The distribution of Ni in four lateritic Ni-goethites that were rapidly dehydroxylated to form hematite by shock heating at 340/400°C and 800°C for 30 min was investigated using synchrotron X-ray diffraction (SXRD), TEM spectroscopy (EELS and EFTEM) and synchrotron X-ray absorption spectroscopy (XAS). The Ni K-edge EXAFS results for non-heated samples showed three distinct Ni–Fe shells, including two edge-sharing (R Ni–Fe ∼ 3.01 and R Ni–Fe ∼ 3.22 Å) and a double corner-sharing (R Ni–Fe ∼ 3.52 Å) complex for most of the samples. These interatomic distances are indicative of Ni substituting for Fe in goethite, which has resulted in an expansion in the goethite structure along the a-axis direction and a contraction along the b-axis direction. Ravensthorpe Ni goethite was considerably different from the other goethites, with two Ni–O interatomic lengths (R Ni–O ∼ 2.04 and 2.46 Å), an edge-sharing (R Ni–Fe ∼3.04 Å) and a corner-sharing (R Ni–Fe ∼ 3.56 Å) complex. The R Ni–O ∼ 2.46 Å bond length is not indicative of Ni substituting for Fe in goethite, nor is it associated with single or multiple scattering events in NiO, Ni(OH)2 or Ni substituting for Fe in Fe oxides. The corresponding Ni K-edge EXAFS results for 340/400°C and 800°C heated samples (i.e. hematite) were very similar. Four distinct metal neighbours correspond to Fe/Ni in face-sharing (R Ni–Fe ∼ 2.87–2.91 Å) and three different corner-sharing complexes (R Ni–Fe ∼ 3.37– 3.41 Å, R Ni–Fe ∼ 3.62– 3.64 Å and R Ni–Fe ∼ 3.92– 4.09 Å) represent Ni substituting for Fe in hematite. The fourth shell is indicative of an inner sphere surface complex. EFTEM maps for Ni in goethite are consistent with the formation of a surface complex as they provide evidence for clustering of Ni on the surface of neoformed hematite crystals. There was no evidence from EXAFS or SXRD supporting the formation of discrete Ni phases (e.g. NiO) as a result of shock heating. Therefore, for Ni-goethites subjected to shock heating at 800°C (i.e. high-temperature dehydroxylation to hematite), most of the Ni is retained in the structures of the neoformed hematites, whereas some of the Ni migrates to the surface of the neoformed hematite where it forms a surface complex. During acid dissolution (e.g. heap leaching) of oxide-type lateritic Ni ores, Ni on the hematite surface is more accessible to acid solutions; therefore, these results may provide a basis for more efficient extraction methods for Ni in oxide-type lateritic Ni ores, as well as providing information on the possible redistribution of Ni in heated goethite-rich soils.
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