Jianqiu Guo

Bulk Growth of Large Area SiC Crystals

The growth of large diameter silicon carbide (SiC) crystals produced by the physical vapor transport (PVT) method is outlined. Methods to increase the crystal diameters, and to turn these large diameter crystals into substrates that are ready for the epitaxial growth of SiC or other non homogeneous epitaxial layers are discussed. We review the present status of 150 mm and 200 mm substrate quality at Cree, Inc. in terms of crystallinity, dislocation density as well as the final substrate surface quality.

Mapping of Lattice Strain in 4H-SiC Crystals by Synchrotron Double-Crystal X-ray Topography

The presence of lattice strain in n-doped 4H-SiC substrate crystals grown by a physical vapor transport method can strongly influence the performance of related power devices that are fabricated on them. Information on the level and the variation of lattice strain in these wafer crystals is thus important. In this study, a non-destructive method is developed based on synchrotron double-crystal x-ray topography to map lattice strains in 4H-SiC wafers. Measurements are made on two 4H-SiC substrate crystals—one is an unprocessed commercial wafer while the other was subject to a post-growth high-temperature heat treatment. Maps of different strain components are generated from the equi-misorientation contour maps recorded using synchrotron monochromatic radiation. The technique is demonstrated to be a powerful tool in estimating strain fields in 4H-SiC crystals. Analysis of the strain maps also shows that the normal strain components vary much more significantly than do the shear/rotation components, indicating that lattice dilation/compression rather than lattice tilt is the major type of deformation caused by both the incorporation of nitrogen dopants and the nucleation of basal plane dislocations.

Prismatic Slip in PVT-Grown 4H-SiC Crystals

Basal plane slip is the most frequently observed deformation mechanism in 4H-type silicon carbon (4H-SiC) single crystals grown by the physical vapor transport (PVT) method. However, it was recently reported that dislocations in such crystals can also glide in prismatic slip systems. In this study, we observed nonuniform distributions of three sets of prismatic dislocations in a commercial 4H-SiC substrate wafer. The nonuniformity is a result of the distribution of resolved shear stress on each prismatic slip system caused by radial thermal gradients in the growing crystal boule. A radial thermal model has been developed to estimate the thermal stress across the entire area of the crystal boule during PVT growth. The model results show excellent agreement with the observations, confirming that radial thermal gradients play a key role in activating prismatic slip in 4H-SiC during bulk growth.

Effect of Doping Concentration Variations in PVT-Grown 4H-SiC Wafers

Synchrotron white beam x-ray topography studies carried out on 4H-SiC wafers characterized by locally varying doping concentrations reveals the presence of overlapping Shockley stacking faults generated from residual surface scratches in regions of higher doping concentrations after the wafers have been subjected to heat treatment. The stacking faults are rhombus-shaped and bound by Shockley partial dislocations. The fault generation process is driven by the fact that in regions of higher doping concentrations, a faulted crystal containing double Shockley faults is more stable␣than a perfect 4H-SiC crystal at the high temperatures (>1000°C) that the wafers are subject to during heat treatment. We have developed a model for the formation mechanism of the rhombus-shaped stacking faults. Our studies show that during heat treatment of the wafer, such double Shockley faults can be generated in regions where dislocation sources are presents (e.g. scratches or low-angle boundaries) and when the nitrogen doping concentration exceeds a certain level.

Direct Determination of Burgers Vectors of Threading Mixed Dislocations in 4H-SiC Grown by PVT Method

In addition to pure threading screw dislocations (TSDs), the presence of threading mixed dislocations (TMDs) (with a component) has been reported both in 4H-SiC axial slices (wafers cut parallel to the growth axis) and in commercial offcut wafers (cut almost perpendicular to the growth axis). In this paper, we first demonstrate a method to quickly distinguish TMDs from TSDs in axial slices via synchrotron white-beam x-ray topography. Since such axial slices are usually not available for commercial purposes, a systematic method is then developed and demonstrated here to unambiguously determine the Burgers vectors of TMDs in 4H-SiC commercial offcut wafers. In this second study, both synchrotron monochromatic-beam x-ray topography and ray-tracing simulation are used. The x-ray topographs were recorded using grazing-incidence geometry. The principle of this method is that the contrast of dislocations on different reflections varies with the relative orientation of Burgers vectors with respect to the diffraction vectors. Measurements confirm that, in a commercial offcut wafer, the majority of the threading dislocations with screw component are mixed-type dislocations.

