A plasma analysis system comprised of Omni-λ300 series grating spectrometer, CCD data acquisition system and optical fiber transmission system was utilized in the present paper to realize the real-time acquisition of plasma emission spectra during the process of radio frequency (RF) magnetron sputtering. The plasma emission spectra produced by NiTa, TiAl ceramic targets and NiAl, TiAl alloy targets were monitored respectively, in addition, the behavior of analysis lines of TaⅡ333.991 nm, NiⅠ362.473 nm, AlⅠ396.153 nm and TiⅠ398.176 nm with time was obtained, according to which the time of pre-sputtering of the four kinds of target materials was fixed. At the same time, for the TiAl alloy target as the research object, the influence of different powers and pressures on the time of pre-sputtering was studied.