Abstract
The thermal decomposition of an aqueous chemical solution deposition Zn2+-precursor is studied by HT-DRIFT (high temperature diffuse reflectance infrared Fourier transform spectroscopy), on-line coupled TGA-EGA (thermogravimetric analysis - evolved gas analysis by Fourier transform infrared spectroscopy (FTIR) and mass spectrometry (MS)), and HT-XRD (high temperature X-ray diffraction). Using these complementary techniques, it is found that the α-hydroxyl group of the citrate ligand plays a significant role in the decomposition pathway of the ammonium zinc acetate citrate precursor. TEM (transmission electron microscopy) shows that crystalline ZnO (zincite) is formed at 390°C, after dehydroxylation of the α-hydroxyl group and subsequent decarboxylation of the Zn2+-precursor complex. Before total calcination, ZnO particles are already formed and a residual organic backbone thereby remains. The results obtained by these complementary techniques clearly indicate the importance of thermal analysis in the preparation of ceramics through chemical solution deposition.
This is a preview of subscription content, log in via an institution to check access.
Similar content being viewed by others
References
R. NOUWEN, J. MULLENS, D. FRANCO, J. YPERMAN and L. C. VAN POUCKE, Vibrational Spectroscopy 10 (1996) 291.
M. K. VAN BAEL, E. KNAEPEN, A. KAREIVA, I. SCHILDERMANS, R. NOUWEN, J. D'HAEN, M. D'OLIESLAEGER, C. QUAEYHAEGENS, D. FRANCO, J. YPERMAN, J. MULLENS and L. C. VANPOUCKE, Supercond. Sci. Technol. 11 (1998) 82.
M. K. VAN BAEL, A. KAREIVA, R. NOUWEN, I. SCHILDERMANS, G. VANHOYLAND, J. D'HAEN, M. D'OLIESLAEGER, D. FRANCO, J. YPERMAN, J. MULLENS and L. C. VAN POUCKE, Int. J. Inorg. Mater. 1 (1999) 259.
Y. NARENDAR and G. L. MESSING, Catalysis Today 35 (1997) 247.
N. WAKIYA, K. SHINOZAKI and N. MIZUTANI, J. Amer. Ceram. Soc. 80(12) (1997) 3217.
T. R. SHROUT and A. HALLIYAL, Am. Ceram. Soc. Bull. 66(4) (1987) 704.
G. VANHOYLAND, R. NOUWEN, M. K. VAN BAEL, J. YPERMAN, J. MULLENS and L. C. VAN POUCKE, Thermochimica Acta 354 (2000) 145.
E. KNAEPEN, M. K. VAN BAEL, I. SCHILDERMANS, R. NOUWEN, J. D'HAEN, M. D'OLIESLAEGER, C. QUAEYHAGENS, D. FRANCO, J. YPERMAN, J. MULLENS and L. C. VAN POUCKE, ibid. 318 (1998) 143.
S. A. A. MANSOUR, ibid. 233 (1994) 257.
J. MULLENS, R. CARLEER, G. REGGERS, J. YPERMAN, J. VANHEES and L. C. VAN POUCKE, ibid. 212 (1992) 219.
J. MULLENS, in “Handbook of Thermal Analysis and Calorimetry,” Vol.1., edited by M. Brown and P. Gallagher (Elsevier, Amsterdam, 1998) p. 509.
J. MULLENS, A. VOS, R. CARLEER, G. REGGERS, J. YPERMAN and L. C. VAN POUCKE, Thermochimica Acta 207 (1992) 337.
R. C. WEAST (ed.), “CRC Handbook of Chemistry and Physics,” 52nd ed. (Chemical Rubber Company, Cleveland, Ohio, 1971/1972).
A. I. VOGEL, in “Textbook of Quantitative Chemical Analysis,” 5th ed., revised by G. H. Jeffrey, J. Besset, J Mendham and R. C. Denney (Longman Scientific & Technical, London, 1989) p. 302.
M. RAJENDRAN and M. S. RAO, J. Solid State Chem. 113 (1994) 239.
C. J. POUCHERT, in “The Aldrich Library of Infrared Spectra,” 2nd ed. (Aldrich Chemical Company, Inc., Wisconsin, 1975). 87
N. B. COLTHUP, L. H. DALY and S. E. WIBERLY, in “Introduction to Infrared and Raman Spectroscopy,” 3rd ed. (Academic Press, New York).
J. LIVAGE, M. HENRY and C. SANCHEZ, Prog. Solid. St. Chem. 18 (1988) 259.
K. NAKAMOTO, in “Infrared & Raman Spectroscopy of Inorganic and Coordination Compounds, Part B.: Application in Coordination, Organometallic and Bioinorganic Chemistry,” 5th ed. (J. Wiley & Sons, New York, 1997).
“Thermolab Instruction Manual: Evolved Gas Analyser for Thermal Analysis—Mass Spectrometry” (Fisons Instruments) p. 37.
Author information
Authors and Affiliations
Rights and permissions
About this article
Cite this article
Van Werde, K., Mondelaers, D., Vanhoyland, G. et al. Thermal decomposition of the ammonium zinc acetate citrate precursor for aqueous chemical solution deposition of ZnO. Journal of Materials Science 37, 81–88 (2002). https://doi.org/10.1023/A:1013141723764
Issue Date:
DOI: https://doi.org/10.1023/A:1013141723764