A new approach to the analysis of carbon-containing materials by the method of secondary ion mass spectrometry is studied, which allows one to determine the concentration of carbon atoms in the states of sp2 and sp3 hybridization. It is proposed to use the ratio of the intensities of cluster secondary ions C8/C7 as the main parameter of the mass spectra of secondary ions characterizing the concentration of N(sp3). From measurements of several test structures, a calibration dependence of N (sp3) on the C8/C7 ratio was obtained. The N(sp3) profiles of diamond-like carbon samples grown on diamond and silicon substrates were measured, showing an N(sp3) concentration of 0.3 to 0.6 for different growth modes and an inhomogeneous distribution of the N(sp3) concentration over the thickness of the samples.

New possibilities offered by the method of secondary ion mass spectrometry (SIMS) for analysis of the phase composition of carbon-containing materials are considered. Differences are established between the mass spectra of three carbon phases: diamond, diamond-like carbon (DLC), and graphite. A simple algorithm for the quantitative determination of different phases in two-phase systems diamond–graphite and DLC–graphite is proposed that is based on the measurement of relative intensities of secondary cluster ions such as C_8/C_5 and CsC_8/CsC_4. It is shown that nonuniform depth profiles of various carbon phases are formed in diamond structures upon laser cutting and in DLC structures upon thermal annealing.