Morphology of basal plane dislocations in 4 H - Si C homoepitaxial layers grown by chemical vapor deposition X. Zhang, S. Ha, Y. Hanlumnyang, C. H. Chou, V. Rodriguez, M. Skowronski, J. J. Sumakeris, M. J. Paisley, and M. J. O’Loughlin Citation: Journal of Applied Physics 101, 053517 (2007); doi: 10.1063/1.2437585 View online: http://dx.doi.org/10.1063/1.2437585 View Table of Contents: http://scitation.aip.org/content/aip/journal/jap/101/5?ver=pdfcov Published by the AIP Publishing Articles you may be interested in Nucleation of in-grown stacking faults and dislocation half-loops in 4H-SiC epitaxy J. Appl. Phys. 114, 123502 (2013); 10.1063/1.4821242 Annealing induced extended defects in as-grown and ion-implanted 4H–SiC epitaxial layers J. Appl. Phys. 108, 013511 (2010); 10.1063/1.3457840 Glide and multiplication of basal plane dislocations during 4 H ‐ Si C homoepitaxy J. Appl. Phys. 102, 093520 (2007); 10.1063/1.2809343 Evolution of basal plane dislocations during 4 H -silicon carbide homoepitaxy Appl. Phys. Lett. 87, 161917 (2005); 10.1063/1.2108109 Anomalous photoluminescence from 3C-SiC grown on Si(111) by rapid thermal chemical vapor deposition Appl. Phys. Lett. 70, 1757 (1997); 10.1063/1.118648 [This article is copyrighted as indicated in the article. Reuse of AIP content is subject to the terms at: http://scitation.aip.org/termsconditions. Downloaded to ] IP: 158.108.130.130 On: Tue, 14 Apr 2015 10:49:44 JOURNAL OF APPLIED PHYSICS 101, 053517 共2007兲 Morphology of basal plane dislocations in 4H-SiC homoepitaxial layers grown by chemical vapor deposition X. Zhang, S. Ha, Y. Hanlumnyang, C. H. Chou, V. Rodriguez, and M. Skowronskia兲 Carnegie Mellon University, 5000 Forbes Avenue, Pittsburgh, Pennsylvania 15213 J. J. Sumakeris, M. J. Paisley, and M. J. O’Loughlin Cree Inc., 4600 Silicon Drive, Durham, North Carolina 27703 共Received 3 October 2006; accepted 19 December 2006; published online 9 March 2007兲 The morphology of basal plane dislocations 共BPDs兲 in 4H-SiC homoepitaxial layers has been investigated by plan-view transmission x-ray topography and molten KOH etching. Three types of BPDs are distinguished based on their morphologies. These include interfacial dislocations, curved dislocations, and circular loop dislocations around micropipes. Their characteristics are studied in detail and possible sources of their formation during epitaxy are discussed. © 2007 American Institute of Physics. 关DOI: 10.1063/1.2437585兴 I. INTRODUCTION The origin and characteristics of basal plane dislocations 共BPDs兲 in 4H-SiC homoepitaxial layers are of great interest from the fundamental understanding point of view as well as due to their effects on the reliability of SiC bipolar devices. It was reported that under forward bias, the voltage drop across SiC p-i-n diodes changes over time.1–3 Extensive research effort worldwide has resulted in good understanding of how and why the degradation phenomenon occurs.4–14 It is attributed to the formation of single layer Shockley-type stacking faults produced by dissociation of basal plane dislocations in the epilayers inherited from the substrates.5,6,15 The stacking faults expand by the motion of mobile silicon-core partial dislocations activated by electron-hole recombination under forward bias.14,16,17 4H-SiC epilayers are usually grown by step-controlled epitaxy, a variant of chemical vapor deposition 共CVD兲. Layers are grown on vicinal substrates with several degrees of off-cut angle with respect to 兵0001其 basal plane. The high step density on the substrate surface allows adatoms to attach at the step edges and prevents two dimensional nucleation which will lead to growth of cubic 3C-SiC polytype. Typical densities of basal plane dislocations in 4H-SiC substrates are in the range of 104 – 105 cm−2.18,19 BPD densities in epilayers are typically significantly lower than those in substrates due to conversion of BPDs in substrates to threading edge dislocations in epilayers.3,18 The conversion is approximately 90% efficient in nonoptimized epitaxy.18,20 The remaining 10% of the BPDs propagate from the substrates into the epilayers along the basal plane.21,22 The influence of growth conditions on the conversion efficiency was investigated including the factors such as C / Si ratio, growth temperature, growth rate, surface preparation process prior to growth, and surface polarity.20,23 Recently developed low BPD growth techniques utilize KOH-etched or patterned substrate surface to enhance BPD conversion. BPD densities as low as 10 cm−2 have been reported.24,25 a兲 Electronic mail: [email protected] 