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The purpose of this study was to develop a rapid and green method for the synthesis of biomass-based materials. A microwave-assisted method was used for the preparation of CaCO3 particles-filled wood powder nanocomposites, which involve natural cellulosic materials, CaCO3, and microwave heating. Dewaxed wood powder was pretreated in the NaOH/urea solution. The urea acts as part of the CO32− source and provides a basic condition for the synthesis of CaCO3. The influences of reaction parameters such as the heating time and the addition of (NH4)2SO4 on the products were investigated by X-ray powder diffraction (XRD), Fourier transform infrared spectrometry (FTIR), scanning electron microscopy (SEM), thermogravimetric analysis (TGA), and differential thermal analysis (DTA). The experimental results demonstrated that the heating time had an effect on the crystallinity and morphology of the nanocomposites. In addition, the presence of (NH4)2SO4 played an important role in the morphology and dispersion of CaCO3 in the nanocomposites.