This work aimed to investigate the carbonaceous deposits on the surface of the coking chamber. Scanning electron microscopy (SEM), X-ray fluorescence spectrum (XRF), Fourier transform infrared spectrometer (FTIR), Raman spectroscopy, X-ray diffraction spectrum (XRD), and X-ray photoelectron spectroscopy (XPS) were applied to investigate the carbonaceous deposits. FTIR revealed the existence of carboxyl, hydroxyl, and carbonyl groups in the carbonaceous deposits. SEM showed that different carbonaceous deposit layers presented significant differences in morphology. XRF and XPS revealed that the carbonaceous deposits mainly contained C, O, and N elements, with smaller amounts of Al, Si, and Ca elements. It was found that in the formation of carbonaceous deposits, the C content gradually increased while the O and N elements gradually decreased. It was also found that the absorbed O2 and H2O took part in the oxidation process of the carbon skeleton to form the =O and −O− structure. The oxidation and elimination reaction resulted in change in the bonding state of the O element, and finally formed compact carbonaceous deposits on the surface of the coking chamber. Based on the analysis, the formation and evolution mechanisms of carbonaceous deposits were discussed.