0021-8979/2007/101共5兲/053517/8/$23.00 A comprehensive understanding of the source and morphology of basal plane dislocations remaining in SiC epilayers is needed. In this study, transmission x-ray topography was used in plan-view geometry to image the BPDs and to investigate their characteristics. Complementary data were obtained by molten KOH etching. Based on these results, possible sources of BPDs in SiC homoepitaxial layers are discussed. II. EXPERIMENT The samples examined in this study were grown by a silane-based CVD method on Si face of 4H-SiC n-type conducting substrates 共n = 8 ⫻ 1018 cm−3兲. The substrates were off cut by 8° from 关0001兴 towards either 关11− 20兴 or 关21 − 30兴 direction. The off-cut direction defined here is opposite to the step-flow direction during epitaxial growth. Most of the epitaxial structures contained 5 m n+-doped 共n = 5 ⫻ 1017 cm−3兲 buffer layers and the top epilayers were doped with nitrogen in 1014 – 1015 cm−3 range. One epitaxial structure had a very thick buffer layer of 50 m 共n = 1 ⫻ 1018 cm−3兲 and a 50 m n−-doped 共n = 2 ⫻ 1015 cm−3兲 epilayer on its top. Plan-view transmission x-ray topographs were obtained using the Mo K␣ radiation. The epiwafers were diced into 1 ⫻ 1 cm2 samples. Either most or all of the substrate thickness was removed by mechanical polishing in order to obtain clear images of BPDs in the epilayers without interference of contrast from the substrates. After polishing, the samples were etched in molten KOH to remove the damage caused by polishing and to map the defect distribution on the surface of epilayers. Some samples were gradually thinned from the substrate side 共including removal of epitaxial buffer layer and part of the epilayer兲 with x-ray topographs taken after each polishing step. This procedure allowed the determination of the locations of dislocations within the epitaxial structure. The thickness uniformity across 1 cm2 area after mechanical polishing was in the range of ±10 m. 101, 053517-1 © 2007 American Institute of Physics [This article is copyrighted as indicated in the article. Reuse of AIP content is subject to the terms at: http://scitation.aip.org/termsconditions. Downloaded to ] IP: 158.108.130.130 On: Tue, 14 Apr 2015 10:49:44 053517-2 Zhang et al. FIG. 1. Transmission x-ray plan-view 共11− 20兲 topographs showing the interfacial dislocations in epiwafers with 共a兲 关11− 20兴 off-cut direction and 共b兲 关21− 30兴 off-cut direction. III. RESULTS AND DISCUSSION Basal plane dislocations in 4H-SiC epilayers have been imaged and reported in numerous publications.4–6,15,26–29 Electroluminescence imaging in a forward-biased p-i-n diode is a straightforward way to map the BPDs that serve as nucleation sites for stacking faults. Straight and curved basal plane dislocations have been observed in the diode structures.4–6,15 However, many of their characteristics, such as the Burgers vectors or locations in the structure, have not always been determined. In addition, some dislocations dissociate and move under very low current density which makes it difficult to image the original line directions of the dislocations. On the other hand, x-ray topography is widely used to provide the structural information of the basal plane dislocations.26–29 In this study, three types of BPDs in 4H-SiC epilayers were distinguished according to their morphologies. The summary of the relevant literature data is included in each of the following sections. A. Interfacial dislocations Long basal plane dislocations 共with lengths of hundred microns to several millimeters兲 perpendicular to the off-cut directions were revealed by plan-view x-ray topography in 4H-SiC epitaxial layers 共marked with triangles in Fig. 1兲. Their positions were determined to be at or close to the epilayer/substrate interface, and therefore they will be referred to as interfacial dislocations. Many of the characteristics of interfacial dislocations are similar to those described by Jacobson et al.,26,27 who referred to this type of BPDs as misfit dislocations. J. Appl. Phys. 101, 053517 共2007兲 Both x-ray topographs in Fig. 1 were obtained using 共11− 20兲 reflection. The g vector is labeled in the figure. Some of the interfacial dislocations are marked with triangles. The image in Fig. 1共a兲 was obtained on a sample consisting of 99 m n− epilayer, 5 m n+ buffer layer, and 12 m of the substrate remaining. The off cut is along the 关11− 20兴 direction, parallel to the g vector. The image in Fig. 1共b兲 was obtained on a sample with 39 m n− epilayer and 30 m of the remaining substrate. The off cut is along the 关21− 30兴 direction, which is 15° counterclockwise