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This paper reports the successful synthesis and formation of nanoparticle forsterite powder by mechanical activation and its subsequent annealing. Talc and magnesium carbonate were used as basic starting reactants. Simultaneous thermal analysis (STA), X-ray diffraction (XRD), scanning electron microscopy (SEM), dynamic light scattering (DLS), atomic absorption spectrometry (AAS) and Fourier transform infrared spectroscopy (FT-IR) techniques were utilized to characterize the as-milled and annealed samples. The results showed that forsterite was not produced directly and that the formation of enstatite was unavoidable during the synthesis of forsterite. The nanoparticle forsterite powder obtained had a crystallite size of 30nm and mean particle size of 135nm after 10h milling and subsequent annealing at 1000°C for 10min.