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We have studied the effects of using water containing micro–nano-bubbles (MNB water) as the solution in which the diamond abrasives with a mean diameter of 0.5 μm are dispersed for the polishing slurry used in the precise mechanical polishing (PMP) of brittle material of GaN. While the formation of small number of clusters of abrasives was seen in the MNB water, the abrasives were basically well dispersed, which were almost comparable to that in pure water with a dispersion agent such as ethylene glycol. Since flocculation was observed for dispersion in pure-water without the addition of the dispersion agent, it was found that MNBs have dispersion effect for micro-sized abrasive particles. Regarding the polishing properties of GaN substrate with the MNB water based polishing slurry, we observed a remarkable increase in the removal rate with no additional surface or subsurface degradation. Additionally, we observed a significantly reduced subsurface damage (SSD) for chemically weak N-face of GaN substrate. It was suggested that these observed effects were most probably a result of the cluster formation in the MNB water and the chemical effect in relation to high energy generation through bubble collapse, respectively.

The relationship between the depth of the subsurface damage (SSD) and the size of the diamond abrasive used for mechanical polishing (MP) of GaN substrates was investigated in detail. GaN is categorized as a hard, brittle material, and material removal in MP proceeds principally to the fracture of GaN crystals. Atomic force microscopy and cathodoluminescence imaging revealed that the mechanical processing generated surface scratches and SSD. The SSD depth reduced as the diamond abrasive size reduced. A comparison of the relationship between the SSD depth and the diamond abrasive size used in the MP of GaN with the same relationship for typical brittle materials such as glass substrates suggests that the MP of GaN substrates proceeds via the same mechanism as glass.

The possibility of chemical mechanical polishing (CMP) as an intermediate ex-situ surface planarization process for thin-film epitaxy devices has been investigated. The surface quality of the homoepitaxial GaN after a surface pretreatment of CMP on the GaN-on-sapphire template drastically improved as compared to that with the regular homoepitaxial process. In addition, it was found that CMP contributed to a reduction in the dislocation densities in the subsequent homoepitaxial GaN layers. The CMP-treated GaN surface exhibited pits, with an average diameter of 0.3 μm, due to the chemical etching effect of the CMP slurry. These pits are thought to enhance the epitaxial lateral over growth of the GaN thin films, leading to a reduction in the dislocation densities in the homoepitaxial GaN layers.

Patterned sapphire substrate (PSS) was fabricated by wet etching solutions with different mixture ratios of H2SO4 to H3PO4 and different temperatures to investigate the fabrication mechanisms. It was found that the mixture ratio and temperature of the etching solutions affect the ratio of the pattern diameter to the pattern depth. In addition, the observed pattern shape was strongly affected by the mixture ratio. To discuss the reaction mechanisms of sapphire with H2SO4 and H3PO4 separately, we estimated the activation energies and reaction frequency factors for each reaction. By the estimated results, the behavior of the observed pattern shape for the etching conditions was well explained. To confirm the fabrication mechanism of pattern shape in the microscopic scale, the electron probe microanalysis (EPMA) inspection of the sapphire surface after H2SO4 and H3PO4 etching were carried out. As a result, it was indicated that the pattern shape is controlled by the step flow reaction with and without impurities in the etching solutions. From the observation of the pattern shape, the estimation of the activation energies and reaction frequency factors, and EPMA inspection of the reaction products for each reaction, a schematic model of the fabrication mechanisms for the wet etching of a PSS was established.

Processing by a laser beam focused within the substrate is used to control the initial bowing of sapphire substrates for III-nitride epitaxy. The process modifies the sapphire crystallinity at and near the focal area from single crystal to an amorphous phase. As volume expansion occurs inside the sapphire, strain is generated and, consequently, changes in the bowing. By controlling the focal depth and process pitch, we demonstrate a ∼250 μm pre-bowed sapphire substrate while only ±15 μm of bowing control is possible with a regular wafering process. We also demonstrate epitaxial growth of III-nitride on the pre-bowed sapphire substrates by metal organic chemical vapor deposition (MOCVD), which suggests an enlargement for the process window for III-nitride epitaxy on sapphire substrate. It is also shown that the pre-bowing by laser treatment functions to improve the crystal quality of grown III-nitride films.