away from the g vector. It is apparent that the interfacial dislocations are not confined to one specific crystallographic direction but instead their average direction is perpendicular to the off cut. Locally, however, the interfacial dislocation line can form angles other than 90° with respect to the off-cut direction and can frequently form a zigzag line. An example of such dislocation is marked with an arrow in Fig. 1共a兲. This characteristic is more evident in the case of interfacial dislocations observed in the epiwafer with a thick buffer layer, as the two marked with arrows in Fig. 2共a兲. The image was obtained on a sample with 50 m n− epilayer, 50 m n+ buffer, and 10 m of the remaining substrate using 共11− 20兲 reflection. The zigzag segments are about 70° clockwise and counterclockwise away from the off-cut direction, showing a tendency to be aligned along 关−2110兴 and 关1 − 210兴 directions. The apparent differences in dislocation densities in Figs. 2共a兲–2共c兲 are explained later in this section. Most of the short curved line contrasts shown in Fig. 1共b兲 are probably produced by the basal plane dislocations in the substrate, since the sample had 30 m of substrate remaining after polishing. Line contrasts other than interfacial dislocations were also observed in Fig. 2共a兲, as the one marked with a solid triangle. They are produced by another type of basal plane dislocations observed in 4H-SiC homoepitaxial layers, referred to as “curved dislocations.” They will be described in the next section. The location of the interfacial dislocations in the epilayer/buffer/substrate structure was determined by gradual removal of material from the substrate side and repeated x-ray imaging. For the epiwafers with 5 m of thin buffer layers, the interfacial dislocations were determined to be within ±15 m from the buffer/substrate interface. Still it was unclear in which part of the epilayer/buffer/substrate structure the dislocations stayed, and 5 m of buffer layer is too thin for mechanical polishing to resolve it. Thus the samples with 50 m thick buffer layer were used to clarify the position of interfacial dislocations. The images shown in Figs. 2共b兲 and 2共c兲 are 共11− 20兲 topographs obtained from the same area as shown in Fig. 2共a兲, with all the substrate removed and buffer layer thinned down to 25 and 5 m, respectively. The long dislocation lines perpendicular to the off-cut direction are clearly visible in Fig. 2共b兲, but are gone in Fig. 2共c兲. This indicates that the interfacial dislocations are present in the top half of the buffer layer. Several very short line contrasts are still visible in Fig. 2共c兲, two of which are labeled with hollow triangles. Compared with Figs. 2共a兲 and 2共b兲, both of these were determined to be from one interfacial dislocation. The left one was produced by a short segment of basal plane dislocation connecting to one end of the [This article is copyrighted as indicated in the article. Reuse of AIP content is subject to the terms at: http://scitation.aip.org/termsconditions. Downloaded to ] IP: 158.108.130.130 On: Tue, 14 Apr 2015 10:49:44 053517-3 Zhang et al. J. Appl. Phys. 101, 053517 共2007兲 FIG. 3. Transmission x-ray plan-view topographs of the same area using 共a兲 共11− 20兲, 共b兲 共01− 10兲, 共c兲 共10− 10兲, and 共d兲 共1 − 100兲 reflections. The sample was from the epiwafer with a 50 m thick buffer layer. FIG. 2. Transmission x-ray plan-view 共11− 20兲 topographs of the same area of the epiwafer with 共a兲 50 m epilayer, 50 m buffer, and 10 m substrate: 共b兲 50 m epilayer and thinned buffer with only 25 m of remaining thickness: and 共c兲 50 m epilayer and 5 m remaining buffer. The two arrows in 共a兲 mark two interfacial dislocations. The solid triangles in 共a兲 and 共b兲 point out one curved dislocation. The two hollow triangles in 共a兲 and 共c兲 point out one end and tip of the zigzag line of one interfacial dislocation. interfacial dislocation and leading to the epilayer/buffer interface. The right one was produced by one tip of the zigzag line of the interfacial dislocation. Their corresponding contrasts in the topograph before the buffer layer being thinned down were labeled with two hollow triangles in Fig. 2共a兲. It should be noted that the length of the curved dislocations 共as the one marked with a solid triangle兲 was reduced as the material was removed from the substrate side. All of them are invisible in Fig. 2共c兲 as most of the buffer layer was removed, indicating that they thread through the entire buffer layer but are not present in the n− epilayer. This could be due to basal plane dislocations converting into threading