Dislocation evolution in 4H-SiC epitaxial layers

4H-SiC commercial wafers and sublimation grown epitaxial layers with a thickness of 100 mum have been studied concerning crystalline structure. The substrate wafers and the epitaxial layers have been separately investigated by high-resolution x-ray diffraction (HRXRD) and synchrotron white beam x-ray topography (SWBXT). The results show that the structural quality was improved in the epitaxial layers in the and directions, concerning domain distribution, lattice plane misorientation, mosaicity, and strain? compared with the substrates. Misoriented domains have merged together to form larger domains while the tilt between the domains was reduced, which resulted in non-splitting in diffraction curves. It is also clear that if the misorientation in the substrate gets too large, we can only see a slight decrease in the misorientation in the layer. At some positions on the substrates there were block structure (mosaicity). omega -rocking curves from epilayers at the same position showed smaller full width at half-maximum (FWHM) values and more uniform and narrow peaks. Curvature was almost the same in grown epilayers compared with the substrates. The shape of the grown epitaxial layers nas concave similarly to the substrates.

Silicon carbide (SiC) substrates with chemical vapor deposition (CVD) grown epilayers have been characterized by synchrotron white beam X-ray topography (SWBXT). Large numbers of circular basal plane dislocation loops (BPDs) were observed in the substrate which were anchored by threading screw dislocations (SDs). Threading edge dislocations (TEDs) are not observed to play an important role in the multiplication of BPDs. A SD-assisted “conservative climb” model is proposed to explain the multiplication of BPDs during growth and/or post-growth processes. BPDs are shown to multiply on adjacent parallel basal planes via single SD-assisted as well as opposite sign SD-pair-assisted “conservative climb”.

The crystalline structural quality of the grown crystals were examined by synchrotron white beam X-ray topography (SWBXT), high resolution triple axis X-ray diffraction (HRTXD) analysis, cathodoluminescence (CL) imaging and chemical etching. Two modes of SWBXT have been performed: (1) the transmission mode when the images of X-ray transmitted through a thin sample slab and (2) the reflection mode from the sample surface. Detailed topographs and HRTXD analyses have been performed on self-seeded grown ZnTe and ZnSe crystals as well as seeded grown ZnSe crystals. The major structural defects revealed on these vapor grown II–VI semiconductors were twins, subgrain boundary and dislocations. Chemical etching and cathodoluminescence revealed the density and shape of the dislocations in grown crystals of ZnSe, CdTe and CdS. The concentrations of impurities and dopants in the grown crystals were examined by Secondary Ion Mass Spectroscopy (SIMS) and Glow Discharge Mass Spectroscopy (GDMS) whereas the distributions of impurities and native point defects were mapped by photoluminescence (PL). The compositional distributions in the grown crystals of ternary ZnSeTe crystals were studied by wavelength dispersive X-ray spectroscopy (WDS), optical transmission measurements and precision density measurements.

Strain and temperature distribution in broad-area high-power laser diodes under operation determined by high resolution X-ray diffraction and topography

Using a combination of synchrotron white beam x-ray topography (SWBXT) and high resolution x-ray diffraction (HRXRD), the structural quality of AlN crystals grown by various sublimation-based techniques have been non-destructively analyzed. Spontaneously nucleated AlN crystals are characterized by very low defect densities but their size is small. Self-seeding results in nucleation of multiple grains of different orientations, a few of which are of good quality while most are highly strained. Using readily available commercial 4H and 6H-SiC substrates, several growth runs have been carried out using different growth conditions to obtain thick AlN layers, either attached to the seed or free-standing. While attached layers are typically cracked and highly strained, crack-free free-standing layers can be obtained by delamination or SiC decomposition. X-ray characterization reveals these crystals have good purity but moderately high defect densities.

