Polymorphic Transitions in Cerium-Substituted Zirconolite (CaZrTi2O7)

Clark, Braeden M.; Sundaram, S. K.; Misture, Scott T.

doi:10.1038/s41598-017-06407-5

Title: Polymorphic Transitions in Cerium-Substituted Zirconolite (CaZrTi₂O₇)

Abstract

Compounds with the formulae CaZr_1–xCe_xTi₂O₇ with x = 0.1–0.5 were synthesized by solid state reaction. Cerium was used as a surrogate for actinide elements. A transition from the 2M polymorph to the 4M polymorph (expanded unit cell due to cation ordering) in zirconolite was observed with increasing cerium content. The presence of both tri- and tetravalent Ce, contrary to formulation, was confirmed using X-ray absorption near edge spectroscopy, suggesting substitution on both Ca and Zr sites. Sintering was carried out via spark plasma sintering, during which the perovskite phase (Ca_0.4Ce_0.4TiO₃) was stabilized due to the reducing conditions of this technique. Scanning electron microscopy and energy dispersive spectrometry revealed that the 2M polymorph was dilute in Ce content in comparison to the 4M-zirconolite. High temperature X-ray diffraction was used to detail the kinetics of perovskite to zirconolite transition. It was found that CaCeTi₂O₇ (cubic pyrochlore) formed as an intermediate phase during the transition. Lastly, our results show that a transition from 2M- to 4M-zirconolite occurs with increasing Ce content and can be controlled by adjusting the P_O2 and the heat treatment temperature.

Authors:

Clark, Braeden M. ^[1]; Sundaram, S. K. ^[1]; Misture, Scott T. ^[1]

Alfred Univ., Alfred, NY (United States)

Publication Date:: Wed Jul 19 00:00:00 EDT 2017

Research Org.:: Alfred University, Alfred, NY (United States)

Sponsoring Org.:: USDOE

OSTI Identifier:: 1393199

Resource Type:: Accepted Manuscript

Journal Name:: Scientific Reports

Additional Journal Information:: Journal Volume: 7; Journal Issue: 1; Journal ID: ISSN 2045-2322

Publisher:: Nature Publishing Group

Country of Publication:: United States

Language:: English

Subject:: 36 MATERIALS SCIENCE

Citation Formats


                    Clark, Braeden M., Sundaram, S. K., and Misture, Scott T. Polymorphic Transitions in Cerium-Substituted Zirconolite (CaZrTi2O7).  United States: N. p., 2017. 
Web.  doi:10.1038/s41598-017-06407-5.

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                    Clark, Braeden M., Sundaram, S. K., & Misture, Scott T. Polymorphic Transitions in Cerium-Substituted Zirconolite (CaZrTi2O7).  United States.  https://doi.org/10.1038/s41598-017-06407-5

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                    Clark, Braeden M., Sundaram, S. K., and Misture, Scott T. Wed .  
"Polymorphic Transitions in Cerium-Substituted Zirconolite (CaZrTi2O7)".  United States.  https://doi.org/10.1038/s41598-017-06407-5.  https://www.osti.gov/servlets/purl/1393199.

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@article{osti_1393199,

  title        = {Polymorphic Transitions in Cerium-Substituted Zirconolite (CaZrTi2O7)},

  author       = {Clark, Braeden M. and Sundaram, S. K. and Misture, Scott T.},

  abstractNote = {Compounds with the formulae CaZr1–xCexTi2O7 with x = 0.1–0.5 were synthesized by solid state reaction. Cerium was used as a surrogate for actinide elements. A transition from the 2M polymorph to the 4M polymorph (expanded unit cell due to cation ordering) in zirconolite was observed with increasing cerium content. The presence of both tri- and tetravalent Ce, contrary to formulation, was confirmed using X-ray absorption near edge spectroscopy, suggesting substitution on both Ca and Zr sites. Sintering was carried out via spark plasma sintering, during which the perovskite phase (Ca0.4Ce0.4TiO3) was stabilized due to the reducing conditions of this technique. Scanning electron microscopy and energy dispersive spectrometry revealed that the 2M polymorph was dilute in Ce content in comparison to the 4M-zirconolite. High temperature X-ray diffraction was used to detail the kinetics of perovskite to zirconolite transition. It was found that CaCeTi2O7 (cubic pyrochlore) formed as an intermediate phase during the transition. Lastly, our results show that a transition from 2M- to 4M-zirconolite occurs with increasing Ce content and can be controlled by adjusting the PO2 and the heat treatment temperature.},

  doi          = {10.1038/s41598-017-06407-5},

  journal      = {Scientific Reports},

  number       = 1,

  volume       = 7,

  place        = {United States},

  year         = {Wed Jul 19 00:00:00 EDT 2017},

  month        = {Wed Jul 19 00:00:00 EDT 2017}

}

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Works referencing / citing this record:

