The stress distribution in bulk AlN crystals seeded on 6H-SiC was theoretically modeled and also determined experimentally from Raman peak positions. The full width at half maximum of the AlN Raman peaks showed the crystal quality improved as its thickness increased. The theoretical frequency shifts of the E 1 ͑transverse optical͒ mode calculated from model-predicted stress were in good agreement with experimental values taken along the edges of crystal samples. The stress was linearly distributed along the depth of the samples, and changed from compressive at the growing surface to tensile at the interface between AlN and SiC for thickness range of several hundred micrometers. Large tensile stresses, up to 0.6 GPa, were detected in the AlN at the interface. The effects of growth temperature and sample thickness were investigated. It is predicted that the AlN on 6H-SiC must be at least 2 mm thick to prevent it from cracking while cooling down the sample from a growth temperature of 2000°C.
Anisotropic chemical etching is an important means for characterizing the polarity and defect density of single crystals. In this letter, we present the results of our studies on the etching of bulk AlN crystals in aqueous potassium hydroxide solution. The nitrogen polarity (0001) basal plane initially etched rapidly, while the aluminum polarity basal plane, and prismatic (1100) planes were not etched. The etch rate of the nitrogen polarity basal plane eventually decreased to zero, as the surface became completely covered with hexagonal hillocks which were bounded by {1101} planes. The hillock density for the self-seeded AlN crystals studied was typically in the range of 5 × 10 7 cm -2 to 10 9 cm -2 . From our analysis of etched AlN crystals, we infer that freely nucleated crystals predominately have the nitrogen to aluminum direction pointing out from the nucleation surface, that is the ends of the AlN crystals facing the source are aluminum polarity.
Single crystalline platelets of aluminum nitride (AlN) were successfully grown by a new technique. It consists of (1) depositing an AlN buffer layer on a SiC substrate by metal organic chemical vapor deposition (MOCVD) below 1100°C, (2) forming an (AlN)x(SiC)1−x alloy film on the AlN film by condensing vapors sublimated at a temperature of 1800°C from a source mixture of AlN-SiC powders, followed by (3) condensing vapors sublimated from a pure AlN source (at 1800°C). The necessity of the first two steps for the successful AlN sublimation growth on SiC substrate was illustrated by the initial nucleation studies of alloys on SiC substrates with and without MOCVD AlN buffer layers: an AlN MOCVD buffer layer leads to continuous, single grain growth mode; The (AlN)x(SiC)1−x alloy film reduces the crack density because its thermal expansion coefficient is intermediate between SiC and AlN. X-ray diffraction (XRD) and Raman spectroscopy studies indicated the high quality of the AlN single crystal.
The effect of substrate preparation on the sublimation growth of AlN at about 1800 °C and 400 torr on (0001) 6H-SiC was investigated. The AlN grew in the step flow growth mode on an off-axis 6H-SiC substrate with a 6H-SiC epilayer, an island growth mode on as-received substrates, and a 2-D growth mode on substrates first coated with an AlN epitaxial layer by MOCVD. Cracks in the deposited AlN crystal due to the lattice and thermal expansion coefficient mismatches were always observed by SEM and optical microscopy.
The morphology and composition of AlN crystals on 6H-SiC (0001) at the initial stage of crystal growth by sublimation re-condensation technique were investigated by SEM and SAM. Discontinuous AlN coverage occurred after 15 minutes growth. The AlN nuclei size, and growth rate increased as temperature increased or pressure decreased. The SiC substrate decomposed leaving hexagonal hillocks; simultaneously, the AlN nucleated on these SiC hillocks apparently rotated by 15° to 30°. The chemical composition of the substrate and different AlN crystal facets were characterized by SAM. The bare substrate area was stoichiometric SiC with insignificant conversion to silicon nitride, while Si and C preferentially incorporated in the AlN at the initial stages of growth on specific crystal planes.
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