Penetration Depth and Defect Image Contrast Formation in Grazing-Incidence X-ray Topography of 4H-SiC Wafers

Synchrotron x-ray topography in grazing-incidence geometry is useful for discerning defects at different depths below the crystal surface, particularly for 4H-SiC epitaxial wafers. However, the penetration depths measured from x-ray topographs are much larger than theoretical values. To interpret this discrepancy, we have simulated the topographic contrast of dislocations based on two of the most basic contrast formation mechanisms, viz. orientation and kinematical contrast. Orientation contrast considers merely displacement fields associated with dislocations, while kinematical contrast considers also diffraction volume, defined as the effective misorientation around dislocations and the rocking curve width for given diffraction vector. Ray-tracing simulation was carried out to visualize dislocation contrast for both models, taking into account photoelectric absorption of the x-ray beam inside the crystal. The results show that orientation contrast plays the key role in determining both the contrast and x-ray penetration depth for different types of dislocation.

Correlation of Lifetime Mapping of 4H-SiC Epilayers with Structural Defects Using Synchrotron X-Ray Topography

Lifetime maps for two 4H-SiC epi-wafers (samples 1 and 2) were recorded using microwave photoconductive decay (μPCD) measurements and correlated with the type and distribution of structural defects mapped by synchrotron X-ray topography (white beam and monochromatic). Sample 1 showed lower lifetime inside one of its higher doped facet regions and along its edges. The low lifetime in the facet region was associated with the presence of a high density of multi-layered Shockley stacking faults (SFs) and low angle grain boundaries (LAGBs). These stacking faults are likely double Shockley stacking faults (DSSFs) and probably nucleated from scratches present on the substrate surface and LAGBs present in that region, propagating during epilayer growth. In contrast, sample 2 showed a reduced carrier lifetime in the middle region associated with a network of interfacial dislocations (IDs) and half loop arrays (HLAs) originating from 3C inclusions that are generated during epilayer growth. Along the edges of both samples, overlapping triangular defects, microcracks and BPD loops lowered lifetime.

Study of defect structures in 6H-SiC a/m-plane pseudofiber crystals grown by hot-wall CVD epitaxy

Structural perfection of silicon carbide (SiC) single crystals is essential to achieve high-performance power devices. A new bulk growth process for SiC proposed by researchers at NASA Glenn Research Center, called large tapered crystal (LTC) growth, based on axial fiber growth followed by lateral expansion, could produce SiC boules with potentially as few as one threading screw dislocation per wafer. In this study, the lateral expansion aspect of LTC growth is addressed through analysis of lateral growth of 6H-SiC a/m-plane seed crystals by hot-wall chemical vapor deposition. Preliminary synchrotron white-beam x-ray topography (SWBXT) indicates that the as-grown boules match the polytype structure of the underlying seed and have a faceted hexagonal morphology with a strain-free surface marked by steps. SWBXT Laue diffraction patterns of transverse and axial slices of the boules reveal streaks suggesting the existence of stacking faults/polytypes, and this is confirmed by micro-Raman spectroscopy. Transmission x-ray topography of both transverse and axial slices reveals inhomogeneous strains at the seed–epilayer interface and linear features propagating from the seed along the growth direction. Micro-Raman mapping of an axial slice reveals that the seed contains high stacking disorder, while contrast extinction analysis (g·b and g·b×l) of the linear features reveals that these are mostly edge-type basal plane dislocations. Further high-resolution transmission electron microscopy investigation of the seed–homoepilayer interface also reveals nanobands of different SiC polytypes. A model for their formation mechanism is proposed. Finally, the implication of these results for improving the LTC growth process is addressed.

Studies of the Origins of Half Loop Arrays and Interfacial Dislocations Observed in Homoepitaxial Layers of 4H-SiC

Dislocation behavior during homo-epitaxy of 4H-SiC on offcut substrates by Chemical Vapor Deposition (CVD) has been studied using Synchrotron X-ray Topography and KOH etching. Studies carried out before and after epilayer growth have revealed that, in some cases, short, edge oriented segments of basal plane dislocation (BPD) inside the substrate can be drawn towards the interface producing screw oriented segments intersecting the growth surface. In other cases, BPD half-loops attached to the substrate surface are forced to glide into the epilayer producing similar screw oriented surface intersections. It is shown that the initial motion of the short edge oriented BPD segments that are drawn from the substrate into the epilayer is caused by thermal stress resulting from radial temperature gradients experienced by the wafer whilst in the epi-chamber. This same stress also causes the initial glide of the surface half-loop into the epilayer and through the advancing epilayer surface. These mobile BPD segments provide screw oriented segments that pierce the advancing epilayer surface that initially replicate as the crystal grows. Once critical thickness is reached, according to the Mathews-Blakeslee model, these screw segments glide sideways under the action of the mismatch stress leaving IDs and HLAs in their wake.