The sublimation growth technique is highly attractive as a commercially viable GaN substrate technology on account of its simplicity and relatively high growth rates. Sublimation growth of GaN using GaN powder source, however, is hampered by formation of liquid Ga in the source. To overcome this limitation, an oxide transport process using a mixture of gallium oxide (Ga2O3) powder and graphite powder as precursors with nitrogen gas as carrier and ammonia as the source of nitrogen has been developed. GaN layers grown by this process were studied by optical microscopy, synchrotron white beam x-ray topography (SWBXT) and high resolution x-ray diffraction (HRXRD) to characterize their structural properties. Studies reveal that the GaN layers grown are single crystal but characterized by dislocation densities and impurities higher than those obtained using GaN powder source. Observed defect distribution is correlated with growth conditions to deduce optimal growth procedure.

In this communication we demonstrate how the difference in laser performance of two highly doped (20 at %) epitaxial layers of Yb-doped KY(WO4)2 (KYW) grown on a KYW substrate and Yb-doped KLu(WO4)2 (KLuW) grown on a KLuW substrate, respectively, is related to the presence of structural stress in the epilayers, investigated by synchrotron white beam X-ray topography. From the results obtained, it is clear that the samples that show a larger amount of structural stress, Yb:KYW/KYW epitaxies, lead to lower efficiency in laser operation, giving a direct correlation between the existence and magnitude of such structural stress and the loss in efficiency of laser performance in such epitaxial layers which, from a spectroscopical point of view, are otherwise equivalent.

Synchrotron X-ray Topography has been shown to be a vital tool for the nondestructive characterization of defects in 4H-SiC crystals [1-2]. Techniques utilizing reflection geometry are particularly useful for discerning defects at different depths below the crystal surface. For example, in studying defects in SiC pin diode structures, which typically comprise a buffer layer homoepitaxially grown on a substrate, with the drift layer grown on top of the buffer layer, it is important to be able to discriminate the depth at which particular defect configurations reside. This is particularly important for the characterization of defects resulting from relaxation processes such as interfacial dislocations and half loop arrays [3]. Accurate discernment of the depth of a defect requires precise measurement of the effective penetration depth of the X-ray beam in the diffraction geometry in question. This paper provides an assessment of the factors controlling that penetration depth in grazing incidence, reflection and back reflection geometries. There are generally two approaches adopted depending of the level of perfection of the crystal. In deformed regions (such as around dislocation cores) the penetration depth is simply determined by photoelectric absorption. In perfect regions it is determined by extinction. We will present a comparison between measured penetration depths in various diffraction geometries with those calculated using these two approaches and develop an optimized model to explain our observations. [1] Muller, G.S., et al., Volume production of high quality SiC substrates and epitaxial layers: Defect trends and device applications. Journal of Crystal Growth, 2012. 352(1): p. 39-42. [2] Dudley, M., et al., Characterization of 100 mm diameter 4H-Silicon carbide crystals with extremely low basal plane dislocation density, Material Science Forum,2001. 65: p. 353-356. [3] Wang, H., Dudley, M., et al., Studies of the Origins of Half-Loop Arrays and Interfacial Dislocations Observed in Homoepitaxial Layers of 4H-SiC. Journal of Electronic Materials, 2015. 44(5): p. 1268-1274

Investigation of character and spatial distribution of threading edge dislocations in 4H-SiC epilayers by high-resolution topography

Effect of the V/III ratio during buffer layer growth on the yellow and blue luminescence in undoped GaN epilayer has been studied by means of photoluminescence spectroscopy and high resolution X-ray diffraction. It is found that the densities of screw and edge threading dislocations increase with the V/III ratio of the buffer layer, and the intensities of the yellow luminescence (YL) and blue luminescence (BL) emissions also increase dramatically. However, the density ratio of the edge threading dislocation to the screw threading dislocation remains invariant, as well as the intensity ratio of YL emission to BL emission. It can be concluded from these phenomena that the edge threading dislocation and screw threading dislocation can enhance the YL and BL emissions, respectively.

