ZnO-activated formation of phase pure perovskite Pb(In1/2Nb1/2)O3-Pb(Zn1/3Nb2/3)O3-PbTiO3 powder

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Abstract

This paper reports on the phase formation of perovskite Pb(In1/2Nb1/2)O3-Pb(Zn1/3Nb2/3)O3-PbTiO3 (PIN-PZN-PT) powder when doped with 0.04 to 0.83 mol% ZnO. Air calcination of undoped powder mixtures for 4 hours at 800°C resulted in a mixture of Pb2Zn0.29Nb1.71O6.565 pyrochlore, PIN-PZN-PT perovskite, and In2O3. ZnO dopant concentrations as low as 0.04 mol% increased the rate of perovskite formation and resulted in near phase pure perovskite powder of 0.5 μm particle size when heated at 800°C in air. In all cases PbTiO3 and Pb(In1/2Nb1/2)O3 formed prior to PIN-PZN-PT formation. ZnO doping promotes perovskite phase formation by increasing the reactivity of the intermediate pyrochlore phase by substituting Zn2+ on Nb5+ sites and forming oxygen vacancies when heated in air. Heating in high Po2 resulted in an incomplete reaction and a mixture of perovskite and pyrochlore whereas low Po2 resulted in phase separation into a mixture of rhombohedral perovskite, tetragonal perovskite, and pyrochlore. The Po2 sensitivity clearly shows that oxygen vacancies due to ZnO-doping are critical for synthesis of phase pure PIN-PZN-PT powder.

Original languageEnglish (US)
JournalJournal of the American Ceramic Society
DOIs
StateAccepted/In press - Jan 1 2019

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Powders
Perovskite
Doping (additives)
Oxygen vacancies
Air
perovskite
Phase separation
Calcination
Particle size
Heating
pyrochlore

All Science Journal Classification (ASJC) codes

  • Ceramics and Composites
  • Materials Chemistry

Cite this

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title = "ZnO-activated formation of phase pure perovskite Pb(In1/2Nb1/2)O3-Pb(Zn1/3Nb2/3)O3-PbTiO3 powder",
abstract = "This paper reports on the phase formation of perovskite Pb(In1/2Nb1/2)O3-Pb(Zn1/3Nb2/3)O3-PbTiO3 (PIN-PZN-PT) powder when doped with 0.04 to 0.83 mol{\%} ZnO. Air calcination of undoped powder mixtures for 4 hours at 800°C resulted in a mixture of Pb2Zn0.29Nb1.71O6.565 pyrochlore, PIN-PZN-PT perovskite, and In2O3. ZnO dopant concentrations as low as 0.04 mol{\%} increased the rate of perovskite formation and resulted in near phase pure perovskite powder of 0.5 μm particle size when heated at 800°C in air. In all cases PbTiO3 and Pb(In1/2Nb1/2)O3 formed prior to PIN-PZN-PT formation. ZnO doping promotes perovskite phase formation by increasing the reactivity of the intermediate pyrochlore phase by substituting Zn2+ on Nb5+ sites and forming oxygen vacancies when heated in air. Heating in high Po2 resulted in an incomplete reaction and a mixture of perovskite and pyrochlore whereas low Po2 resulted in phase separation into a mixture of rhombohedral perovskite, tetragonal perovskite, and pyrochlore. The Po2 sensitivity clearly shows that oxygen vacancies due to ZnO-doping are critical for synthesis of phase pure PIN-PZN-PT powder.",
author = "Brova, {Michael J.} and Watson, {Beecher H.} and Kupp, {Elizabeth Rader} and Fanton, {Mark Andrew} and {Meyer, Jr.}, {Richard Joseph} and Messing, {Gary Lynn}",
year = "2019",
month = "1",
day = "1",
doi = "10.1111/jace.16296",
language = "English (US)",
journal = "Journal of the American Ceramic Society",
issn = "0002-7820",
publisher = "Wiley-Blackwell",

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T1 - ZnO-activated formation of phase pure perovskite Pb(In1/2Nb1/2)O3-Pb(Zn1/3Nb2/3)O3-PbTiO3 powder

AU - Brova, Michael J.

AU - Watson, Beecher H.

AU - Kupp, Elizabeth Rader

AU - Fanton, Mark Andrew

AU - Meyer, Jr., Richard Joseph

AU - Messing, Gary Lynn

PY - 2019/1/1

Y1 - 2019/1/1

N2 - This paper reports on the phase formation of perovskite Pb(In1/2Nb1/2)O3-Pb(Zn1/3Nb2/3)O3-PbTiO3 (PIN-PZN-PT) powder when doped with 0.04 to 0.83 mol% ZnO. Air calcination of undoped powder mixtures for 4 hours at 800°C resulted in a mixture of Pb2Zn0.29Nb1.71O6.565 pyrochlore, PIN-PZN-PT perovskite, and In2O3. ZnO dopant concentrations as low as 0.04 mol% increased the rate of perovskite formation and resulted in near phase pure perovskite powder of 0.5 μm particle size when heated at 800°C in air. In all cases PbTiO3 and Pb(In1/2Nb1/2)O3 formed prior to PIN-PZN-PT formation. ZnO doping promotes perovskite phase formation by increasing the reactivity of the intermediate pyrochlore phase by substituting Zn2+ on Nb5+ sites and forming oxygen vacancies when heated in air. Heating in high Po2 resulted in an incomplete reaction and a mixture of perovskite and pyrochlore whereas low Po2 resulted in phase separation into a mixture of rhombohedral perovskite, tetragonal perovskite, and pyrochlore. The Po2 sensitivity clearly shows that oxygen vacancies due to ZnO-doping are critical for synthesis of phase pure PIN-PZN-PT powder.

AB - This paper reports on the phase formation of perovskite Pb(In1/2Nb1/2)O3-Pb(Zn1/3Nb2/3)O3-PbTiO3 (PIN-PZN-PT) powder when doped with 0.04 to 0.83 mol% ZnO. Air calcination of undoped powder mixtures for 4 hours at 800°C resulted in a mixture of Pb2Zn0.29Nb1.71O6.565 pyrochlore, PIN-PZN-PT perovskite, and In2O3. ZnO dopant concentrations as low as 0.04 mol% increased the rate of perovskite formation and resulted in near phase pure perovskite powder of 0.5 μm particle size when heated at 800°C in air. In all cases PbTiO3 and Pb(In1/2Nb1/2)O3 formed prior to PIN-PZN-PT formation. ZnO doping promotes perovskite phase formation by increasing the reactivity of the intermediate pyrochlore phase by substituting Zn2+ on Nb5+ sites and forming oxygen vacancies when heated in air. Heating in high Po2 resulted in an incomplete reaction and a mixture of perovskite and pyrochlore whereas low Po2 resulted in phase separation into a mixture of rhombohedral perovskite, tetragonal perovskite, and pyrochlore. The Po2 sensitivity clearly shows that oxygen vacancies due to ZnO-doping are critical for synthesis of phase pure PIN-PZN-PT powder.

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