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Understanding the Synthesis of Disordered Rock Salt (DRX) Disordered rock salt (DRX) oxides and oxyfluorides represent a promising class of cathode materials due to their exceptional compositional flexibility, including Ni- and Co-free variants that achieve capacities exceeding 250 mAh/g. For systems containing Mn and Ti (such as Li1.1Mn0.8Ti0.1O1.9F0.1), the former serves as the primary redox-active species, while the latter plays a stabilizing role by accommodating local distortions within the lattice. In situ synchrotron X-ray diffraction (XRD) reveals that DRX formation proceeds through multiple ordered rock-salt-related crystalline intermediates, beginning at 480 °C and homogenizing by 950–1000 °C. Complementary ex situ X-ray absorption spectroscopy (XAS) on quenched reaction intermediates show that Ti is incorporated into the DRX framework at lower temperatures than Mn (~700 °C vs. 950–1000 °C), highlighting how both in situ XRD and ex situ XAS are complementary measurement techniques to study the formation pathway of DRX.
Ti K-edge (a) Crystallographic structure of reaction intermediates (b) Weight fraction of precursors and intermediates formed during synthesis
Mn K-edge (a,b) Ti and Mn K-edge XAS spectra
Combining in-situ XRD during DRX synthesis with ex-situ XRD/XAS on quenched intermediates enables tracking of intermediate formation and final DRX framework, and reveals how temperature governs Transition Metal incorporation.
Source: Z. Liang et al (2025).
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