Hostname: page-component-cd9895bd7-jn8rn Total loading time: 0 Render date: 2024-12-27T02:31:36.900Z Has data issue: false hasContentIssue false

Preparation of Nanocrystalline Titania Powder by Aerosol Pyrolysis of Titanium Alkoxide

Published online by Cambridge University Press:  10 February 2011

P.P. Ahonen
Affiliation:
VTT Chemical Technology, Aerosol Technology Group, P.O.Box 1401, FIN-02044 VTT, Finland, [email protected]
E.I. Kauppinen
Affiliation:
VTT Chemical Technology, Aerosol Technology Group, P.O.Box 1401, FIN-02044 VTT, Finland, [email protected]
J.L. Deschanvres
Affiliation:
Laboratoire des Matériaux et du Génie Physique (LMGP), ENSPG, Rue de la Houille-Blanche, Domaine Universitaire, BP46, 38402 Saint-Martin-d'Heres, France
J.C. Joubert
Affiliation:
Laboratoire des Matériaux et du Génie Physique (LMGP), ENSPG, Rue de la Houille-Blanche, Domaine Universitaire, BP46, 38402 Saint-Martin-d'Heres, France
G. Van Tendeloo
Affiliation:
EMAT-University of Antwerp (RUCA), Groenenborgerlaan 171, B-2020 Antwerp, Belgium
Get access

Abstract

Nanocrystalline titania powders were prepared via aerosol pyrolysis of titanium tetrabutoxide precursor. As-received and annealed powders were characterized by XRD, SEM and TEM (+EDS), thermogravimetry, Raman- and IR-spectrometry, surface area analysis and XRF. In addition, gas-phase mass size distributions were obtained by low-pressure impactor aerosol measurements. Powders consisted of micrometer sized spherical particles. Amorphous titanium oxide powders were obtained at lower pyrolysis temperatures and only after subsequent thermal annealings crystallized titania was formed. Not until at 500°C in nitrogen and 580°C in air did pyrolysis synthesis form nanocrystalline anatase phase in-situ. During the annealing at 900°C for one hour rutile phase was usually approached, but phase pure anatase was obtained when powder had been synthesized in nitrogen atmosphere at 500°C. The proposed reason for the thermally stable anatase formation is the formation of oxygen deficient anatase phase which has a high thermal barrier to convert to rutile. Titanium tetrabutoxide evaporation and subsequent gas-to-particle formation of additional 30-80 nm particles was observed in nitrogen atmosphere at temperatures higher than precursor boiling point.

Type
Research Article
Copyright
Copyright © Materials Research Society 1998

Access options

Get access to the full version of this content by using one of the access options below. (Log in options will check for institutional or personal access. Content may require purchase if you do not have access.)

References

REFERENCES

1. Kroschwitz, I. and Howe-Grant, M., Kirk-Othmer Encyclopedia of Chemical Technology, Vol. 24 (John Wiley & Sons, Inc., 1997), pp. 235241.Google Scholar
2. Ollis, D.F., Pelizzetti, E., Serpone, N., Environ. Sci. Tech. 5, 1523 (1991).Google Scholar
3. Egashira, M., Chem. Lett. 389 (1988).Google Scholar
4. Nair, P., Mizukami, F., Okubo, T., Nair, J., Keizer, K., Burggraaf, A.J., AIChE Journal 43, 2710 (1997).Google Scholar
5. Brinker, C.J. and Scherer, G.W., Sol-gel science: the physics and chemistry of sol-gel processing, (Academic Press, 1990).Google Scholar
6. Okuyama, K., Jeung, J.-T., Kousaka, Y., Nguyen, H.V., Wu, J.W., Flagan, R.C., Chem. Eng. Sci. 44 (6), 13691375 (1989).Google Scholar
7. Visca, M. and Matijevic, E., J. Coll. Interf. Sci. 68, 308319 (1979).Google Scholar
8. Ishizawa, H., Sakurai, O., Mizutani, N., Kato, M., Yogyo-Kyokai-Shi 93 (7), 382–86 (1985).Google Scholar
9. Durand-Keklikian, L. and Partch, R.E., J. Aerosol Sci. 19, 511521(1988).Google Scholar
10. Park, D.G. and Burlitch, J.M., J. Sol-Gel Sci. Tech. 6, 235249 (1996).Google Scholar
11. Murugavel, P., Kalaiselvam, M., Raju, A.R., Rao, C.N.R., J. Mater. Chem. 7, 14331438 (1997).Google Scholar
12. Rubio, J., Oteo, J.L., Villegas, M., Duran, P., J. Mater. Sci. 32, 643652 (1997).Google Scholar
13. Langlet, M., Walz, D., Marage, P., Joubert, J.C., Thin Solid Films 221, 4454 (1992).Google Scholar
14. Langlet, M. and Joubert, J.C., in Chemistry of Advanced Materials, edited by Rao, C.N.R. (Blackwell Scientific Publications, 1992), pp. 5576.Google Scholar
15. Van, J. Landuyt and Amelinckx, S., Mat. Res. Bull. 5, 267274 (1970).Google Scholar