Comprehensive characterization of hydride VPE grown GaN layers and templates

GaN community has recently recognized that it is imperative that the extended, and point defects in GaN and related materials, and the mechanisms for their formation are understood. This is a first and an important step, which must be followed by defect reduction before full implementation of this material and its allied binaries/ternaries in devices. This review is based on a recent concerted effort to establish benchmarks as far as defects are concerned, and identify the basic issues involved. Samples were analyzed for extended defects by TEM and chemical etches, for polarity by electric force microscopy and convergent beam electron diffraction (CBED), for point defects by DLTS, for optical quality and deep defects by photoluminescence (PL), for vacancies by positron annihilation, for donor and acceptor like states within the gap by ODMR and EPR, and for carrier transport targeted for defects and impurities by variable temperature and magnetic field-dependent Hall measurements. Hydride VPE samples grown at Lincoln Laboratories with 1.5, 5.5 and 55 μm thicknesses were investigated for defects by TEM, and their polarity was found to be Ga-polarity, as expected, by CBDE combined with simulations. The density of misfit dislocations at the substrate/EPI interface was determined to be on the order of 10 13 cm -2 based on high-resolution electron microscopy images. The threading dislocation density decreased gradually with distance from the interface, reaching a value of about 10 8 cm -2 at the surface of a 55 μm film. A 200 μm thick laser separated and free-standing HVPE grown GaN template grown at Samsung was also characterized similarly. The free surface and substrate sides were confirmed to be Ga- and N-polarity, respectively. The density of dislocations near the N-face was determined to be, in order, (3 ± 1) x 10 7 and (4 ± 1) x 10 7 by cross-sectional TEM and plan-view TEM, respectively. Identical observations on the Ga-face revealed the defect concentration to be less than 1 x 10 7 cm -2 by plan-view TEM and 5 x 10 5 cm -2 by cross-sectional TEM. Defects in a 10 μm thick GaN layer grown by HVPE at Lincoln Laboratory have been investigated by photo electrochemical (PEC) etching, and by wet etching in hot H 3 PO 4 acid and molten KOH. Threading vertical wires (i.e. whiskers) and hexagonal-shaped etch pits are formed on the etched sample surfaces by PEC and wet etching, respectively. Using atomic force microscopy, one finds the density of whisker-like features to be 2 x 10 9 cm -2 , the same value found for the etch-pit density on samples etched with both H 3 PO 4 and molten KOH. Values agree well with TEM results. A free standing GaN template has been characterized for its structural and optical properties using X-ray diffraction, defect delineation etch followed by imaging with atomic force microscopy (AFM). The Ga-face and the N-face of the c-plane GaN exhibited a wide variation in terms of the defect density. The defect concentrations on Ga- and N-faces were about 5 x 10 5 cm -2 for the former and about 1 x 10 7 cm -2 for the latter, again in good agreement with TEM results mentioned above. High resolution X-ray rocking curves (omega scans) were measured. The [0 0 2] symmetric and [104] asymmetric peaks in 10 μm thick HVPE films had FWHM values between 5.8 and 7.9 arcmin, and 3.9 and 5.2 arcmin, respectively. The Samsung template investigated had wide diffraction peaks (20.6 and 24 arcmin for [0 0 2] and [1 0 4] diffractions, respectively) on the Ga-face, similar for the N-face, when a 2 mm slit size was used. When the slit size was reduced to 0.02 mm, the Ga- and N-face [0 0 2] peaks reduced to 69 and 160 arcsec. A bowing radius of 1.2 m was calculated to account for increased broadening with wider slits.