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Ca3Co4O9 is a p-type semiconducting material that is well-known for its thermoelectric (TE), magnetic, electronic, and electro-optic properties. In this study, sol-gel autoignition was used to prepare Ca3Co4O9 at different calcination temperatures (773, 873, 973, and 1073 K) and time (4, 6, 8, 10, 12, and 14 h) using starch as a fuel. The phase and microstructure of the prepared Ca3Co4O9 powder were investigated. Thermogravimetry-differential thermal analysis (TGA) confirms that the final weight loss occurred at 1073 K to form Ca3Co4O9 stable powder. The variable-pressure scanning electron microscopy (VP-SEM) images show that the size of powder particles increases from 1.15 to 1.47 μm as calcination time increases from 4 to 12 h, and the size remains almost constant thereafter. A similar patt is also observed on the increment of the crystallite size and percentage of crystallinity with X-ray diffraction (XRD) analysis. The highest crystallinity is found about 92.9％ when the powder was calcinated at 1073 K for 12 and 14 h with 458 and 460 ? crystallite size, respectively. Energy dispersive X-ray spectroscopy (EDS) analysis demonstrates that the calcinated powder has a high intensity of Ca, Co, and O with uniform distribution. High-resolution transmission electron microscopy (HRTEM) images prove that there is no distinct lattice distortion defect on the crystal structure.