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Formation, Structure, and Material Properties From the Reaction Product of M(OCHMe2)4 (M=Ti, Zr) And HOAc

Published online by Cambridge University Press:  21 February 2011

Todd M. Alam
Affiliation:
Dept. of Chem., U. of N.M., Albuquerque, NM Sandia National Laboratories, The Advanced Materials Laboratory, Albuquerque, NM
Timothy J. Boyle
Affiliation:
Dept. of Chem., U. of N.M., Albuquerque, NM
Catherine D. Buchheit
Affiliation:
Dept. of Chem., U. of N.M., Albuquerque, NM
Robert W. Schwartz
Affiliation:
Dept. of Chem., U. of N.M., Albuquerque, NM
Joseph W. Ziller
Affiliation:
Dept. of Chem., U. of N.M., Albuquerque, NM Dept. of Chem. U.C.‐Irvine, Irvine, CA
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Abstract

In attempt to ultimately control the characteristics of the PZT films, we have decided to investigate some of the basic chemistry associated with these solutions. Frequently, these solutions have been generated from Group IV metal alkoxides in acetic acid (HOAc). Therefore, studies of the simple reactivity between M(OCHMe2)4 (M = Ti, Zr) and HOAc have been undertaken. These reactions were monitored by 1H, 13C, 17O NMR, FT-IR, TGA/DTA, and single crystal X‐ray studies. Films were produced from spin‐coat deposition of crystalline material (from the titanium reaction) in toluene and aged solutions as well.

Type
Research Article
Copyright
Copyright © Materials Research Society 1998

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References

REFERENCES

1 This work has been reported in part by: Boyle, T.J. and Schwartz, R.W., “An Investigation of Group (IV) Alkoxides as Property Controlling Reagents in the Synthesis of Ceramic Materials”, Comments on Inorganic Chemistry, in press. Google Scholar
2 a. Schwartz, R.W., Assink, R.A., and Headley, T.J., Mat. Res. Soc. Symp. Proc, 243, 245 (1992). b. G. Yi, Z. Wu, and M. Sayer, J. Appl. Phys., 64, 2717 (1988). c. K.D. Budd, S.K. Dey, and D.A. Payne, Brit. Ceram. Soc. Proc, 36, 107 (1985).CrossRefGoogle Scholar
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4 a. Spectra were obtained on an Nicolet Magna FT‐IR‐System 550 (KBr pellet, 32 scans), b. IR of 1: IR (KBr pellet) 2970.7 (s), 2930.9 (s), 2866.4 (s), 2712.8 (w), 2621.8 (w), 1569.7 (s), 1442.3 (s), 1377.4 (m), 1360.0 (m), 1329.3 (w), 1163.5 (vs), 1132.3 (vs), 1014.5 (vs), 954.4 (m), 855.9 (m), 798.2 (w), 663.6 (m). 632.4, 601.1 (m) cm‐', c. IRof2: (KBr pellet) 2970.5 (s), 2935.0 (m), 2929.0 (m), 2897.5 (w), 2889.4 (w), 2881.4 (w), 2872.7 (w), 2866.0 (w), 1603.1 (vs), 1579.2 (vs), 1558.9 (vs), 1454.8 (s), 1418.9 (s), 1375.8 (w), 1359.0 (w), 1339.9 (w), 1325.5 (w), 1169.9(s), 1136.4 (vs), 1019.1 (vs), 954.5 (w), 854.0 (w), 796.6 (m), 791.8 (m), 696.0 (m), 664.9 (m) cm”1.Google Scholar
5 NMR spectra were obtained on a Brucker 250 MHz NMR spectrometer (CöDó or toluene‐ds). The H2170 (external reference) for 170 NMR was kindly donated by D.L. Clark (Los Alamos National Laboratory).Google Scholar
6 Esterification of acetic acid: J. March Advanced Organic Chemistry, Reactions, Mechanisms, and Structure Sr‐i Ed. (John Wiley and Sons, New York, 1985) Chapter 10, 348.Google Scholar
7 ? NMR resonances for: 1 (C6D6): δ = 5.79, (sept.), 5.03 (mult.), 4.09 (sept.), 4.61 (bs), 2.01 (s), 1.93 (s), 1.73 to 1.65 (mult.), 1.62 to 1.55 (mult.), 1.43 to 1.33 (mult.), 1.01 (s), 0.99 (s). Methyl/methine region = 0.123; 2 (C7D8) δ = 5.71 (sept.), 5.32 to 5.11 (mult.), 5.08 to 4.93 (mult.), 4.80 (sept.), 4.59 (sept.), 4.26 to 4.18 (mult.), 2.99 (sept.), 2.00 (s), 1.97 (s), 1.96 (d), 1.95 (s), 1.93 (s), 1.87 (s), 1.80 (s), 1.77 (s), 1.76 (s), 1.64 (s), 1.62 (s), 1.58, 1.54 (s). 1.55 to 1.23 (mult.), 1.26 (s), 1.23 (s), 0.87 (m). Methyl/methine region = 0.082.Google Scholar
8 Private communications with R.A. Assink (Sandia National Laboratories), T.M. Alam (Univ. of New Mexico), and D.L. Clark (L.A.N.L.). Refered to: a) D.W. Boykin, 170 NMR Spectroscopy in Organic Chemistry, (CRC Press, Boca Raton, 1991). b) W.G. Klemperer, Angew. Chem. Int. Ed. Engl., 17, 246 (1978).CrossRefGoogle Scholar
9 Bradley, D.C., Mehrotra, F.C., and Gaur, P.D., Metal Alkoxides (Academic Press, New York, 1978). b. K.G. Caulton and L.G. Hubert‐Pfalzgraf, Chem. Rev., 90, 969 (1990). c. D.C. Bradley, Chem. Rev., 89, 1317 (1989). d. D.C. Bradley, H. Chudzynska, D.M. Frigo, M.B. Hursthouse, and M.A. Mazid, J. Chem. Soc, Chem. Commun. 1258 (1988). e. CD. Chandler, C. Roger, and M.J. Hampden‐Smith, Chem. Rev. 93, 1205 (1993).Google Scholar
10 Schwartz, R.W., Voigt, J.A., Buchheit, C.D., and Boyle, T.J., Cer. Trans.‐ Proc. Am. Ceramic Society, PAC Rim Meeting, November, 1993, Honolulu, HI, in press.Google Scholar

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Formation, Structure, and Material Properties From the Reaction Product of M(OCHMe2)4 (M=Ti, Zr) And HOAc
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