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Mesoporous titania–silica composite from sodium silicate and titanium oxychloride. Part I: grafting method

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Abstract

In this study, we report a versatile method for designing a titania–silica composite using relatively inexpensive precursors. The composite was synthesized by grafting (impregnating) a precursor of a guest component into the preformed host’s solid network. The latter was prepared using sodium silicate as a silica precursor in the presence of cetyltrimethylammonium bromide (CTAB). A freshly prepared solution of titanium oxychloride (TiOCl2, titania precursor that is relatively stable) was introduced into the host’s network to develop a titania–silica composite with initial ratio of Ti:Si = 1. The final product has the overall ratio of Ti:Si = 7:3 and was obtained after calcination for 5 h at 600–1000 °C. The XRD patterns for the calcined samples indicate the presence of TiO2, and there was a significant increase in peak intensity as the calcination temperature increased. EDS, XRF, and FT-IR analyses indicated the formation of a highly pure composite rich in Ti, Si, and O. A Si–O–Ti band at 954 cm−1 was observed, confirming the formation of a titania–silica composite. A composite with optimum properties (homogenous dispersion of the composite and less individual oxide phase separation) was obtained at 600 °C. A similar experiment was also conducted in the absence of CTAB. In this case, the final product was microporous, rendering it unsuitable for some applications.

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Acknowledgements

We would like to thank the Ministry of Commerce and Industries of the Republic of Korea for financial support under the R & D Innovation Fund for Small and Medium Business Administration (Project Application No. S1017370).

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Authors and Affiliations

  1. Department of Chemical Engineering, Hanyang University, 1271 Sa 3-dong, Sangnok-gu, Ansan-si, Gyeonggi-do, 426-791, Republic of Korea

    Askwar Hilonga, Pradip B. Sarawade & Hee Taik Kim

  2. E&B Nanotech. Co., Ltd., Ansan-si, Gyeonggi-do, Republic of Korea

    Jong-Kil Kim

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  1. Askwar Hilonga
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  2. Jong-Kil Kim
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  3. Pradip B. Sarawade
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  4. Hee Taik Kim
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Correspondence to Hee Taik Kim.

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Hilonga, A., Kim, JK., Sarawade, P.B. et al. Mesoporous titania–silica composite from sodium silicate and titanium oxychloride. Part I: grafting method. J Mater Sci 45, 1255–1263 (2010). https://doi.org/10.1007/s10853-009-4076-5

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  • DOI: https://doi.org/10.1007/s10853-009-4076-5

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