Off-axis 4H-SiC Research Articles

Structural Characterization of Graphene Grown by Thermal Decomposition of Off-Axis 4H-SiC (0001)

We present a nanoscale morphological and structural characterization of few layers of graphene grown by thermal decomposition of off-axis 4H-SiC (0001). A comparison between transmission electron microscopy (TEM) in cross-section and in plan view allows to fully exploit the potentialities of TEM. Such a comparison was used to get information on the number of graphene layers as well as on the rotational order between the layers and with respect to the substrate. Some peculiar structures observed by TEM (wrinkles) could only be systematically measured by atomic force microscopy (AFM). In particular, the density and the height of the wrinkles in the few layers of graphene was investigated.

Growth mechanisms and defect structures of B12As2 epilayers grown on 4 H-SiC substrates

Epitaxial growth of icosahedral B12As2 on c-plane 4H-SiC substrates has been analyzed. On on-axis c-plane 4H-SiC substrates, Synchrotron white beam x-ray topography (SWBXT) revealed the presence of a homogenous solid solution of twin and matrix B12As2 epilayer domains. High resolution transmission electron microscopy (HRTEM) and scanning transmission electron microscopy (STEM) both revealed the presence of an ∼20nm thick, disordered transition layer at the interface. (0003) twin boundaries are shown to possess fault vectors such as 1/3[1–100]B12As2, which originate from the mutual shift between the nucleation sites. On the contrary, B12As2 epilayers grown on c-plane 4H-SiC substrates intentionally misoriented from (0001) towards [1–100] is shown to be free of rotational twinning. SWBXT, HRTEM and STEM all confirmed the single crystalline nature and much higher quality of the films. In addition, no intermediate layer between the epilayer and the substrate was observed. It is proposed that the vicinal steps formed by hydrogen etching on the off-axis 4H-SiC substrate surface before deposition cause the film to adopt a single orientation during nucleation process. This work also demonstrates that c-plane 4H-SiC with offcut toward [1–100] is potentially a good substrate choice for the growth of high-quality, single crystalline B12As2 epilayers for future device applications.

Reduction of Triangular Defects on 100mm 4° off-axis 4H-SiC using a Chloride Based CVD process

ABSTRACTHomoepitaxial layers were grown with very low surface roughness on 4", 4˚ off-axis substrates, but a new kind of large obtuse angled triangular defect that spanned 1000-2000 μm was observed. Process changes resulted in reduction of the size and concentration of these triangular defects from 3.5cm-2 to 0.13cm-2. Both large and small triangular defects were found to have a similar core structure. No degradation in the epitaxial morphology or quality was seen due to the process change. JBS diodes fabricated on wafers with large triangular defects had much higher leakage when the triangular defects were present in the active area of the diodes.

Investigation on AlN epitaxial growth and related etching phenomenon at high temperature using high temperature chemical vapor deposition process

Thick AlN layers were grown by high temperature chemical vapor deposition (HTCVD) on 8° off-axis (0 0 0 1) 4H-SiC, on-axis (0 0 0 1) 6H-SiC and on-axis (0 0 0 1) AlN templates between 900 °C and 1600 °C. The experimental set-up consists of a vertical cold-wall reactor working at low pressure in which the reactions take place on a graphite susceptor heated by induction. The reactants used are ammonia (NH 3) and aluminum chlorides (AlCl x ) species in situ formed via Cl 2 reaction with high purity aluminum wire. As-grown AlN layers have been characterized by Scanning Electron Microscopy (SEM), X-ray diffraction (XRD), Transmission Electron Microscopy (TEM), Optical Profilometry, Atomic Force Microscopy (AFM) and Raman spectroscopy. In this study, the influence of the deposition temperature and the N/Al ratio in the gas phase is studied in order to stabilize epitaxial growth. The epitaxy on AlN template is favored using a low N/Al ratio in the gas phase and a high temperature above 1400 °C. The crystalline quality of epitaxial AlN layers is found to increase with increasing deposition temperature from 1400 to 1500 °C. Growth rates up to 14 μm h −1 have been reached for epitaxial AlN layers. An important etching phenomenon is also observed at high temperature: apparition of pin holes certainly around threading dislocations at 1400–1500 °C and substrate etching at 1600 °C.

