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It is described for the first time the synthesis and characterization of NiMn2O4 employing the Mn ores from the Amazon Region as starting material, instead of using commercial reagents as normally occurs in its synthesis process. Initially, an Mn ore was transformed into a single product, the octahedral layer (OL) manganese oxide with Ni2+ ions interlayer (Ni-OL-2), which was used as a matrix to obtain NiMn2O4 by thermal decomposition. The following techniques were used for characterization: X-ray diffraction (XRD), X-ray fluorescence spectroscopy (XRF), infrared spectroscopy (FTIR), thermal analysis (TG-DTA), scanning (SEM) and transmission (TEM) electron microscopies. The results revealed that Mn oxide ore composed of nsutite mineral transformed into a well-ordered crystalline Ni-OL-2 phase, after the hydrothermal and cation exchange process. The thermal decomposition of Ni-OL-2 produced the nickel manganite phase at 850 °C with spherical ball morphology and crystal sizes in the range of 200-300 nm.

Óxido hidróxido de manganês (γ - MnOOH) do tipo da manganita foi sintetizado por uma rota simples, em que a chave precursora K-birnessita foi preparada pelo método sol-gel. O tratamento hidrotermal da estrutura lamelar do tipo da birnessita favorece a obtenção de estruturas em túnel, sendo que o tamanho destes túneis depende das condições empregadas na síntese (pH, temperatura e tempo). A comprovação da formação de manganita sob as condições de síntese empregadas foi verificada pelas técnicas de difração de raios X, microscopia eletrônica de varredura, análises termogravimétrica e térmica diferencial e espectroscopia de infravermelho. Manganese oxyhydroxide (g - MnOOH) of the manganite type has been synthesized by a simple route with K-birnessite prepared by the sol-gel method. The hydrothermal treatment of the lamellar birnessite type structure facilitates the formation of tunnel structures where the size of the tunnels depends on the synthesis conditions (pH, temperature and time). The evidence of manganite formation under the synthesis conditions were made by X-ray diffraction, scanning electron microscopy, thermogravimetry, differential thermal analysis and infrared spectroscopy.