ones at the epilayer/buffer interface. However, clear contrasts of the ends and tips of zigzag lines remain in Fig. 2共c兲 for some interfacial dislocations. This indicates that those segments of the interfacial dislocations may extend into the epilayer. Based on the observation described above, the position of interfacial dislocations is determined to be in the top half portion of the buffer layer. They are closer to the epilayer/ buffer interface than the buffer/substrate interface. The randomly oriented straight lines visible in Figs. 2共b兲 and 2共c兲 are contrasts due to polishing scratches. The set of six prismatic reflections of 兵11− 20其 and 兵1 − 100其 was used to determine the Burgers vector of interfacial dislocations. Figures 3共a兲–3共d兲 show four topographs of the same area using 共11− 20兲, 共01− 10兲, 共10− 10兲, and 共1 − 100兲 reflections, respectively. The sample consisted of 50 m n− epilayer, 50 m n+ buffer layer, and 10 m substrate. The interfacial dislocation lines are out of contrast in the 共1 − 100兲 reflection. Thus their Burgers vector is determined to be along the 关11− 20兴 direction 共parallel to the offcut direction兲. The same extinction condition applied to the interfacial dislocations in the epiwafers with thin buffer layers. Jacobson et al.27 proposed that the interfacial dislocations are formed due to the misfit strain between SiC substrate and epilayer induced by different nitrogen doping concentrations. These authors considered the different radii of substitutional nitrogen atoms and the host carbon atoms and calculated the lattice parameter change with nitrogen doping concentration. Increasing the nitrogen concentration tends to reduce the lattice parameters of the host SiC crystal. In their back-reflection x-ray topography experiments, edge-type dislocation lines perpendicular to the off cut were detected in 30 m thick 4H-SiC epilayer doped with 3 ⫻ 1015 cm−3 nitrogen grown on conducting substrate with a nitrogen doping concentration of 3 ⫻ 1019 cm−3. However, such features were not found in the epilayers with the same growth conditions and nitrogen doping concentration grown on substrates doped with 4 ⫻ 1018 or 1.3⫻ 1019 cm−3 nitrogen. These experimental results indicated that the formation of interfacial dislocations was related to the misfit strain between substrate and epilayer induced by different nitrogen doping concentrations. There are two widely accepted models for nucleation of misfit dislocations.30 One is through the elongation of a grown-in dislocation to form a segment of misfit dislocation [This article is copyrighted as indicated in the article. Reuse of AIP content is subject to the terms at: http://scitation.aip.org/termsconditions. Downloaded to ] IP: 158.108.130.130 On: Tue, 14 Apr 2015 10:49:44 053517-4 Zhang et al. FIG. 4. Transmission x-ray plan-view 共11− 20兲 topograph showing two interfacial dislocations. Triangles point out one pinning point on each interfacial dislocation. line at the interface. The other model argues that the dislocation half-loops nucleate on the surface of the growing epilayer and glide into the crystal, finally forming misfit dislocation lines at the interface. In either case, the dislocations start gliding only after a relatively thick epilayer has been deposited and enough strain energy has accumulated. The minimum energy of the relaxed system is achieved if the misfit segment is located at the interface. In the epilayer/ buffer/substrate structure with three doping concentrations, the interfacial dislocations should be located close to the buffer/substrate interface because both the epilayer and buffer layer are compressively strained with respect to the substrate, and the nitrogen doping concentration difference is larger between substrate and buffer than that between buffer and epilayer. However, the interfacial dislocations were determined to be located in the top half of the thick buffer layer, closer to the epilayer/buffer interface than the buffer/ substrate interface. It should also be noted that some of the interfacial dislocations show the characteristic of a moving dislocation pinned by an obstacle, as shown in Fig. 4. The image was obtained using 共11− 20兲 reflection on a sample with 50 m epilayer, 50 m buffer layer, and 10 m substrate. Two interfacial dislocations are imaged in the topograph, while other line contrasts are produced by curved dislocations. One pinning point on each interfacial dislocation is marked with one triangle. This morphology indicates that the dislocations are moving towards the substrate side in the buffer layer. Both interfacial dislocations