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Synthesis Of Highly Ordered Macroporous Minerals: Extension of the Synthetic Method to Other Metal Oxides and Organic-Inorganic Composites

Published online by Cambridge University Press:  15 February 2011

C.F. Blanford
Affiliation:
Department of Chemistry, University of Minnesota, Minneapolis, Minnesota 55455
T.N. Do
Affiliation:
Department of Chemistry, University of Minnesota, Minneapolis, Minnesota 55455
B.T. Holland
Affiliation:
Department of Chemistry, University of Minnesota, Minneapolis, Minnesota 55455
A. Stein
Affiliation:
Department of Chemistry, University of Minnesota, Minneapolis, Minnesota 55455
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Abstract

The facile synthesis of three-dimensional macroporous arrays of titania, zirconia and alumina was recently reported [1]. The synthesis of these materials has now been extended to the oxides of iron, tungsten, and antimony, as well as a mixed yttrium-zirconium system and organically modi- fied silicates. These materials were characterized by Fourier-transform infrared spectroscopy (FTIR), scanning electron microscopy (SEM), transmission electron microscopy (TEM), selected area electron diffraction (SAED), X-ray energy dispersive spectrometry (EDS), and powder X-ray diffraction (XRD). Ordered structures of iron, tungsten, and antimony were formed from alkoxide precursors as in the originally reported synthesis, but the template was removed at a lower temperature. Samples of vinyl- and 2-cyanoethyl-modified silicates were formed from a mixture of organotrialkoxysilane and tetraalkoxysilane precursors; the polystyrene template was removed by extraction with a THF/acetone mixture. These results show the ease of extending the original syn- thesis to a wide range of systems. Also, the ability to form homogenous mixed-metal oxides will be important for tailoring the dielectric and photonic properties of these materials.

Type
Research Article
Copyright
Copyright © Materials Research Society 1999

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References

1. Holland, B.T., Blanford, C.F., and Stein, A., Science 281, pp. 538540 (1998).Google Scholar
2. Lobo, R.F. and Davis, M.E., Microporous Mater. 3, pp. 6169 (1994).Google Scholar
3. Yoshikawa, M., Wagner, P., Lovallo, M., Tsuji, K., Takewaki, T., Chen, C.Y, Beck, L.W., Jones, C., Tsapatsis, M., Zones, S.I., and Davis, M.E., J. Phys. Chem. B 102, pp. 71397147 (1998).Google Scholar
4. Davis, M.E., Chem. Eur. J. 3, pp. 17451750 (1997).Google Scholar
5. Wagner, P., Yoshikawa, M., Lovallo, M., Tsuji, K., Tsapatsis, M., and Davis, M.E., Chem. Commun. pp. 21792180 (1997).Google Scholar
6. Beck, J.S., Vartuli, J.C., Roth, W.J., Leonowicz, M.E., Kresge, C.T., Schmitt, K.D., Chu, C.T.-W., Olson, D.H., Sheppard, E.W., McCullen, S.B., Higgins, J.B., and Schlenker, J.L., J. Am. Chem. Soc. 114, pp. 1083410843 (1992).Google Scholar
7. Corma, A., Kan, Q., Navarro, M., J. Prez-Pariente, and F. Rey, Chem. Mater. 9, pp. 21232126 (1997).Google Scholar
8. Khushalani, D., Kuperman, A., Ozin, G.A., Tanaka, K., Garcés, J., Olken, M.M., and Coombs, N., Adv. Mater. 7, pp. 842846 (1995).Google Scholar
9. Zhao, D., Feng, J., Huo, Q., Melosh, N., Fredrickson, G.H., Chmelka, B.F., and Stucky, G.D., Science 279, pp. 548552 (1998).Google Scholar
10. Antonietti, M., Berton, B., Göltner, C., and Hentze, H.P., Adv. Mater. 10, pp. 154159 (1998).Google Scholar
11. Imhof, A. and Pine, D.J., Nature 389, pp. 948951 (1997).Google Scholar
12. Imhof, A. and Pine, D.J., Adv. Mater. 10, pp. 697700 (1998).Google Scholar
13. Velev, O.D., Jede, T.A., Lobo, R.F., and Lenhoff, A.M., Nature 389, pp. 447448 (1997).Google Scholar
14. Holland, B.T., Blanford, C.F., Do, T.N., and Stein, A., submitted to Chem. Mater. (1998).Google Scholar
15. Wijnhoven, J.E.G.J. and Vos, W.L., Science 281, pp. 802804 (1998).Google Scholar
16. Park, S.H. and Xia, Y, Chem. Mater. 10, pp. 17451747 (1998).Google Scholar
17. Zakhidov, A.A., Baughman, R.H., Igbal, Z., Cui, C., Khayrullin, I., Dantas, S.O., Marti, J., and Ralchenko, V.G., Science 282, pp. 897901 (1998).Google Scholar
18. McClune, W.F., Ed. JCPDS -Powder Diffraction File. Newton Square, PA, International Center for Diffraction Data Google Scholar
19. All ranges of values are given based at least ten measurements and are reported at the 95% confidence limit.Google Scholar
20. Smith, J.D. in Comprehensive Inorganic Chemistry, vol. 2, edited by Bailar, J.C. Jr., Emeldus, H.J., Nyholm, S.R., and Trotman-Dickenson, A.F. (Pergamon Press, Oxford, 1973), pp. 547683.Google Scholar
21. Roberts, E.J. and Fenwick, F, J. Am. Chem. Soc. 50, pp. 21252147 (1928).Google Scholar
22. Fast Fourier transforms (FFTs) were used to determine the spatial periodicity of images acquired in the TEM of particles at different angles. The FFT patterns were consistent with a diamond fcc lattice and were indexed accordingly.Google Scholar
23. Lim, M.H., Blanford, C.F., and Stein, A., J. Am. Chem. Soc. 119, pp. 40904091 (1997).Google Scholar
24. Lim, M.H., Blanford, C.F., and Stein, A., Chem. Mater. 10, pp. 467470 (1998).Google Scholar
25. Lim, M.H. and Stein, A., Mater. Res. Soc. Symp. Proc., in press (1998).Google Scholar
26. Huo, Q., Margolese, D.I., and Stucky, G.D., Chem. Mater. 8, pp. 11471160 (1996).Google Scholar