Epitaxial Growth of 4H-SiC on 4° Off-Axis Substrate for Power Devices

Homo-epitaxial layers are successfully grown on Si-face 4° off-axis 4H-SiC substrates using the horizontal hot-wall chemical vapor deposition system. The smooth surface without morphological defects is obtained by the optimized in situ etching process and growth temperature. Schottky diodes fabricated on the epilayer present a typical I—V characteristic. This is the first report of Schottky diodes fabricated on 4° off-axis 4H-SiC substrates made in China.

Comparative micro-photoluminescence investigation of ZnO hexagonal nanopillars and the seeding layer grown on 4H-SiC

We report on a comparative micro-photoluminescence investigation of ZnO hexagonal nanopillars (HNPs) and the seeding layer grown on the off-axis 4H-SiC substrate. Transmission electron microscope (TEM) results establish that a thin seeding layer continuously covers the terraces of 4H-SiC prior to the growth of ZnO HNPs. Low temperature photoluminescence (LTPL) shows that ZnO HNPs are only dominated by strong donor bound exciton emissions without any deep level emissions. Micro-LTPL mapping demonstrates that this is specific also for the seeding layer. To further understand the recombination mechanisms, time-resolved micro-PL spectra (micro-TRPL) have been collected at 5 K and identical bi-exponential decays have been found on both the HNPs and seeding layer. Temperature-dependent TRPL indicates that the decay time of donor bound exciton is mainly determined by the contributions of non-radiative recombinations. This could be explained by the TEM observation of the non-radiative defects in both the seeding layer and HNPs, like domain boundaries and dislocations, generated at the ZnO/SiC interface due to biaxial strain.

Weak Localization and Universal Conductance Fluctuations on Epitaxial Graphene Grown on the C-Face of 8°off-Axis 4H-SiC Substrates

We report magnetotransport measurements in single epitaxial graphene layers grown on the C-face of an 8° off-axis 4H-SiC substrate using high temperature annealing conditions with a graphite cap covering the sample. The graphene sheets were found p-type doped, with mobilities varying between 1000 and 11000 cm²/V.s from device to device at 1.6 K. We examine the signature of weak localization and universal conductance fluctuations at weak magnetic field and we show that the phase coherence lengths extracted from the two phenomena are in satisfactory agreement.

Effect of nitrogen impurity on the stabilization of 3C–SiC polytype during heteroepitaxial growth by vapor–liquid–solid mechanism on 6H–SiC substrates

This work reports on the stabilization of 3C–SiC polytype during heteroepitaxial growth by vapor–liquid–solid (VLS) on on-axis and 2° off-axis 6H–SiC(0001) substrates using Si–Ge as liquid phase. It was found that, depending on growth conditions (mainly temperature or nitrogen amount in the reactor), the deposit could be either a complete 3C or 6H–SiC layer or even a mixture of both polytypes. The proportion of 3C inside the deposit increases when 1) nitrogen amount in the reactor increases or 2) temperature is decreased. Though the effect of temperature could be explained in terms of 3C–SiC initial island dissolution, the influence of nitrogen is less obvious but it is shown to be effective at the early stage of growth. Several hypotheses are proposed such as SiC lattice modification by N incorporation or surface effects during the early stage of growth.

Nanoscale structural characterization of epitaxial graphene grown on off-axis 4H-SiC (0001)

In this work, we present a nanometer resolution structural characterization of epitaxial graphene (EG) layers grown on 4H-SiC (0001) 8° off-axis, by annealing in inert gas ambient (Ar) in a wide temperature range (Tgr from 1600 to 2000°C). For all the considered growth temperatures, few layers of graphene (FLG) conformally covering the 100 to 200-nm wide terraces of the SiC surface have been observed by high-resolution cross-sectional transmission electron microscopy (HR-XTEM). Tapping mode atomic force microscopy (t-AFM) showed the formation of wrinkles with approx. 1 to 2 nm height and 10 to 20 nm width in the FLG film, as a result of the release of the compressive strain, which builds up in FLG during the sample cooling due to the thermal expansion coefficients mismatch between graphene and SiC. While for EG grown on on-axis 4H-SiC an isotropic mesh-like network of wrinkles interconnected into nodes is commonly reported, in the present case of a vicinal SiC surface, wrinkles are preferentially oriented in the direction perpendicular to the step edges of the SiC terraces. For each Tgr, the number of graphene layers was determined on very small sample areas by HR-XTEM and, with high statistics and on several sample positions, by measuring the depth of selectively etched trenches in FLG by t-AFM. Both the density of wrinkles and the number of graphene layers are found to increase almost linearly as a function of the growth temperature in the considered temperature range.