are connected at their ends to basal plane dislocations extending towards the epilayer side and the substrate side approximately along the off-cut direction. By measuring their lengths projected to the off-cut direction, their positions could be determined. The two basal plane dislocations extend towards the epilayer side end at the epilayer/buffer interface. They may have converted to threading dislocations in the n− epilayer. X-ray topography in plan-view geometry can be used to determine the relation between interfacial dislocations and other basal plane dislocations in the epitaxial layers and/or in the substrate. One example was shown in Fig. 4 and described in the previous paragraph. The ends of the interfacial dislocations could be in the form of either a threading or a basal plane dislocation extending into the epilayer or the substrate. Since threading dislocations will propagate along the c axis and they are unlikely to glide in the system with J. Appl. Phys. 101, 053517 共2007兲 FIG. 5. Schematics of the four configurations of the interfacial dislocations 共IDs兲 in the buffer layer related to other basal plane dislocations 共BPDs兲. A1, both ends connected to BPDs through buffer and epilayer above the interfacial dislocation; A2, both ends connected to BPDs only in buffer above the interfacial dislocation, then converting to threading edge dislocations 共TEDs兲 in the n− epilayer; B1, one end connected to a BPD in the substrate, the other end connected to a BPD through buffer and epilayer; and B2, one end connected to a BPD in the substrate, the other end connected to a BPD in the buffer layer, then converting to a TED in the n− layer. few dislocations and low strain,31 only two configurations are consistent with the misfit-induced glide model for interfacial dislocations. One is that both ends of the interfacial dislocation are connected to basal plane dislocations above it in the epitaxial layer 共configuration A兲. Configuration A corresponds to the formation of interfacial dislocations through glide of basal plane dislocation half-loops nucleated on the surface of growing epilayer. The other configuration is that one end is connected to a basal plane dislocation in the substrate while the other end is connected to a basal plane dislocation above it in the epitaxial layer 共configuration B兲. Configuration B corresponds to the formation of interfacial dislocations through the elongation of basal plane dislocations propagating from the substrate at the interface. In the epilayer/buffer/substrate structure, each configuration will contain two categories assuming that the basal plane dislocations in the buffer layer could possibly convert to threading edge dislocations 共TEDs兲 in the epilayer at the epilayer/ buffer interface. Thus totally four types are expected for the relation between interfacial dislocations in the buffer layer and other basal plane dislocations. They are A1, both ends connected to BPDs through buffer and epilayer above the interfacial dislocation; A2, both ends connected to BPDs only in buffer above the interfacial dislocation, then converting to TEDs in the n− epilayer; B1, one end connected to a BPD in the substrate, the other end connected to a BPD through buffer and epilayer; and B2, one end connected to a BPD in the substrate, the other end connected to a BPD in the buffer layer, then converting to a TED in the n− layer. The schematics of the four configurations in a cross-sectional view are shown in Fig. 5. The off-cut angle was exaggerated in the schematics. The vertical and tilted lines indicate the TEDs and BPDs, respectively. The horizontal lines in the top half of the buffer layer indicate the interfacial dislocations 共IDs兲. Over 20 interfacial dislocations were examined in the epiwafers with thick and thin buffer layers, both ends of which could be differentiated without overlap with other features in the topographs. Eighteen of them show configuration B2, three exhibit configuration B1, two exhibit configuration A2, and none corresponds to configuration A1. Representative examples are shown in Fig. 6. Both topographs in Fig. 6 [This article is copyrighted as indicated in the article. Reuse of AIP content is subject to the terms at: http://scitation.aip.org/termsconditions. Downloaded to ] IP: 158.108.130.130 On: Tue, 14 Apr 2015 10:49:44 053517-5 Zhang et al. J. Appl. Phys. 101, 053517 共2007兲 FIG. 6. Transmission x-ray plan-view 共11− 20兲 topographs obtained from two different epiwafers. Interfacial dislocations with configurations A2, B1, and B2 are labeled. Ends of the interfacial dislocations are marked