Real-time synchrotron x-ray studies of low- and high-temperature nitridation of c-plane sapphire

The plasma nitridation kinetics of c-plane sapphire at both low (200-300 deg. C) and high (750 deg. C) substrate temperatures was examined using grazing-incidence real-time x-ray diffraction, in situ x-ray reflection and in situ reflection high-energy electron diffraction (RHEED). These monitored the evolution of the nitride thickness, strain, and surface structure during nitridation. The evolution of the AlN(1010) peak showed that the heteroepitaxial strain in the first layer of nitride is already significantly relaxed relative to the substrate. Subsequent layers grow with increasing relaxation. In both the high- and low-temperature nitridation cases, the results suggest that the early stage nitridation is governed by a complex nucleation and growth process. Nitridation at both temperatures apparently proceeds in a two-dimensional growth mode with the initial nucleating islands consisting of several monolayers which grow laterally. At low temperature the growth slows or even stops after impingement of the nucleating islands covering the surface, possibly due to low diffusivities through the existing layer. Initial formation and growth rates of nucleating islands at high temperatures are comparable to those at low temperatures, but subsequent growth into the substrate is significantly enhanced over the low temperature case, consistent with activation energies of 0.1-0.25 eV