Mitigation Of Gadolinium Oxychloride Impurity During Co-precipitation Of Gadolinium Zirconate

Abstract

This study investigates the influence of precursor chemistry on impurity formation, phase evolution, and microstructural development in Gd₂Zr₂O₇ synthesized by co-precipitation. Use of ZrOCl₂ precursor resulted in the formation of a GdOCl impurity in powders calcined at 800 °C and subsequently sintered at 1500 °C. The GdOCl content increased from ∼4 vol% to ∼20 vol% with increasing precursor concentration. Washing of co-precipitates reduced but did not fully eliminate residual chlorine. Thermogravimetric analysis suggests the gradual removal of chlorine-containing species at elevated temperatures. Consistent trends observed from wavelength-dispersive X-ray fluorescence and Rietveld refinement are indicative of progressive chlorine removal and an associated shift toward stoichiometric Gd₂Zr₂O₇. Phase-pure gadolinium zirconate was achieved by increasing the calcination temperature to 1400 °C or by sintering at 1600 °C. The alternative use of a chloride-free precursor (ZrO(NO₃)₂) also avoids GdOCl impurity. These results highlight the influence of precursor chemistry on phase evolution and chemical homogeneity.

Department(s)

Materials Science and Engineering

Comments

Office of Naval Research, Grant N00014-24-1-2768

Keywords and Phrases

Co-precipitation synthesis; Rare-earth compounds; Spark plasma sintering

International Standard Serial Number (ISSN)

0921-5107

Document Type

Article - Journal

Document Version

Citation

File Type

text

Language(s)

English

Rights

© 2026 Elsevier, All rights reserved.

Publication Date

01 Nov 2026

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