with arrows. Two triangles in 共a兲 mark both ends of one interfacial dislocation, whose configuration could not be determined by x-ray topography in plan-view geometry. were obtained using 共11− 20兲 reflection. Figure 6共a兲 was obtained on a sample with 50 m epilayer, 50 m buffer layer, and 10 m of remaining substrate. Figure 6共b兲 was obtained on a sample with 99 m epilayer, 5 m buffer layer, and 12 m of remaining substrate. Interfacial dislocations with A2, B1, and B2 configurations are labeled in the two topographs. Ends of the interfacial dislocations are marked with arrows. It could be seen that for configuration A2, two short basal plane dislocations, both in the buffer layer above the interfacial dislocation, are connected to its ends. For configuration B2, one BPD in the buffer layer and one BPD from the substrate are connected to each end of the interfacial dislocation. That the BPD segment in the substrate is not visible in Fig. 6共b兲 might be due to the thickness variance of the sample after mechanical polishing such that at the region shown in the topograph the substrate was totally removed. The corresponding BPDs in the substrate had been detected in the 共11− 20兲 topograph obtained at the same area with 45 m of remaining substrate 共the image is not shown in this paper兲. For configuration B1, one BPD continuing through both the buffer layer and the n− epilayer is connected to the interfacial dislocation, as the one shown in Fig. 6共b兲. However, configurations other than A2, B1, and B2 could also exist. For example, the interfacial dislocation marked with two triangles in Fig. 6共a兲 has no visible BPD connecting to either of its ends. The BPD close to its left end was detected as a separate dislocation by polishing experiment. After part of the buffer layer was removed, the BPD and the end of the interfacial dislocation were clearly separated. For such an interfacial dislocation, its end is difficult to be differentiated between connecting to a threading dislocation and to a BPD which is too short to be resolved. [This article is copyrighted as indicated in the article. Reuse of AIP content is subject to the terms at: http://scitation.aip.org/termsconditions. Downloaded to ] IP: 158.108.130.130 On: Tue, 14 Apr 2015 10:49:44 053517-6 Zhang et al. FIG. 7. Transmission x-ray plan-view 共11− 20兲 topograph obtained from a sample with 50 m epilayer, 50 m buffer, and 10 m substrate. Three curved basal plane dislocations are marked with triangles. Two arrows point out two pinning sites on one curved dislocation. To summarize the observations described above, interfacial dislocations are edge-type dislocations with the average line direction perpendicular to the off-cut direction. Frequently, they are close to or at the epilayer/substrate interface. In structures with thick buffer layer, the interfacial dislocations are found in the top half of the buffer layer. The dislocation lines are zigzagged, with zigzag segments about 70° away from the off-cut direction, showing a tendency to be aligned along the 关−2110兴 and 关1 − 210兴 directions. Pinning points due to point sources or threading dislocations were detected along the interfacial dislocation lines, which indicates that they are moving towards the substrate. Most of the interfacial dislocations are connected to one basal plane dislocation from the substrate at one end and to another BPD continuing toward the epilayer surface on the other end. Based on these observations, the formation of interfacial dislocations may be due to the sideway glide of preexisting basal plane dislocations in the buffer layer propagating from the substrate. The long dislocation lines perpendicular to the off cut can move towards the buffer/substrate interface driven by the stress in the epitaxial layers. At this stage, it is not clear whether the stress is due to doping-induced misfit strain. In addition, a number of unanswered questions remain: where does the sideway glide start, how does the glide continue for millimeters, why do some dislocations glide for millimeters while others in the same epilayer do not move more than 500 m, and why have not the interfacial dislocations in the thick buffer layer reached the buffer/substrate interface. Further investigation is needed to resolve these issues. B. Curved dislocations The second type of basal plane dislocations frequently revealed by plan-view x-ray topography in 4H-SiC epitaxial layers is curved dislocations. Representative examples are shown in Fig. 7, marked with triangles. The image was obtained on a sample with 50 m epilayer, 50 m buffer layer, and 10 m of