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  5. Selective Synthesis of Defect-Rich LaMnO<sub>3</sub> by Low-Temperature Anion Cometathesis

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Article
en
2023

Selective Synthesis of Defect-Rich LaMnO<sub>3</sub> by Low-Temperature Anion Cometathesis

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en
2023
Vol 63 (7)
Vol. 63
DOI: 10.1021/acs.inorgchem.3c03305

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Gerbrand Ceder
Gerbrand Ceder

University of California, Berkeley

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Gia Thinh Tran
Allison Wustrow
Daniel O’Nolan
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Abstract

The synthesis of complex oxides at low temperatures brings forward aspects of chemistry not typically considered. This study focuses on perovskite LaMnO3, which is of interest for its correlated electronic behavior tied to the oxidation state and thus the spin configuration of manganese. Traditional equilibrium synthesis of these materials typically requires synthesis reaction temperatures in excess of 1000 °C, followed by subsequent annealing steps at lower temperatures and different p(O2) conditions to manipulate the oxygen content postsynthesis (e.g., LaMnO3+x). Double-ion exchange (metathesis) reactions have recently been shown to react at much lower temperatures (500-800 °C), highlighting a fundamental knowledge gap for how solids react at lower temperatures. Here, we revisit the metathesis reaction, LiMnO2 + LaOX, where X is a halide or mixture of halides, using in situ synchrotron X-ray diffraction. These experiments reveal low reaction onset temperatures (ca. 450-480 °C). The lowest reaction temperatures are achieved by a mixture of lanthanum oxyhalide precursors: 2 LiMnO2 + LaOCl + LaOBr. In all cases, the resulting products are the expected alkali halide salt and defective La1-ϵMn1-ϵO3, where ϵ = x/(3 + x). We observe a systematic variation in defect concentration, consistent with a rapid stoichiometric local equilibration of the precursors and the subsequent global thermodynamic equilibration with O2 (g), as revealed by computational thermodynamics. Together, these results reveal how the inclusion of additional elements (e.g., Li and a halide) leads to the local equilibrium, particularly at low reaction temperatures for solid-state chemistry.

How to cite this publication

Gia Thinh Tran, Allison Wustrow, Daniel O’Nolan, Songsheng Tao, Christopher J. Bartel, Tanjin He, Matthew J. McDermott, Brennan C. McBride, Karena W. Chapman, Simon J. L. Billinge, Kristin A. Persson, Gerbrand Ceder, James R. Neilson (2023). Selective Synthesis of Defect-Rich LaMnO<sub>3</sub> by Low-Temperature Anion Cometathesis. , 63(7), DOI: https://doi.org/10.1021/acs.inorgchem.3c03305.

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Publication Details

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Article

Year

2023

Authors

13

Datasets

0

Total Files

0

Language

en

DOI

https://doi.org/10.1021/acs.inorgchem.3c03305

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