Recent results of GaN bulk growth performed in Poland are presented. Two technologies are described in detail: halide vapor phase epitaxy and basic ammonothermal. The processes and their results (crystals and substrates) are demonstrated. Some information about wafering procedures, thus, the way from as-grown crystal to an epi-ready wafer, are shown. Results of other groups in the world are briefly presented as the background for our work.
X-ray topography defect analysis of entire 1.8-inch GaN substrates, using the Borrmann effect, is presented in this paper. The GaN wafers were grown by the ammonothermal method. Borrmann effect topography of anomalous transmission could be applied due to the low defect density of the substrates. It was possible to trace the process and growth history of the GaN crystals in detail from their defect pattern imaged. Microscopic defects such as threading dislocations, but also macroscopic defects, for example dislocation clusters due to preparation insufficiency, traces of facet formation, growth bands, dislocation walls and dislocation bundles, were detected. Influences of seed crystal preparation and process parameters of crystal growth on the formation of the defects are discussed.
Photoluminescence (PL) from GaN substrates fabricated by the ammonothermal growth method was studied in a wide range of temperatures and excitation intensities, both with steady-state and time-resolved PL techniques. Three defect-related PL bands were detected: the ultraviolet luminescence band with the zero-phonon line at 3.27 eV, the Zn-related BL1 band with a maximum at 2.9 eV, and the yellow luminescence band (labeled YL2) with a maximum at 2.3 eV. The YL2 band belongs to an unknown defect and is different from the CN-related YL1 band. Its maximum blueshifts by 0.06 eV with increasing excitation intensity and redshifts by more than 0.1 eV with a time delay after a laser pulse. The YL2 band is preliminarily attributed to a defect complex containing the gallium vacancy.
In this paper, we investigate, using X-ray Bragg diffraction imaging and defect selective etching, a new type of extended defect that occurs in ammonothermally grown gallium nitride (GaN) single crystals. This hexagonal “honeycomb” shaped defect is composed of bundles of parallel threading edge dislocations located in the corners of the hexagon. The observed size of the honeycomb ranges from 0.05 mm to 2 mm and is clearly correlated with the number of dislocations located in each of the hexagon’s corners: typically ~5 to 200, respectively. These dislocations are either grouped in areas that exhibit “diameters” of 100–250 µm, or they show up as straight long chain alignments of the same size that behave like limited subgrain boundaries. The lattice distortions associated with these hexagonally arranged dislocation bundles are extensively measured on one of these honeycombs using rocking curve imaging, and the ensemble of the results is discussed with the aim of providing clues about the origin of these “honeycombs”.
The results of basic ammonothermal crystallization of gallium nitride are described. The material is mainly analyzed in terms of the formation of stress (called stress-induced polarization effect) and defects (threading dislocations) appearing due to a stress relaxation process. Gallium nitride grown in different positions of the crystallization zone is examined in cross-polarized light. Interfaces between native ammonothermal seeds and new-grown gallium nitride layers are investigated in ultraviolet light. The etch pit densities in the seeds and the layers is determined and compared. Based on the obtained results a model of stress and defect formation is presented. New solutions for improving the structural quality of basic ammonothermal gallium nitride crystals are proposed.