Authors:
G. Ingo CNR Istituto di Chimica dei Materiali CP 10 00016 Monterotondo Stazione, Roma Italy CP 10 00016 Monterotondo Stazione, Roma Italy

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C. Riccucci CNR Istituto di Chimica dei Materiali CP 10 00016 Monterotondo Stazione, Roma Italy CP 10 00016 Monterotondo Stazione, Roma Italy

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G. Bultrini Università di Catania Dipartimento di Chimica v.le A. Doria 6 95125 Catania Italy v.le A. Doria 6 95125 Catania Italy

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S. Dirè Università di Trento Dipartimento Ingegneria dei Materiali 38050 Mesiano-Trento Italy 38050 Mesiano-Trento Italy

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G. Chiozzini CNR Istituto di Chimica dei Materiali CP 10 00016 Monterotondo Stazione, Roma Italy CP 10 00016 Monterotondo Stazione, Roma Italy

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Abstract  

Amorphous SiO2, TiO2 and xSiO2–(1–x)TiO2 ceramic materials with selected values of x 0.5, 0.7 and 0.9, have been prepared via sol-gel process using silicon tetraethoxysilane (TEOS) and titanium tetraisopropoxide Ti(OPri)4. By means of the combined use of differential thermal analysis (DTA),thermogravimetry (TG), X-ray diffraction (XRD), scanning electron microscopy (SEM),X-ray photoelectron spectroscopy (XPS) and X-ray induced Auger electron spectroscopy(XAES), the surface microchemical structure and morphology of the sol-gel materials have been studied as a function of thermal treatments carried out in air up to 1200C. In the range of temperature from 50 to 450C, DTA-TG results evidence a remarkable mass loss due to the evaporation of organic solvents entrapped in the sol-gel materials and of the remnant organic components of the precursor metal alkoxides. In the range of temperature from 400 to about 1000C, by means of the combined use of DTA, XRD, XPS and XAES techniques as a function of temperature and of chemical composition, it is possible to evidence the formation of crystalline phases such as quartz, anatase and rutile. Furthermore, line shape analysis of O1s XPS peak allows to distinguish between single O–Ti and O–Si bonds and also to disclose the presence of cross linking Si–O–Ti bonds, that act as bridges between SiO2and TiO2 moieties. As a function of temperature, Si–O–Ti bonds are broken and the formation of new Ti–O and Si–O bonds as in TiO2 and SiO2takes place as well as a silica segregation phenomenon.

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Journal of Thermal Analysis and Calorimetry
Language English
Size A4
Year of
Foundation
1969
Volumes
per Year
1
Issues
per Year
24
Founder Akadémiai Kiadó
Founder's
Address
H-1117 Budapest, Hungary 1516 Budapest, PO Box 245.
Publisher Akadémiai Kiadó
Springer Nature Switzerland AG
Publisher's
Address
H-1117 Budapest, Hungary 1516 Budapest, PO Box 245.
CH-6330 Cham, Switzerland Gewerbestrasse 11.
Responsible
Publisher
Chief Executive Officer, Akadémiai Kiadó
ISSN 1388-6150 (Print)
ISSN 1588-2926 (Online)

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