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Abstract: Insertion/extraction of lithium ions into/from Bi2Se3 crystals was investigated by means of cyclic voltammetry. The process of insertion is reflected in the appearance of two bands on voltammograms at ∼1.7 and ∼1.5V, corresponding to the insertion of Li+ ions into octahedral and tetrahedral sites of the van der Waals gap of these layered crystals. The process of extraction of Li+ ions from the gap results in the appearance of four bands on the voltammograms. The bands 1 and 2 at ∼2.1 and ∼2.3V correspond to the extraction of a part of Li+ guest ions from the octahedral and tetrahedrals sites and this extraction has a character of a reversible intercalation/deintercalation process. A part of Li+ ions is bound firmly in the crystal due to the formation of negatively charged clusters of the (LiBiSe2.Bi3Se4 −) type. A further extraction of Li+ ions from the van der Waals gap is associated with the presence of bands 3 and 4 placed at ∼2.5 and ∼2.7V on the voltammograms as their extraction needs higher voltage due to the influence of negative charges localized on these clusters. [ABSTRACT FROM AUTHOR]