remaining substrate using 共11− 20兲 reflection. Curved dislocations are also visible in Figs. 2, 4, and 6共a兲, as mentioned in the previous section. As can be estimated from the length of the dislocation lines projected to the off-cut direction, some of the curved J. Appl. Phys. 101, 053517 共2007兲 FIG. 8. Transmission x-ray plan-view 共11− 20兲 topograph showing basal plane dislocation half-loops nucleated from a point source close to the epilayer surface. The step-flow direction is marked with an arrow at the right top corner. The positions of the epilayer surface and buffer/substrate interface on one basal plane are labeled with two white lines. basal plane dislocations continue through the entire epitaxial layer, while others extend only within the buffer layer, as the three marked with triangles in Fig. 7. This observation was also supported by gradual removal experiments. The curved basal plane dislocations which only stay in the buffer layer may have converted to threading edge dislocations at the epilayer/buffer interface. There are several even shorter BPDs visible in Fig. 7. Their exact locations in the epilayer/ buffer/substrate structure are not clear. Although the morphology of curved dislocations is quite diverse, most of them have a scalloped shape with lobes bowing out towards the substrate side. Such morphology is indicative of a moving dislocation which was pinned at several points. A representative example is the curved dislocation at the right bottom corner of Fig. 7. Two pinning points along the dislocation line are marked with arrows. The direction of lobes indicates the direction of dislocation motion which is towards the substrate. The Burgers vector of the curved basal plane dislocations was determined to be along 关11− 20兴, parallel to the off-cut direction. All of the above observations are indicative of the 4H-SiC epitaxial layers being under stress, which is also consistent with the characteristics of interfacial dislocations described in the previous section. An additional indication of the presence of significant stresses in the epitaxial layers was provided by observation of dislocation pile ups shown in Fig. 8. The topograph was obtained using 共11− 20兲 reflection on a sample from the epiwafer with thick buffer layer and with 10 m of remaining substrate. The arrow at the right top corner points the stepflow direction. The corresponding positions of epilayer surface and buffer/substrate interface on one basal plane are marked by two white lines. The image shows a number of semicircular dislocation lines terminating on the epilayer surface. The dislocations apparently nucleated at the point source located at the center of the semicircular loops close to the surface of the epilayer. The dislocations then moved towards the substrate and piled up at the buffer/substrate interface. The fact that the dislocations did not propagate into the substrate could be due to the reversal of the stress sign which [This article is copyrighted as indicated in the article. Reuse of AIP content is subject to the terms at: http://scitation.aip.org/termsconditions. Downloaded to ] IP: 158.108.130.130 On: Tue, 14 Apr 2015 10:49:44 053517-7 Zhang et al. J. Appl. Phys. 101, 053517 共2007兲 FIG. 9. 共a兲 Transmission x-ray plan-view 共−2110兲 topograph showing three micropipes with basal plane dislocation 共BPD兲 loops around them. The inset shows a higher magnification image of the BPD loops around the micropipe labeled with a triangle. 共b兲 Optical image of the same area after molten KOH etching. The three micropipes were marked with white arrows. 关共c兲–共e兲兴 Optical images of corresponding micropipe open cores on back side 共C face兲 of the sample. could be expected if the stress was induced by the misfit between epitaxial layers and substrate. Curved dislocations could also be seen in Fig. 8. Our topography observations of curved dislocations are consistent with images obtained by electroluminescence on 4H-SiC p-i-n diodes.4–6 Most of the dislocations observed by electroluminescence were believed to be connected with basal plane dislocations in the substrates. In addition, Tsuchida et al.29 observed similar features of basal plane dislocations by x-ray topography in 4H-SiC epilayers grown on 共0001兲 and 共000− 1兲 substrates with off-cut direction towards 关1 − 100兴. The dislocations tended to align roughly parallel to the step-flow direction during epitaxial growth and had a mixed or pure edge character. C. Circular loop dislocations around micropipes Micropipes are superscrew dislocations with hollow cores.32,33 Basal plane dislocations around micropipes