Conditions favorable to the deposition of Si
3N
4 on pure steel substrates by means of an inductively coupled, externally heated plasma discharge were determined, and comparisons made with reducedpressure CVD. A push-pull Hartley RF (13.56MHz) oscillator with a maximum output of 70W was designed using a triode. The reactive gases-NH
3 and SiN
4-were diluted with Ar to a prescribed concentration. Test pieces of pure steel measuring 5×5×0.5mm were prepared, their surfaces were polished using diamond paste, and the Si
3N
4 was deposited onto the surfaces.
It was found that the optimum distance between the test pieces and the oscillator electrode was 25cm, and the optimum ratio of NH
3 and SiH
4 gases was 1:2.5. Investigating the effect of reaction temperature and deposition time under these conditions, it was found that in the case of plasma CVD, 800°C was a boundary value above which film thickness decreased, while the rate of film growth varied with deposition time depending on whether the reaction temperature was below or above 750°C. Comparison with reduced-pressure CVD indicated that this was due to the effect of Coulomb discharge, and it was found by differential thermal analysis and X-ray diffraction that in Si
3N
4 at 746°C or less, deposits were amorphous.
Further, at 800°C, film growth proceeded rapidly, reaching 12.5μm after 30min but thereafter decreased and was only 15μm after 240min. In reduced-pressure CVD, film growth proceeded linearly for 60min and thereafter almost linearly although with a decreased slope, reaching 12.5μm after 240min at 800°C.
Investigation of the apparent activation energy of the growth of the Si
3N
4 including a diffusion layer in the initial reaction period gave a value of 20kcal/mol at 750°C or less for plasma CVD, and 12 kcal/mol at 700-800°C for reduced pressure CVD.
抄録全体を表示