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MoO3 is now utilized as a promising catalyst due to its high activity and favorable mobility at low temperature. Its spectral data and surface microstructures were characterized by Fourier transform infrared spectra (FT-IR) and Field emission scanning electron microscope (FESEM). Thermo-analysis of the carbon black was performed over nano-MoO3 catalyst in a thermogravimetric analyzer (TGA) at various heating rates and soot-catalyst ratios. Through the analysis of kinetic parameters, we found that the heat transfer effect and diffusion effect can be removed by setting lower heating rates and soot-catalyst ratios. Therefore, a strategy for selecting proper thermogravimetric parameters were established, which can contribute to the better understanding of thermo-analytical process.