Diamond film was deposited on the pure titanium substrate by CH4-H2 gas mixture using MPCVD method. In order to carboxylate the surface of the diamond film, it was chemically treated in H2SO4:HNO3 (9:1, case 1) stirred at room temperature or in H2SO4:HNO3 (3:1, case 2) stirred at reflux. The oxidized diamond film was successively treated with 0.1M NaOH for 2hours and 0.1M HCl at 363K for 2hours, and then washed by distilled water. The surface of diamond film was observed by scanning electron microscopy (SEM). The diamond film was characterized using Raman spectroscopy and X-ray diffraction (XRD). Carboxylated diamond film was evaluated by Fourier transform infrared spectrometer (FT-IR), Mini secondary ion mass spectrometer (Mini SIMS) and X-ray photoelectron spectroscopy (XPS). In the FT-IR spectrum, the peak at 1640cm -1 was assigned with C=O stretching vibration of carboxylic acid. In the Mini SIMS profile, the peak intensities of mass number 16 (-O-) and 17 (-OH) were increased after the chemical treatment. The XPS results indicated COO- group and C=O group on the surface of diamond film.