueous solution of titania which was synthesized through the acid-catalyzed hydrolysis of titanium isopropoxide. The sols gelled in 2-4 days, and then were dried for 6-8 days. The dry gels were sintered at 1450-1500°C to produce clear, dense, microstructure-free glasses. The gels underwent a total shrinkage of ∼50% to yield glass rods about 50 mm long and 5 mm in diameter, or glass discs about 4 cm in diameter and 5 mm thick. The drying step was most critical in the production of crack-free specimens. In the gel, the transmission electron microscope (TEM) revealed the presence of 1-5 nm rutile microcrystallites uniformly distributed within a network of colloidal silica particles. After sintering to 1450-1500°C, though, a dense, transparent, microstructure-free glass was created. Fourier transform infrared spectroscopy (FTIR) verified the formation of an amorphous solid-solution of titania and silica after sintering. The thermal expansion of the glasses was measured using a differential dilatometer. The average linear coefficients of thermal expansion (CTE @ 25-675°C) varied between +5 × 10-7 and -0.2 × 10-7°C-1 in the range 0 to 9% TiO2. The glass with 7.2% TiO2 exhibited a zero thermal expansion coefficient at 150-210°C. The hysteresis in CTE on heating and cooling was of the order of 0.01-0.02 ppm.

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