Two different kinds of mullite precursors with composition 3Al2O3•2SiO2 (3:2) were prepared by conventional drying ethanol solution and spray-drying aqueous solution of aluminum nitrate nanohydrate and tetraethoxysilane, respectively. The results of scanning electron microscope (SEM) indicate that one powder consists of irregular particles with size of 1-10μm, the other powder is made of inhomogeneously sized hollow spherical particles with mean size of 0.5-5μm. The TG-DTA curves indicate the hollow spherical particles are unfavorable to eliminate the decomposed products. After the precursors were sintered by Spark Plasma Sintering at 1450°C for 10min, the microstructures of the former are made of fine equiaxed grains with sizes of around 0.5μm, the latter consist of elongated grains distributed in the matrix of fine grains with imhomogenous size of 0.5~10μm due to the liquid phase forming. The different microstructures lead to the former sintered body is transparent, while, the sample from spray-drying is opaque.