Temperature Dependent Structural Evolution of Graphene Layers on 4H-SiC(0001)

In this study we examined the structural evolution of graphene grown on 8° off-axis 4H-SiC(0001) substrates at temperatures from 1600°C to 1700°C in Ar ambient. Morphological transformation of SiC substrate after annealing was examined by Tapping Mode Atomic Force Microscopy. Moreover, by etching-out graphene layers from graphitized SiC substrates in selective trenches we determined the number of graphene layers. Numbers of graphene layers were then independently confirmed by Transmission Electron Microscopy imaging.

Effect of Inter-Well Coupling between 3C and 6H in-Grown Stacking Faults in 4H-SiC Epitaxial Layers

Both 3C and 6H stacking faults have been observed in a low doped 4H-SiC epitaxial layer grown in a hot-wall CVD reactor on a heavily doped (off-axis) 4H-SiC substrate. They appear differently on the different parts of sample, with energetic dispersion ranging from 3.01 eV to 2.52 eV. Since they behave as natural type-II quantum wells in the 4H-SiC matrix, the thickness dependence of the excitonic recombination is investigated using the standard effective mass approximation. The results are discussed in terms of built-in electric field and inter-well coupling effects.

Electrical and Structural Properties of AlGaN/GaN Heterostructures Grown onto 8°-Off-Axis 4H-SiC Epilayers

In this work the electrical and structural properties of AlGaN/GaN heterostructures grown onto 8°-off-axis 4H-SiC epilayers were investigated. A morphological and structural analysis of the samples showed the presence of “V-shaped” near-surface defects in the AlGaN layer, with a preferential orientation along the miscut direction [11-20]. In the presence of these defects an anisotropy of the current-voltage characteristics of high electron mobility transistors (HEMTs), fabricated with two different orientations, was observed. The sheet carrier density ns and the channel mobility n were determined from the device characteristics. The results were discussed considering the possible implications for AlGaN/GaN HEMT technology.

TEM Observation of 8 Deg Off-Axis 4H-SiC (0001) Surfaces Planarized by Catalyst-Referred Etching

We have developed a novel abrasive-free planarization method called catalyst-referred etching (CARE). A CARE-processed 8 deg off-axis 4H-SiC (0001) surface is investigated by cross-sectional transmission electron microscopy (TEM). The surface is composed of alternating wide and narrow terraces with single-bilayer-height steps, which are similar to the structure observed on a CARE-processed on-axis 4H-SiC (0001) surface. These results indicate that the structure appears on CARE-processed surfaces regardless of the off-cut angle.

Geometrical Control of 3C and 6H-SiC Nucleation on Low Off-Axis Substrates

Growth of 3C or 6H-SiC epilayers on low off-axis 6H-SiC substrates can be mastered by changing the size of the on axis plane formed by long terraces in the epilayer using geometrical control. The desired polytype can be selected in thick (~200 µm) layers of both 6H-SiC and 3C-SiC polytypes on substrates with off-orientation as low as 1.4 and 2 degrees. The resultant crystal quality of the 3C and the 6H-SiC epilayers, grown under the same process parameters, deteriorates when lowering the off-orientation of the substrate.

Multidimensional characterization, Landau levels and Density of States in epitaxial graphene grown on SiC substrates

Using high-temperature annealing conditions with a graphite cap covering the C-face of, both, on axis and 8° off-axis 4H-SiC samples, large and homogeneous single epitaxial graphene layers have been grown. Raman spectroscopy shows evidence of the almost free-standing character of these monolayer graphene sheets, which was confirmed by magneto-transport measurements. On the best samples, we find a moderate p-type doping, a high-carrier mobility and resolve the half-integer quantum Hall effect typical of high-quality graphene samples. A rough estimation of the density of states is given from temperature measurements.

Chlorinated precursor study in low temperature chemical vapor deposition of 4H-SiC

