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Monodisperse micro-nano nickel powders have been prepared by chemical reduction of aqueous solution NiSO₄, NaOH and NaH₂PO₂, and the influence of pH value and initial concentration of NiSO₄ on the size, structure, morphology and microwave absorption properties of nickel powders were investigated. The crystal structure of nickel powders was characterized by X-ray diffraction (XRD). And the morphology of the as-synthesized products was characterized by scanning electron microscopy (SEM) and transmission electron microscopy (TEM). The microwave absorption properties of the composite materials were characterized by network analyzer. The result indicates that the growth of nickel powders produced by NiSO₄ and NaH₂PO₂ at alkaline condition deeply relies on pH value and initial concentration of NiSO₄ in reaction system. Different sizes of nickel powders with the diameter of 1.5$\mu$m and 180nm were produced at the pH value of 10 and initial concentration of NiSO₄ at 0.5mol/L. The network analyzer showed definite microwave absorption properties of nickel powders with different sizes in the range of 0.5–18.0GHz.