Peroxide-based route free from halides for the synthesis of lead titanate powder

E. R. Camargo; M. Kakihana

doi:10.1021/cm000363y

Peroxide-based route free from halides for the synthesis of lead titanate powder

E. R. Camargo, M. Kakihana

Research output: Contribution to journal › Article › peer-review

55 Citations (Scopus)

Abstract

PbTiO₃ has been successfully synthesized at reduced temperatures (500-700°C) using neither organics (including alkoxides) nor undesirable halides. Water-soluble peroxytitanic complexes [Ti(OH)₃O₂]^- were prepared by the reaction between titanium metal and hydrogen peroxide at pH = 11. A solution of lead nitrate was added to the peroxytitanic acid solution and an amorphous precipitate of lead and titanium was formed, which was filtered and washed to eliminate the nitrate ion. The precipitate was calcined between 200 and 700°C in a closed alumina boat. The precipitate was characterized by ICP, TG, Raman spectroscopy, XRD, and SEM, and the calcined lead titanate was characterized by BET, Raman spectroscopy, XRD, and SEM. The amorphous precipitate showed a small weight loss (11.45%). Powders calcined at temperatures higher than 500°C showed pure tetragonal PbTiO₃ perovskite phase on the XRD patterns and Raman spectra and a large surface area in the range of 6-22 m² g^-1. The average diameter of the particles was calculated from the SEM image as 100 nm.

Original language	English
Pages (from-to)	1181-1184
Number of pages	4
Journal	Chemistry of Materials
Volume	13
Issue number	4
DOIs	https://doi.org/10.1021/cm000363y
Publication status	Published - 2001
Externally published	Yes

ASJC Scopus subject areas

Chemistry(all)
Chemical Engineering(all)
Materials Chemistry

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@article{b235a0d4b3114ec4964a1cc2f63384e1,

title = "Peroxide-based route free from halides for the synthesis of lead titanate powder",

abstract = "PbTiO3 has been successfully synthesized at reduced temperatures (500-700°C) using neither organics (including alkoxides) nor undesirable halides. Water-soluble peroxytitanic complexes [Ti(OH)3O2]- were prepared by the reaction between titanium metal and hydrogen peroxide at pH = 11. A solution of lead nitrate was added to the peroxytitanic acid solution and an amorphous precipitate of lead and titanium was formed, which was filtered and washed to eliminate the nitrate ion. The precipitate was calcined between 200 and 700°C in a closed alumina boat. The precipitate was characterized by ICP, TG, Raman spectroscopy, XRD, and SEM, and the calcined lead titanate was characterized by BET, Raman spectroscopy, XRD, and SEM. The amorphous precipitate showed a small weight loss (11.45%). Powders calcined at temperatures higher than 500°C showed pure tetragonal PbTiO3 perovskite phase on the XRD patterns and Raman spectra and a large surface area in the range of 6-22 m2 g-1. The average diameter of the particles was calculated from the SEM image as 100 nm.",

author = "Camargo, {E. R.} and M. Kakihana",

year = "2001",

doi = "10.1021/cm000363y",

language = "English",

volume = "13",

pages = "1181--1184",

journal = "Chemistry of Materials",

issn = "0897-4756",

publisher = "American Chemical Society",

number = "4",

}

TY - JOUR

T1 - Peroxide-based route free from halides for the synthesis of lead titanate powder

AU - Camargo, E. R.

AU - Kakihana, M.

PY - 2001

Y1 - 2001

N2 - PbTiO3 has been successfully synthesized at reduced temperatures (500-700°C) using neither organics (including alkoxides) nor undesirable halides. Water-soluble peroxytitanic complexes [Ti(OH)3O2]- were prepared by the reaction between titanium metal and hydrogen peroxide at pH = 11. A solution of lead nitrate was added to the peroxytitanic acid solution and an amorphous precipitate of lead and titanium was formed, which was filtered and washed to eliminate the nitrate ion. The precipitate was calcined between 200 and 700°C in a closed alumina boat. The precipitate was characterized by ICP, TG, Raman spectroscopy, XRD, and SEM, and the calcined lead titanate was characterized by BET, Raman spectroscopy, XRD, and SEM. The amorphous precipitate showed a small weight loss (11.45%). Powders calcined at temperatures higher than 500°C showed pure tetragonal PbTiO3 perovskite phase on the XRD patterns and Raman spectra and a large surface area in the range of 6-22 m2 g-1. The average diameter of the particles was calculated from the SEM image as 100 nm.

AB - PbTiO3 has been successfully synthesized at reduced temperatures (500-700°C) using neither organics (including alkoxides) nor undesirable halides. Water-soluble peroxytitanic complexes [Ti(OH)3O2]- were prepared by the reaction between titanium metal and hydrogen peroxide at pH = 11. A solution of lead nitrate was added to the peroxytitanic acid solution and an amorphous precipitate of lead and titanium was formed, which was filtered and washed to eliminate the nitrate ion. The precipitate was calcined between 200 and 700°C in a closed alumina boat. The precipitate was characterized by ICP, TG, Raman spectroscopy, XRD, and SEM, and the calcined lead titanate was characterized by BET, Raman spectroscopy, XRD, and SEM. The amorphous precipitate showed a small weight loss (11.45%). Powders calcined at temperatures higher than 500°C showed pure tetragonal PbTiO3 perovskite phase on the XRD patterns and Raman spectra and a large surface area in the range of 6-22 m2 g-1. The average diameter of the particles was calculated from the SEM image as 100 nm.

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U2 - 10.1021/cm000363y

DO - 10.1021/cm000363y

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JO - Chemistry of Materials

JF - Chemistry of Materials

SN - 0897-4756

IS - 4

ER -

Peroxide-based route free from halides for the synthesis of lead titanate powder

Abstract

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