Thermoanalytical studies of titanium(IV) acetylacetonate xerogels with emphasis on evolved gas analysis

• Published in: Journal of thermal analysis and calorimetry Vol. 88; no. 2; pp. 557 - 563
• Main Authors: ACIK, I. Oja, MADARASZ, J, KRUNKS, M, TONSUAADU, K, JANKE, D, POKOL, G, NIINISTÖ, L
• Format: Conference Proceeding Journal Article
• Language: English
• Published: Dordrecht Springer 01.05.2007
• Subjects: Chemistry; Colloidal state and disperse state; Exact sciences and technology; General and physical chemistry; General, apparatus, technics of preparation; Fourier transformation; Coupled method; Gas release; Thermogravimetry; titania-xerogels; Differential thermal analysis; Gas analysis; Precursor; sol-gel; Infrared spectrometry; EGA-MS; Acetylacetone; EGA-FTIR; titania; Sol gel process; Thermal analysis; Titanium oxide; Xerogel; Evolved gas analysis; simultaneous TG/DTA; Mass spectrometry
• ISSN: 1388-6150; 1588-2926; 1572-8943
• DOI: 10.1007/s10973-006-8064-6

Thermal decomposition of precursor xerogels for TiO2, obtained by gelling of acetylacetonate-modified titanium(IV) tetraisopropoxide (prepared at Ti-alkoxide:acetylacetone molar ratios of 1:1 (Ti-1) and 1:2 (Ti-2)) in boiling 2-methoxyethanol, was monitored by simultaneous TG/DTA/EGA-MS and EGA-FTIR measurements. Thermal degradation processes of Ti-1 and Ti-2 in the temperature range of 30-700 deg C consist of six mass loss steps, the total mass loss being 46.3% and 54.4%, respectively. EGA by FTIR and MS revealed release of H2O below 120 deg C; followed by evolution of acetone and acetic acid between approximately 100 and 320 deg C, and that of CO2 up to 560 deg C. Acetylacetone is evolved to a significant extent from sample Ti-2 at 120-200 deg C.