Synthesis of Titania-supported Copper Nanoparticles via Refined Alkoxide Sol-gel Process

• Published in: Journal of nanoparticle research : an interdisciplinary forum for nanoscale science and technology Vol. 3; no. 2-3; p. 113
• Main Authors: Wu, Jeffrey Cs, Tseng, I-hsiang, Chang, Wan-chen
• Format: Journal Article
• Language: English
• Published: Dordrecht Springer Nature B.V 01.06.2001
• Subjects: Acetic acid; Copper; Hydrolysis; Nanoparticles; Titanium
• ISSN: 1388-0764; 1572-896X
• DOI: 10.1023/A:1017553125829

Nanoparticles of titania and copper-loaded titania were synthesized by a refined sol-gel method using titanium butoxide. Unlike the conventional sol-gel procedure of adding water directly, the esterification of anhydrous butanol and glacial acetic acid provided the hydrolyzing water. In addition, acetic acid also served as a chelating ligand to stabilize the hydrolysis-condensation process and minimize the agglomeration of titania. Following the hydrolysis, Cu/TiO^sub 2^ was prepared by adding copper chloride to titania sol. The sol was dried, then calcined at 500^sup °^C to remove organics and transformed to anatase titania which was verified by XRD. Cu/TiO^sub 2^ was further hydrogen-reduced at 300^sup °^C. The recovery of Ti was exceeded by an average of 95% from titanium butoxide. TEM micrographs show that the Cu/TiO^sub 2^ particles are near uniform. The average crystallite sizes are 17-20 nm estimated from the peak broadening of XRD spectra. The bandgaps of TiO^sub 2^ and reduced Cu/TiO^sub 2^ range from 2.70 to 3.15 eV estimated from the diffusive reflective UV-Vis spectra. XPS analysis shows that Cu 2p^sub 3/2^ is 933.4 eV indicating primary Cu^sub 2^O form on the TiO^sub 2^ supports. The binding energy of Ti does not exhibit chemical shift suggesting negligible interaction of Cu cluster and TiO^sub 2^ support.[PUBLICATION ABSTRACT]