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Effect of phase separation in metal carboxylate gels on perovskite lead magnesium niobate crystallization

Published online by Cambridge University Press:  31 January 2011

Yeshwanth Narendar  and
Gary L. Messing
Yeshwanth Narendar
Affiliation:
Department of Materials Science and Engineering, The Pennsylvania State University, University Park, Pennsylvania 16802–4801
Gary L. Messing
Affiliation:
Department of Materials Science and Engineering, The Pennsylvania State University, University Park, Pennsylvania 16802–4801
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Abstract

Phase separation during the synthesis and decomposition of lead magnesium niobate (PMN)–ethylenediaminetetraacetic acid (EDTA) and PMN–citrate gels strongly affects perovskite Pb(Mg1/3Nb2/3)O3 phase formation. The PMN–EDTA gel was synthesized from a solution containing Pb–EDTA, Mg–EDTA, and peroxo–citrato–niobium complexes at pH 8. Pb–EDTA precipitation was avoided by using Pb:EDTA in the mole ratio >1:2.5 and flash pyrolyzing the PMN–EDTA solution at 225 °C. Consequently, the PMN yield increased from 80 to 98 wt%. The sequential decomposition of Pb–EDTA, Mg–EDTA, and peroxo–citrato–Nb in the PMN–EDTA precursor in 1 vol% O2 leads to phase separation of Pb and PbO and thus lowers the PMN yield to 92 wt%. At PO2 > 2.5 vol% the Pb, Mg, and Nb complexes cothermolyze to form ≥97 % perovskite PMN. The presence of a heterometallic citrato–Pb–Mg–Nb complex in PMN–citrate leads to oxygen partial pressure independent codecomposition of the Pb, Mg, and Nb complexes. Accordingly, PMN yields of ≥96 wt% were obtained from the PMN–citrate precursor for oxygen partial pressures between 1 and 5 vol%.

Type
Articles
Information
Journal of Materials Research , Volume 14 , Issue 10 , October 1999 , pp. 3921 - 3931
Copyright
Copyright © Materials Research Society 1999

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