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The goal of the paper is to study the charge transfer and reactions at the columbite-(Fe) (FeNb2O6) mineral surface during the HF leaching process. In this paper, X-ray photoelectron spectroscopy (XPS), leaching experiments, and density functional theory (DFT) calculations were used to study the surface element adsorption, charge distribution, chemical state, and energy changes of the mineral surface during the process of leaching columbite–(Fe) with different concentrations of hydrofluoric acid. The results showed that as the concentration of F atoms was increased during the acid leaching process, the Nb–O bond was more likely to be broken than the Fe–O bond; the amount of charge transferred from Nb atom to F atom (0.78 e–0.94 e/atom) was greater than that from Fe atom to the F atom (0.25 e–0.28 e/atom), so it was determined that compared to Fe atoms, it was easier for the Nb atoms to bind to F. The results of XPS analysis showed that the electron binding energies of Nb5+–O, Fe3+–O, and Fe2+–O bonds on the mineral surface increased sequentially, and the M–O bond broke during the acid leaching process, forming more stable M–F bonds. Therefore, the Nb5+–F bonds were easier to form a stable structure. Combined with the ICP results, it was found that in the filtrate after 5M HF and 10M HF acid leaching minerals, c(Nb)/c(Fe) were 2.69 and 2.95, respectively, and the concentration ratio of Nb to Fe element in the mineral was 2 which was lower than 2.69 and 2.95, confirming the result of DFT calculation and illustrating that Nb atoms in columbite-(Fe) mineral were more soluble than Fe atoms.

Interfacial Structure Change and Selective Dissolution of Columbite–(Fe) Mineral during HF Acid Leaching