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<p>Yttria (Y<sub>2</sub>O<sub>3</sub>) is a refractory ceramic of great technological importance. The material with a stable cubic crystal structure transforms into a monoclinic phase when ball-milled under specific conditions. The synthesis methodology can be engineered to have mixed phase (cubic + monoclinic) Y<sub>2</sub>O<sub>3</sub>. Scanning transmission electron microscopy (STEM)-based electron energy-loss spectroscopy (EELS) is an elegant method to characterize these phases. This paper provides an experimental methodology to use the electron energy-loss near-edge structure (ELNES) of oxygen (O) K-edge as a fingerprint to uniquely identify the phases. The spectrum so obtained was corroborated with simulated patterns. The distortion of the octahedral network of O in the cubic-Y<sub>2</sub>O<sub>3</sub> structure crafts a monoclinic structure and this is manifested as a reduction in peak separation (ΔE) at the O K<sub>1</sub> and K<sub>2</sub>—edges as compared to the same for the higher symmetry cubic structure. The unique insight provided by the O K-edge EELS is discussed in the context of phase identification and may be extended to rare-earth oxide polymorphs.</p> Graphical Abstract <p></p>

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Characterization of Cubic and Monoclinic Phases in Ball-Milled Nanocrystalline-Y2O3 Using Experimental and Simulated Oxygen K-Edge Positions in STEM-EELS

  • 期刊论文

  • 出版模式：

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  • 发表日期：

    2025年6月28日

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  • B. R. Vaishnavi Krupa,
  • Akhil G. Nair,
  • Chanchal Ghosh,
  • Anindya Bhattacharyya,
  • Arup Dasgupta,
  • R. Divakar

摘要

Yttria (Y2O3) is a refractory ceramic of great technological importance. The material with a stable cubic crystal structure transforms into a monoclinic phase when ball-milled under specific conditions. The synthesis methodology can be engineered to have mixed phase (cubic + monoclinic) Y2O3. Scanning transmission electron microscopy (STEM)-based electron energy-loss spectroscopy (EELS) is an elegant method to characterize these phases. This paper provides an experimental methodology to use the electron energy-loss near-edge structure (ELNES) of oxygen (O) K-edge as a fingerprint to uniquely identify the phases. The spectrum so obtained was corroborated with simulated patterns. The distortion of the octahedral network of O in the cubic-Y2O3 structure crafts a monoclinic structure and this is manifested as a reduction in peak separation (ΔE) at the O K1 and K2—edges as compared to the same for the higher symmetry cubic structure. The unique insight provided by the O K-edge EELS is discussed in the context of phase identification and may be extended to rare-earth oxide polymorphs.

Graphical Abstract