The departure process of residual Ga in diamond-like carbon (DLC) film synthesized by focused-ion-beam chemical vapor deposition (FIB-CVD) was investigated by measuring Rutherford backscattering (RBS) spectra of FIB-CVD DLC films after heat treatment in various conditions. The annealing temperature and annealing time were varied in the range of 473-973 K and 0-64 h, respectively. The decrease in Ga concentration and transfer of Ga in the FIB-CVD DLC film were not observed due to heat treatment at less than 573 K. The transfer of residual Ga from inside the film to the surface, and the formation of Ga spheres, which were surrounded by a graphite shell, were observed after heat treatment at 673 K, but Ga concentration did not vary much. When the annealing temperature was higher than 773 K, a decrease in the Ga concentration was observed. The depth profile of Ga in the DLC film in the RBS spectra was observed to divide into two peaks when treated with heat at temperatures higher than 673 K. This splitting can be interpreted as the difference in the desorption rate of Ga in the DLC, graphite shell, and Si substrate.