The successful growth of 2-in. β-Ga2O3 crystals by the edge-defined, film fed growth (EFG) method was demonstrated. The optimization of growth conditions for larger single crystalline β-Ga2O3 is discussed in detail. The seeding conditions of temperature and neck width were found to be the most important factors to grow single crystals. X-ray rocking curve measurements of β-Ga2O3 crystals were conducted to estimate the dislocation densities of the grown crystals. Etch pit densities (EPDs) of the β-Ga2O3 crystals were also measured using KOH solution to measure the dislocation densities. The results were discussed combining with crystal growth parameters such as neck width to clarify the mechanisms of propagation and the origin of dislocations in crystals from phenomenological and crystallographic points of view.

We review a new approach to the bowing management of sapphire substrates for III-nitride epitaxy based on the internally focused laser processing. The laser process modifies the phase of the sapphire, inducing a volume expansion effect that enables the bow to be managed. Bowing control is required in two main areas: 1) control of the initial bow of the sapphire substrate, and 2) reduction in the bow after the epitaxy. The initial bow control was demonstrated for ~250 μm pre-bowed convex and concave sapphire substrates. The effect of the pre-bowed substrate on III-nitride epitaxy was also experimentally verified with an in situ curvature monitoring system during the III-nitride epitaxy; the possibility to accommodate substrate bowing to any target values by applying the initial offset to the substrate was also confirmed. When applied to the substrate after the epitaxy, the same technique was successful in flattening of the substrate for a subsequent chip-fabrication process. This new approach provides wide flexibility in the design engineering of epitaxial and device fabrication processes. Thus, it accelerates the realization of larger diameter device processes with III-nitride/sapphire.

High-quality thick GaN layers were directly grown by hydride vapor phase epitaxy on sapphire substrates preliminary processed by a laser beam focused within the substrate. The critical thickness for crack generation was improved drastically from 10–20 µm for regular substrates to 220–250 µm by using the laser processed sapphire substrates. Layers of 200 µm thickness grown on the laser processed sapphire substrates exhibited a crack-free surface over the entire 2-in. area and a threading dislocation density as low as 1×107 cm-2, which is one order of magnitude lower than that achievable with a regular sapphire substrate.

The importance of the atomically well-controlled surface of sapphire substrate with slight misorientation and ideally minimized surface roughness for III–nitride epitaxy is discussed in detail. An atomically controlled surface of sapphire substrate with slight misorientation angle is modeled and an almost ideal level of atomic surface roughness of sapphire substrate is found to be obtained by a chemical mechanical polishing (CMP) with colloidal silica. Cathodoluminescence (CL) imaging indicated the complete absence of subsurface damage induced by mechanical polishing. GaN and AlN thin films are grown on misoriented sapphire substrate with an atomically controlled surface by the CMP to investigate the misorientation angle of both sapphire and grown GaN and AlN thin films. An interface model is proposed to explain the difference in misorientation angle between sapphire and III–nitride thin films, providing strong evidence of the necessity of atomically controlled surface of sapphire substrate for III–nitride epitaxy.

Reduction of the bowing of GaN-on-sapphire and GaN-on-silicon substrates was demonstrated with an internally focused laser processing. Stress implantation was successfully achieved inside the sapphire and silicon substrates by the internally focused laser process to compensate for the strain generated by the GaN/sapphire and GaN/Si systems which resulted in substrate bow reduction. This new approach gives us a larger flexibility in the design engineering of epitaxial and device fabrication processes and thus accelerates the realization of a larger diameter device process with GaN-on-sapphire and GaN-on silicon.