Low temperature (1300 °C) chemical vapor deposition (CVD) of SiC has gained interest in the last years for being less demanding in terms of reaction chamber lifetime, but also for allowing higher p-type dopant incorporation. Chloride-based CVD at low temperatures has been studied using chloromethane with tetrachlorosilane or silane, respectively and with or without controlled HCl addition. In this study we explore the use of methyltrichlorosilane (MTS) at growth temperatures (1300 °C) significantly lower than what is commonly used for homoepitaxial growth of SiC (1600 °C). MTS is a molecule containing all the needed precursor atoms; its effects are compared to the standard CVD chemistry, consisting of silane, ethylene, and HCl. Very different chemistries between the two precursor systems are proposed; in the case of MTS, C/Si ratios higher than 1 were required, however using the standard chemistry ratios lower than 1 were needed to obtain a defect-free epitaxial layer. We also demonstrate the need of using Cl/Si ratios as high as 15 to achieve a growth rate of 13 μm/h for 8° off-axis 4H-SiC epitaxial layers at 1300 °C. Limitations due to the low growth temperature are discussed in light of the experimental evidence on the growth mechanism as determined by the morphology degradation and the limited growth rate. Finally a comparison between the epilayers morphology obtained on 4H-SiC substrates with different off-cuts are presented, confirming the importance of lower C/Si ratios for 4° off-axis material and the inevitable growth of the cubic SiC polytype on on-axis substrates.

Hydride vapor phase epitaxy of high structural perfection thick AlN layers on off-axis 6H-SiC

The employment of more than 10 μm thick AlN epilayers on SiC substrates for AlGaN/GaN high-electron-mobility transistors (HEMTs) substantially raises their performance in high-power energy-efficient amplifiers for 4G wireless mobile stations. In this paper, structural properties and surface morphology of thick AlN epilayers deposited by hydride vapor phase epitaxy (HVPE) on off-axis conductive 6H-SiC substrates are reported. The epilayers were examined in detail by high-resolution X-ray diffraction (XRD), atomic force microscopy (AFM), Nomarski differential interference contrast (DIC), scanning electron microscopy (SEM), and selective wet chemical etching. At optimal substrate preparation and growth conditions, a full width at half-maximum (FWHM) of the XRD rocking curve (RC) for the symmetric (00.2) reflex was very close to that of the substrate (less than 40 arcsec) suggesting low screw dislocation density in the epilayer (∼10 6 cm −2) and small in-plane tilt misorientation. Reciprocal space mapping around asymmetric reflexes and measured lattice parameters indicated a fully relaxed state of the epilayers. The unit-cell-high stepped areas of the epilayers with 0.5 nm root mean square (RMS) roughness over 1×1 μm 2 scan were alternated with step-bunching instabilities up to 350 nm in height. Low warp of the substrates makes them suitable for precise epitaxy of HEMT structures.

Electronic properties of BaTiO3/4H-SiC interface

The possibility of barium titanate (BaTiO 3 ) application in silicon carbide (SiC) technology has been elaborated in terms of the dielectric film quality and properties of the BaTiO 3 /4H-SiC interface. High resistivity, high-k thin films containing La 2 O 3 admixture were applied as gate insulator of metal-insulator-semiconductor (MIS) structure. The thin films were deposited by means of radio frequency plasma sputtering (RF PS) of sintered BaTiO 3 + La 2 O 3 (2 wt.%) target on 8° off-axis 4H-SiC (0001) epitaxial layers doped with nitrogen. The results of current-voltage and capacitance-voltage measurements are presented for MIS capacitors.

Growth of monolayer graphene on 8° off-axis 4H–SiC (000–1) substrates with application to quantum transport devices

Using high temperature annealing conditions with a graphite cap covering the C-face of an 8° off-axis 4H–SiC sample, large and homogeneous single epitaxial graphene layers have been grown. Raman spectroscopy shows evidence of the almost free-standing character of these monolayer graphene sheets, which was confirmed by magnetotransport measurements. We find a moderate p-type doping, high carrier mobility, and half integer quantum Hall effect typical of high quality graphene samples. This opens the way to a fully compatible integration of graphene with SiC devices on the wafers that constitute the standard in today’s SiC industry.

Investigation of dislocations in 8° off-axis 4H-SiC epilayer

This paper reports that the etching morphology of dislocations in 8° off-axis 4H-SiC epilayer is observed by using a scanning electronic microscope. It is found that different types of dislocations correspond with different densities and basal plane dislcation (BPD) array and threading edge dislocation (TED) pileup group lie along some certain crystal directions in the epilayer. It is concluded that the elastic energy of threading screw dislocations (TSDs) is highest and TEDs is lowest among these dislocations, so the density of TSDs is lower than TEDs. The BPDs can convert to TEDs but TSDs can only propagate into the epilyer in spite of the higher elastic energy than TEDs. The reason of the form of BPDs array in epilayer is that the big step along the basal plane caused by face defects blocked the upstream atoms, and TEDs pileup group is that the dislocations slide is blocked by dislocation groups in epilayer.