have been observed in the bulk material in the form of circular loops.33,34 Similar features, i.e., circular basal plane dislocation loops, were also observed around micropipes in the epilayers. Figure 9共b兲 shows the optical image of the etch pattern of an area on the epilayer surface with three micropipes in it 共marked with white arrows兲. The magnified images of their corresponding open cores on the back side 共C face兲 are shown in Figs. 9共c兲–9共e兲. The defect located in the lower right corner of Fig. 9共b兲 was actually composed of an array of micropipes easily distinguishable in Fig. 9共e兲. Plan-view x-ray topographs of the same area were obtained using 共−2110兲 reflection, as shown in Fig. 9共a兲. The step-flow direction and the g vector are labeled with two arrows. The substrate was totally removed, thus only defects in the epilayer were imaged. Circular loops of basal plane dislocations could be seen around each of the three micropipes. The inset of Fig. 9共a兲 shows a higher magnification image of the BPD loops around the micropipe labeled with a triangle. The dislocation density near the center of micropipes is too high to permit resolving individual dislocations. The BPD loops extend up to 300 m from the micropipes with the number of loops and their spatial extent correlating with the total Burgers vector of the defects. For example, higher density of BPD loops and larger spatial extent were observed around the micropipe array at the lower right corner of Fig. 9共a兲 than the other two lone micropipes shown in the same figure. All six prismatic reflections were used to determine Burger’s vectors of the BPD loops. Different dislocation loops were out of contrast under different reflections, indicating that they had different Burgers vectors. Our observation is similar to that reported on the bulk SiC crystal by Pirouz33 and Vetter and Dudley34 using transmission electron microscopy 共TEM兲. TEM provided a higher resolution than x-ray topography so that partial dislocations separated by stacking faults were identified. Twigg et al.35 also reported observation of faulted dislocation loops near micropipe in 4H-SiC p-i-n diodes. The high density of basal plane dislocations around micropipes in epilayers could not be explained by mobile BPDs pinned by the superscrew dislocations since the BPD density in epilayers is generally low. Also the model could not explain why a higher density of BPDs is associated with an array of micropipes than with a lone micropipe. A more plausible model could be that the basal plane dislocations nucleate at the micropipes. However, if the micropipes are pure screw dislocations with Burger’s vector along 关0001兴, they should not produce shear stresses resolved in the basal plane. This apparent contradiction needs to be resolved. [This article is copyrighted as indicated in the article. Reuse of AIP content is subject to the terms at: http://scitation.aip.org/termsconditions. Downloaded to ] IP: 158.108.130.130 On: Tue, 14 Apr 2015 10:49:44 053517-8 In addition to the three types of basal plane dislocations discussed in this paper, we have observed two more types that bound stacking faults in the epitaxial layers. Their morphologies, structures, and nucleation mechanisms will be discussed in separate publications. IV. CONCLUSIONS Three types of basal plane dislocations in 4H-SiC homoepitaxial layers were differentiated based on their morphologies observed in the plan-view x-ray topographs. These are interfacial dislocations, curved dislocations, and circular loop dislocations around micropipes. The first two types have a Burgers vector along the off-cut direction and their morphologies are largely consistent with both types moving towards the substrate during epitaxial growth under the influence of shear stress. They are either produced by glide of the BPDs propagating from the substrate into epitaxial layers or by BPD nucleation on the surface followed by glide towards the epilayer/substrate interface. Basal plane dislocation loops appear to nucleate around micropipes throughout the epitaxial growth. They could extend several hundred microns from the nucleation source and have all three possible 具11− 20典 Burgers vectors. ACKNOWLEDGMENT This work was supported in part by ONR Grant No. N00014-02-C-0302, monitored by Dr. Harry Dietrich. 1 J. Appl. Phys. 101, 053517 共2007兲 Zhang et al. J. P. Bergman, H. Lendenmann, P. A. Nilsson, U. Lindefelt, and P. Skytt, Mater. Sci. Forum 353–356, 299 共2001兲. 2 H. Lendenmann, F. Dahlquist, N. Johansson, R. Soderholm, P. A. Nilsson, J. P. 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