Phase analysis and reduction behaviour of Ce dopant in zirconolite
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Kaur, Rajveer; Gupta, M.; Kulriya, P. K.
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Similar Records

Title: Polymorphic Transitions in Cerium-Substituted Zirconolite (CaZrTi2O7)

Abstract

Citation Formats

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Oxygen migration in A2B2O7 pyrochlores journal, April 2001

Solid solution limits in synroc zirconolite journal, January 1983

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The solubility of cerium in La2Ti2O7 by DFT + U calculations journal, November 2015

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Feasibility Limits in Using Cerium as a Surrogate for Plutonium Incorporation in Zircon, Zirconia and Pyrochlore journal, January 2000

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Zirconolite transformation under reducing conditions journal, November 1998

The incorporation of plutonium and neptunium in zirconolite and perovskite journal, June 1998

Waste Immobilization in Glass and Ceramic Based Hosts book, April 2010

Study of cerium solubility in Gd2Zr2O7 by DFT+U calculations journal, December 2011

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Solid solution of metal oxides in the zirconolite phase CaZrTi2O7. II: The ternary phase CaZrxTi3−xO7 journal, July 1992

Conduction in polar crystals. I. Electrolytic conduction in solid salts journal, January 1938

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Title: Polymorphic Transitions in Cerium-Substituted Zirconolite (CaZrTi₂O₇)

The Incorporation of Cerium in Zirconolite
journal, January 1996

Oxygen migration in A2B2O7 pyrochlores
journal, April 2001

Solid solution limits in synroc zirconolite
journal, January 1983

Zirconolite-Rich Ceramics for Actinide Wastes
journal, January 1994

The solubility of cerium in La2Ti2O7 by DFT + U calculations
journal, November 2015

Defects and diffusion in pyrochlore structured oxides
journal, October 1998

The Preparation of PuP ₂ O ₇ and PuPO ₄ ¹
journal, December 1957

Feasibility Limits in Using Cerium as a Surrogate for Plutonium Incorporation in Zircon, Zirconia and Pyrochlore
journal, January 2000

Synthesis of (Ca,Ce3+,Ce4+)2Ti2O7: a pyrochlore with mixed-valence cerium
journal, May 2005

Zirconolite transformation under reducing conditions
journal, November 1998

The incorporation of plutonium and neptunium in zirconolite and perovskite
journal, June 1998

Waste Immobilization in Glass and Ceramic Based Hosts
book, April 2010

Study of cerium solubility in Gd2Zr2O7 by DFT+U calculations
journal, December 2011

Low-temperature reactive hot-pressing of cerium-doped titanate composite ceramics and their aqueous stability
journal, April 2014

Solubility of Ce4+ and Sr2+ in the pyrochlore lattice of Gd2Zr2O7 for simulation of Pu and alkaline earth metal
journal, January 2006

Effects of self-radiation damage in Cm-doped Gd2Ti2O7 and CaZrTi2O7
journal, April 1986

Large-volume atmosphere-controlled high-temperature x-ray diffraction furnace
journal, June 2003

The oxygen positional parameter in pyrochlores and its dependence on disorder
journal, January 2002

Solid solution of metal oxides in the zirconolite phase CaZrTi2O7. II: The ternary phase CaZrxTi3−xO7
journal, July 1992

Conduction in polar crystals. I. Electrolytic conduction in solid salts
journal, January 1938

Molecular dynamics simulation of the α-recoil nucleus displacement cascade in zirconolite
journal, November 2002

Self-propagating high-temperature synthesis of CeO2 incorporated zirconolite-rich waste forms and the aqueous durability
journal, October 2015

Swelling induced by alpha decay in monazite and zirconolite ceramics: A XRD and TEM comparative study
journal, May 2014

Immobilisation of high level nuclear reactor wastes in SYNROC
journal, March 1979

The durability of synroc
journal, August 1992

Analysis and Structural Determination of Nd-Substituted Zirconolite-4M
journal, March 1997

A DFT+U study of cerium solubility in La2Zr2O7
journal, May 2012

Phase analysis and reduction behaviour of Ce dopant in zirconolite
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Synchrotron x‐ray spectroscopy investigation of the Ca _{1− x} Ln _x ZrTi _{2− x} (Al, Fe) _x O ₇ zirconolite ceramics (Ln = La, Nd, Gd, Ho, Yb)
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