Abstract
Early-stage processes involving the polymerization of zirconium species in aqueous solutions at elevated temperatures (∼100 °C) as well as colloid formation were studied. Small-angle x-ray scattering (SAXS) data were analyzed via Guinier, “longrods,” and Porod plots to determine particle growth kinetics and morphology. Our SAXS data suggest that zirconium tetramers and octamers polymerize into larger clusters and elongated-rod-(or needle)-shaped primary particles, which have a length of a few nanometers and a radius of gyration of cross section between 4 and 5 Å. Cube-shaped particles are aggregates of the needlelike primary particles. The transition from zirconium tetramer to a colloidal sol particle follows a mass-fractal growth (1 < fractal dimension, D <3)
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References
E. Matijević, Progr. Colloid Polymer Sci. 61, 24 (1976).
E. Matijević, Langmuir 10, 8 (1994).
A. Clearfield, Inorg. Chem. 3, 146 (1964a).
A. Clearfield, Rev. Pure Appl. Chem. 14, 91 (1964b).
H. Sariçimen, Powder Technol. 27, 23 (1980).
E. Tani, M. Yoshimura, and S. Sōmiya, J. Am. Ceram. Soc. C-181 (1981).
P.E. D. Morgan, J. Am. Ceram. Soc. C-204 (1984).
M.A. Blesa, A.J. G. Maroto, S. I. Passaggio, N. E. Figliolia, and G. Rigotti, J. Mater. Sci. 20, 4601 (1985).
A. Bleier and R. M. Cannon, in Better Ceramics Through Chemistry II, edited by C. J. Brinker, D. E. Clark, and D.R. Ulrich (Mater. Res. Soc. Symp. Proc. 73, Pittsburgh, PA, 1986), p. 71.
Y-X. Huang and C-J. Guo, Powder Technol. 72, 101 (1992).
Y.T. Moon, D.K. Kim, and C.H. Kim, J. Am. Ceram. Soc. 78, 1103 (1995).
R.W. Siegel, Sci. Am. December, 74 (1996).
L.M. Toth, J. S. Lin, and L.K. Felker, J. Phys. Chem. 95, 3106 (1991).
A. Singhal, L. M. Toth, J. S. Lin, and K. Affholter, J. Am. Chem. Soc. 118, 11529 (1996).
A. Clearfield, J. Mater. Res. 5, 161 (1990).
J. A. Juston, R. M. Richardson, S. L. Jones, and C. Norman, in Better Ceramics Through Chemistry IV, edited by B.J. J. Zelinsky, C.J. Brinker, D. E. Clark, and D. R. Ulrich (Mater. Res. Soc. Symp. Proc. 180, Pittsburgh, PA, 1990), p. 123.
M. Henry, J. P. Jolivet, and J. Livage, Struct. Bond. 77, 153 (1992).
J. Livage, M. Chatry, M. Henry, and F. Taulelle, in Better Ceramics Through Chemistry V, (Mater. Res. Soc. Symp. Proc. 271, Pittsburgh, PA, 1992), p. 201.
C.H. Byers, M.T. Harris, and D.F. Williams, Ind. Eng. Chem. Res. 26, 1916 (1987).
A. Guinier and G. Fournet, Small Angle Scattering of X-rays (John Wiley, New York, 1955).
A. Guinier, Ann. Phys. 12 161 (1939).
J. E. Martin and A. J. Hurd, J. Appl. Crystallogr. 20, 61 (1987).
R. Jullien and R. Botet, Aggregation and Fractal Aggregates (World Scientific, Singapore, 1987).
J. Teixeira, J. Appl. Crystallogr. 21, 781 (1988).
P.W. Schmidt, The Fractal Approach to Heterogeneous Chemistry, edited by D. Avnir (John Wiley & Sons, New York, 1989), p. 67.
A. Bunde and S. Havlin, Fractals and Disordered Systems (Springer-Verlag, New York, 1991).
M.Z-C. Hu, M.T. Harris, and C. H. Byers, J. Colloid Inter. Sci. 198, 87 (1998).
G.M. Muha and P.A. Vaughan, J. Chem. Phys. 33, 194 (1960).
M. Åberg, Acta Chem. Scand. A 31, 171 (1964).
M. Åberg and J. Glaster, Inorg. Chim. Acta 206, 53 (1993).
S. Hannane, F. Bertin, and J. Bouix, Bull. Soc. Chem. Fr. 127, 43 (1990).
R.L. Angstadt and S. Y. Tyree, J. Inorg. Nucl. Chem. 24, 913 (1962).
J. A. Johnson and K.A. Kraus, J. Am. Chem. Soc. 78, 3937 (1956).
A. Clearfield and P. A. Vaughan, Acta Crystallogr. 9, 555 (1956).
T.C. W. Mak, Can. J. Chem. 46, 3491 (1968).
M.D. Atherton and H. Sutcliffe, J. Less-Common Met. 138, 63 (1988).
K. Lee and A. McCormick, personal communication, University of Minnesota, Minneapolis, Minnesota.
L.L. Hench and J. K. West, Chem. Rev. 90, 33 (1990).
E.J. A. Pope, in Better Ceramics Through Chemistry V, edited by M.J. Hampden-Smith, W. G. Klemperer, and C. J. Brinker (Mater. Res. Soc. Symp. Proc. 271, Pittsburgh, PA, 1992), p. 213.
D.W. Schaefer and K.D. Keefer, in Better Ceramics Through Chemistry II, edited by C. J. Brinker, D. E. Clark, and D. R. Ulrich (Mater. Res. Soc. Symp. Proc. 73, Pittsburgh, PA 1986), p. 277.
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Hu, M.Z.C., Zielke, J.T., Lin, J.S. et al. Small-angle x-ray scattering studies of early-stage colloid formation by thermohydrolytic polymerization of aqueous zirconyl salt solutions. Journal of Materials Research 14, 103–113 (1999). https://doi.org/10.1557/JMR.1999.0017
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DOI: https://doi.org/10.1557/JMR.1999.0017