Preparation of titania from tetrakis(diethylamino)titanium via hydrolysis

Yoshizumi Ishikawa; Hideyasu Honda; Yoshiyuki Sugahara

doi:10.1023/A:1008718723502

Preparation of titania from tetrakis(diethylamino)titanium via hydrolysis

Yoshizumi Ishikawa, Hideyasu Honda, Yoshiyuki Sugahara

School of Advanced Science and Engineering

Research output: Contribution to journal › Article › peer-review

3 Citations (Scopus)

Abstract

The conversion of tetrakis(diethylamino)titanium (Ti(NEt₂)₄) into titania via either a combination of hydrolysis (Ti(NEt₂)₄:THF:H₂O = 1:10:x, x = 2, 4, 10) at ambient conditions and calcination (method A) or hydrolysis in a water-tetrahydrofuran (THF) mixture (Ti(NEt₂)₄:THF:H₂O = 1:10:100) at reflux (method B) was investigated. Titanium tertiary butoxide (Ti(O^tBu)₄) was also used as a substitute for Ti(NEt₂)₄. The hydrolysis via method A resulted in the formation of amorphous solids containing organics. Thermal analyses showed that the hydrolysis products showed mass losses up to 500°C probably due to the presence of diethylamine (Et₂NH) formed via the hydrolysis of Ti(NEt₂)₄ in the hydrolysis products, while a mass loss of the hydrolysis product from Ti(O^tBu)₄ was completed up to about 200°C. After calcination at ≥600°C, anatase or a mixture of anatase and rutile was obtained. The crystallization behavior of the hydrolysis products from Ti(NEt₂)₄ was different from that of the hydrolysis product from Ti(O^tBu)₄. The hydrolysis via method B gave only an amorphous material from Ti(NEt₂)₄, while a crystalline titania (anatase and brookite) formed from Ti(O^tBu)₄.

Original language	English
Pages (from-to)	365-369
Number of pages	5
Journal	Journal of Sol-Gel Science and Technology
Volume	19
Issue number	1-3
DOIs	https://doi.org/10.1023/A:1008718723502
Publication status	Published - 2000 Dec

ASJC Scopus subject areas

Electronic, Optical and Magnetic Materials
Ceramics and Composites
Chemistry(all)
Biomaterials
Condensed Matter Physics
Materials Chemistry

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title = "Preparation of titania from tetrakis(diethylamino)titanium via hydrolysis",

abstract = "The conversion of tetrakis(diethylamino)titanium (Ti(NEt2)4) into titania via either a combination of hydrolysis (Ti(NEt2)4:THF:H2O = 1:10:x, x = 2, 4, 10) at ambient conditions and calcination (method A) or hydrolysis in a water-tetrahydrofuran (THF) mixture (Ti(NEt2)4:THF:H2O = 1:10:100) at reflux (method B) was investigated. Titanium tertiary butoxide (Ti(OtBu)4) was also used as a substitute for Ti(NEt2)4. The hydrolysis via method A resulted in the formation of amorphous solids containing organics. Thermal analyses showed that the hydrolysis products showed mass losses up to 500°C probably due to the presence of diethylamine (Et2NH) formed via the hydrolysis of Ti(NEt2)4 in the hydrolysis products, while a mass loss of the hydrolysis product from Ti(OtBu)4 was completed up to about 200°C. After calcination at ≥600°C, anatase or a mixture of anatase and rutile was obtained. The crystallization behavior of the hydrolysis products from Ti(NEt2)4 was different from that of the hydrolysis product from Ti(OtBu)4. The hydrolysis via method B gave only an amorphous material from Ti(NEt2)4, while a crystalline titania (anatase and brookite) formed from Ti(OtBu)4.",

author = "Yoshizumi Ishikawa and Hideyasu Honda and Yoshiyuki Sugahara",

year = "2000",

month = dec,

doi = "10.1023/A:1008718723502",

language = "English",

volume = "19",

pages = "365--369",

journal = "Journal of Sol-Gel Science and Technology",

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T1 - Preparation of titania from tetrakis(diethylamino)titanium via hydrolysis

AU - Ishikawa, Yoshizumi

AU - Honda, Hideyasu

AU - Sugahara, Yoshiyuki

PY - 2000/12

Y1 - 2000/12

N2 - The conversion of tetrakis(diethylamino)titanium (Ti(NEt2)4) into titania via either a combination of hydrolysis (Ti(NEt2)4:THF:H2O = 1:10:x, x = 2, 4, 10) at ambient conditions and calcination (method A) or hydrolysis in a water-tetrahydrofuran (THF) mixture (Ti(NEt2)4:THF:H2O = 1:10:100) at reflux (method B) was investigated. Titanium tertiary butoxide (Ti(OtBu)4) was also used as a substitute for Ti(NEt2)4. The hydrolysis via method A resulted in the formation of amorphous solids containing organics. Thermal analyses showed that the hydrolysis products showed mass losses up to 500°C probably due to the presence of diethylamine (Et2NH) formed via the hydrolysis of Ti(NEt2)4 in the hydrolysis products, while a mass loss of the hydrolysis product from Ti(OtBu)4 was completed up to about 200°C. After calcination at ≥600°C, anatase or a mixture of anatase and rutile was obtained. The crystallization behavior of the hydrolysis products from Ti(NEt2)4 was different from that of the hydrolysis product from Ti(OtBu)4. The hydrolysis via method B gave only an amorphous material from Ti(NEt2)4, while a crystalline titania (anatase and brookite) formed from Ti(OtBu)4.

AB - The conversion of tetrakis(diethylamino)titanium (Ti(NEt2)4) into titania via either a combination of hydrolysis (Ti(NEt2)4:THF:H2O = 1:10:x, x = 2, 4, 10) at ambient conditions and calcination (method A) or hydrolysis in a water-tetrahydrofuran (THF) mixture (Ti(NEt2)4:THF:H2O = 1:10:100) at reflux (method B) was investigated. Titanium tertiary butoxide (Ti(OtBu)4) was also used as a substitute for Ti(NEt2)4. The hydrolysis via method A resulted in the formation of amorphous solids containing organics. Thermal analyses showed that the hydrolysis products showed mass losses up to 500°C probably due to the presence of diethylamine (Et2NH) formed via the hydrolysis of Ti(NEt2)4 in the hydrolysis products, while a mass loss of the hydrolysis product from Ti(OtBu)4 was completed up to about 200°C. After calcination at ≥600°C, anatase or a mixture of anatase and rutile was obtained. The crystallization behavior of the hydrolysis products from Ti(NEt2)4 was different from that of the hydrolysis product from Ti(OtBu)4. The hydrolysis via method B gave only an amorphous material from Ti(NEt2)4, while a crystalline titania (anatase and brookite) formed from Ti(OtBu)4.

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