We examined the crystal and magnetic properties of the polymorphic LiFeO \(_2\) compound using Mössbauer spectra (MS), X-ray diffraction data (XRD), and magnetic measurements. X-ray diffraction analysis of \(\alpha\) -LiFeO \(_2\) and \(\beta '\) -LiFeO \(_2\) phases reveals that short-range ordering observed in the \(\alpha\) -LiFeO \(_2\) phase is potentially linked to the \(\beta '\) -LiFeO \(_2\) phase nanoregions. Low-temperature MS of the \(\alpha\) -LiFeO \(_2\) phase reveal a complicated disordered magnetic state below 90 K. Rietveld analysis of the XRD data of the \(\gamma\) -LiFeO \(_2\) phase reveals a defect microstructure. These defects produce a complicated distribution of the hyperfine magnetic field estimated from MS. While it is not possible to produce the \(\beta '\) -LiFeO \(_2\) phase in pure form, extended annealing of the \(\alpha\) -LiFeO \(_2\) phase at 400 \(^\circ\) C yields a nanocomposite material comprising nanoregions of both \(\beta '\) -LiFeO \(_2\) and \(\gamma\) -LiFeO \(_2\) phases.
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