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Combustion-derived synthesis of nanostructured copper oxide (CuO) materials was synthesized by oxalic acid as a fuel, and copper nitrate as an oxidant. The combustion product showed mixed phases of CuO and Cu 2 O. The pure nanocrystalline CuO phase was obtained upon subsequent annealing of the combustion product at 700 °C for 3 h, whereas the planetary ball-milling of the combustion product at 300 rpm for 10 h yielded CuO phase with two weak peaks of Cu 2 O phase. The microstructural and optical properties of CuO nanomaterials were explored by X-ray diffraction (XRD), field emission scanning electron microscopy (FESEM), Fourier transform infrared (FT-IR), near infrared (NIR), and diffused reflectance spectroscopic (DRS) techniques. The annealed powder XRD pattern confirms that it crystallizes in a monoclinic C12/c1 (15) structure with lattice parameters: a = 0.4687( 4), b = 0.3419(3), c = 0.5128(4) nm, and β = 99° 39′ (4) with average crystalline size, D of 30.89 nm. The agglomeration of fine particles is seen for the ball-milled powder, while the annealed powder revealed different particle sizes in the range of 254 ~ 835 nm as evidenced from FESEM images. The NIR reflectance of (~ 45%) CuO powder (annealed) can be used as black pigments in color industries. The annealed CuO powder reveals narrow Raman peaks than ball-milled powder.

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