Electron-hole recombination enhanced glide of Shockley partial dislocations bounding expanding stacking faults and their interactions with threading dislocations in 4H silicon carbide epitaxial layers have been studied using synchrotron white beam X-ray topography and in situ electroluminescence. The mobile silicon-core Shockley partial dislocations bounding the stacking faults are able to cut through threading edge dislocations leaving no trailing dislocation segments in their wake. However, when the Shockley partial dislocations interact with threading screw dislocations, trailing 30o partial dislocation dipoles are initially deposited in their wake due to the pinning effect of the threading screw dislocations. These dipoles spontaneously snap into their screw orientation, regardless the normally immobile carbon-core Shockley partial dislocation components in the dipoles. They subsequently cross slip and annihilate, leaving a prismatic stacking fault in (2-1-10) plane with the displacement vector 1/3[01-10].

Channel-cut monochromators can be easily incorporated in high-resolution image techniques. However, polishing on the inner diffracting surfaces is difficult because of blockage by the opposite face. To address this difficulty, an open-faced monolithic monochromator has been designed, produced and tested using x-rays at the Advanced Photon Source (APS). The open-faced channel cut has a "Z"-shape geometry with a hole in the mid section to allow passage of the diffracted beam. The open geometry allowed chemical mechanical polishing so that an optically smooth finish on both surfaces was achieved. The high-resolution x-ray imaging and topography measurements revealed that the new design introduces significantly less distortions in the phase-contrast images compared with conventional channel-cut monochromators produced using etching alone.

Sulphamic acid (HSO3NH2) is a potential material that exhibits excellent piezoelectric and non-linear optical properties. Nucleation and growth kinetics give valuable information about the crystal growth process, which can be employed in the growth of large size crystals. Thus we have studied its nucleation parameters such as solubility, metastable zone width, induction period, interfacial tension, critical free energy, volume free energy change, critical nucleus and found that good quality sulphamic acid crystal can be grown at low temperature. Growth of good quality crystal was done by adopting slow evaporation solution growth technique at room temperature and as a result, good quality single crystal was grown. The grown bulk single crystal of the title compound was subjected to various characterization analyses. Its unit cell dimensions were confirmed using powder X-ray diffraction. Further its crystalline perfection was assessed using high resolution X-ray diffraction and X-ray topography techniques and it was found that it is reasonably good. Its various functional groups were identified from the Fourier transform-Raman method. Nanoindentation was performed to identify the load dependence and independence of hardness (H) and Young's modulus (E) using the Oliver–Pharr method and it was found that both H and E exhibit peak load dependence. Photopyroelectric study was performed to identify its thermal properties such as thermal diffusivity (α), thermal conductivity (k), thermal effusivity (e), and heat capacity (cp). These studies reveal that it has high thermal stability compared to other single crystals. The optical homogeneity of the grown crystal was assessed using a birefringence interferometer and it was found to be reasonably good.

The origin of expanded single Shockley-type stacking faults in forward-current degradation of 4H-SiC p–i–n diodes was investigated by the stress-current test. At a stress-current density lower than 25 A cm−2, triangular stacking faults were formed from basal-plane dislocations in the epitaxial layer. At a stress-current density higher than 350 A cm−2, both triangular and long-zone-shaped stacking faults were formed from basal-plane dislocations that converted into threading edge dislocations near the interface between the epitaxial layer and the substrate. In addition, the conversion depth of basal-plane dislocations that expanded into the stacking fault was inside the substrate deeper than the interface. These results indicate that the conversion depth of basal-plane dislocations strongly affects the threshold stress-current density at which the expansion of stacking faults occurs.

Ammonothermal Gallium Nitride (GaN) substrates are the most promising substrates for homoepitaxial growth of GaN films having low dislocation density. Growth-induced structural inhomogeneities in these substrates were investigated by high-resolution X-ray topography (HR-XRT) and high-resolution X-ray diffraction (HR-XRD). A one-to-one correlation of defects was observed in photoluminescence imaging. From the HR-XRD intrinsic rocking curve widths were found to be 16 arcsecs indicating superior crystalline quality. The lattice constants were measured from symmetric and asymmetric reflections to be similar to bulk values indicting low sample strian. The true dislocation density, from the HR-XRT images, was observed to be of the order of 102 cm–2 in the samples, and the radius of curvature was greater than 600 m. Growth striations were observed in the a and m-pane samples and are attributed to inhomogeneity in impurity incorporation during growth. Photoluminescence imaging showed deep level luminescent centers along the growth striations.