Polymerized Complex Synthesis of Perovskite Lead Titanate at Reduced Temperatures:  Possible Formation of Heterometallic (Pb,Ti)-Citric Acid Complex

Abstract

Perovskite PbTiO 3 powders were prepared by a polymerized complex technique at relatively low temperatures, viz. 400-600 °C. Heating of a mixed solution of citric acid (CA), ethylene glycol (EG), and Pb and Ti ions with a molar ratio of Pb/Ti/CA/EG ) 1/1/10/40 at 130 °C produced a yellowish transparent polymeric gel without any precipitation, which after pyrolysis at 300 °C was converted to a powder precursor for PbTiO 3 . We suggest, based on the results of Raman and 13 C NMR spectroscopies, that a heterometallic (Pb,Ti)-CA 3 chelate complex formed in a starting Pb/Ti/CA/EG solution and it was thermally stable upon polymerization at 130 °C. Chemical analyses showed no PbO loss during calcination of powder precursors at 400-700 °C, which led to the conclusion that a solid-state reaction between isolated PbO and TiO 2 particles was not responsible for PbTiO 3 formation, but PbTiO 3 formed directly by thermal decomposition of the powder precursor above 400 °C.

Preparation and Characterization of Yttrium-Titanium Citrate Complexes

“…The results might contribute to better understandig of the chemistry of the complexation process involved in PCM application. 4 and CA in EG, ensuring the above mentioned ratio. Necessary measures were taken to prevent the Ti 4+ hydrolysis.…”

“…or Pb 2+ )±Ti 4+ systems [3,4]. The deprotonation of the alcoholic OH group, proceeding only in the bimetallic solutions, is one of the main proofs for the formation of mixed-metal complexes in solution [1±4].…”

A novel route to perovskite lead zirconate titanate from glycolate precursors via the sol–gel process

“…[8 -10] The FTIR spectrum of PZT4 dried gel shows a visible broad peak at 3500 cm −1 (ν O-H), [2] smaller peaks at 1725 and 1630 cm −1 (ν C-O) and a peak at 1085 cm −1 (ν C-O-Pb). [13,14] The broad peak at 783 cm −1 can be identified as the Pb-O-Zr stretching. [2,13,14] These peaks are identical to those of PbZrO 3 and PbTiO 3 dried gels, indicating the Pb-O-Ti and Pb-O-Zr stretchings.…”

Síntese e Caracterização do Composto SrTi1-xFexO3 Nanoestruturado

“…Nas últimas décadas, a utilização do método dos precursores poliméricos ou método Pechini 41 na síntese de diferentes óxidos policatiônicos na forma de pó ou filmes finos vem sendo realizada com grande sucesso [42][43][44][45][46][47] .…”

“…Inicialmente, a preparação da resina precursora ST foi realizada através do método dos precursores poliméricos tradicional 26,44 . Seguindo essa nova metodologia, a preparação da resina ST foi realizada através do preparo de um poliéster de titânio e de outro poliéster de estrôncio, os quais foram misturados e aquecidos para a formação da resina polimérica precursora ST.…”