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This contribution reports on the synthesis and the main physical properties of p-type NiO nanoparticles synthesized for the first time by a completely green process using Agathosma betulina plant extract as an effective oxidizing/reducing agent. The surface/interface and volume room temperature properties by TEM, EDS, XRD, FTIR, Raman and photoluminescence as well as XPS are reported. Likewise, a standard blade made film of pressed n-type NiO nanoparticles onto p-type Silicon substrate of such nanoparticles exhibited a good photodiode response in the NIR spectral range.