The dynamics of magnetic ordering in a natural hemo-ilmenite solid solution

We investigated the micromagnetic properties of hemo-ilmenite particles in an alluvial soil. All magnetic accessory minerals except the weathering resistant hemo-ilmenite grains were removed from the soil matrix by chemical treatment with concentrated acid followed by magnetic separation. X-ray diffraction revealed hemo-ilmenite grains with single crystal properties and an ilmenite mole fraction of y D 0.86. Magnetization versus applied magnetic field plots in a temperature range between 6 and 300 K were recorded in order to study the hysteresis and the exchange properties. In addition, field and frequency-dependent AC susceptibility measurements were performed with and without a DC bias field in order to analyse the dynamic magnetization of the sample down to 3 K. The hemo-ilmenite particles are considered as a mixed system with nano-sized cation-ordered areas (COA) and cation-disordered areas (CDA), which differ in their local Fe-(III) concentration. Ferrimagnetic single-domain order in the Fe-(III)-enriched CDA started at about 220 K. Upon cooling gradual transdomain transformation generates multidomain order. A maximum in the blocking distribution was reached at 44 K, followed by the onset of spin-glass dynamics. At lower temperature, blocking of superparamagnetic clusters in the COA created antiferromagnetic (AFM) ordering, which became more prominent with decreasing temperature. The interaction between the spin-glass like CDA and the AFM areas was documented by the onset of exchange bias at T < 20 K. The occurrence of exchange bias as well as spin-glass dynamics in the hemo-ilmenite grains is probably an effect of the inhomogeneity of the local Fe-(III) concentration. This effect leaves a magnetically competitive regime with areas showing ilmenite-like magnetic properties, and Fe-(III) rich disordered areas with magnetic long-range ordering up to 220 K and frustration near the ordering temperature of ilmenite.