Aloysius Sakwe

On the lattice parameters of silicon carbide

The thermal expansion coefficients of the hexagonal SiC polytypes 4H and 6H and with Al and N dopants have been determined for temperatures between 300 and 1770 K. Further, a set of the room temperature lattice parameters in dependence on doping with N, Al, and B has been obtained. Data for the thermal expansion were taken on a triple axis diffractometer for high energy x rays with a photon energy of 60 keV, which allows the use of large single crystals with a volume of at least 6×6×6 mm3 without the need to consider absorption. The room temperature measurements for samples with different dopants have been performed on a four-circle diffractometer. The thermal expansion coefficients along the a- and c-directions, α11 and α33, increase from 3×10−6 K−1 at 300 K to 6×10−6 K−1 at 1750 K. It is found that α11 and α33 are isotropic within 107 K−1. At high temperatures both coefficients for doped samples are ∼0.2×10−6 and 0.3×10−6 K−1 lower than for the undoped material.

Analysis of Graphitization during Physical Vapor Transport Growth of Silicon Carbide

We have analyzed the graphitization process of the source material during physical vapor transport growth of SiC by comparison of experimental monitoring (digital x-ray imaging, and 13 C-labeling) and 2D numerical modeling of the sublimation and recrystallization process. Growth runs under different conditions (temperature and inert gas pressure) were used for verification of the calculated source evolution. Effects like formation of a condensed disk on top of the source material, consumption of SiC powder close to the hot graphite walls, mass transport through the core part and along the side walls could be confirmed. The rate of the sublimation and recrystallization effect, however, was overestimated by the model in the range of the experimental parameters in this study. Regardless of the latter, the crystal growth rate was described very well (modeling: 280µm/h, experiment: 310µm/h and 300µm/h).

Thermal Expansion Coefficients of 6H Silicon Carbide

The thermal expansion of 6H Silicon Carbide with different dopant concentrations of aluminum and nitrogen was determined by lattice parameter measurements at temperatures from 300 K to 1575 K. All samples have a volume of at least 6 x 6 x 6 mm3 to ensure that bulk properties are measured. The measurements were performed with a triple axis diffractometer with high energy x-rays with a photon energy of 60 keV. The values for the thermal expansion coefficients along the a- and c-direction, α11 and α33, are in the range of 3·10-6 K-1 for 300 K and 6·10-6 K-1 for 1550 K. At high temperatures the coefficients for aluminum doped samples are approximately 0.5·10-6 K-1 lower than for the nitrogen doped crystal. α11 and α33 appear to be isotropic.

Basal Plane Dislocation Dynamics in Highly p-Type Doped versus Highly n-Type Doped SiC

The long term performance of today’s SiC based bipolar power devices suffer strongly from stacking fault formation caused by slip of basal plane dislocations, the latter often originating from the n-type doped SiC substrate wafer. In this paper, using sequentially p-type / n-type / p-type doped SiC crystals, we address the question, whether basal plane dislocation generation and annihilation behaves differently in n-type and p-type SiC. We have found that basal plane dislocations are absent or at least appear significantly less pronounced in p-type doped SiC, which may become of great importance for the stacking fault problem in SiC.

Growth and Characterization of 13C Enriched 4H-SiC for Fundamental Materials Studies

We have carried out the growth and basic characterization of isotopically enriched 4HSi 13C crystals. In recent years the growth of 13C enriched 6H-SiC has been performed in order to carry out fundamental materials studies (e.g. determination of phonon energies, fundamental bandgap shift, carbon interstitial defect study, analysis of the physical vapor transport (PVT) growth process). For electronic device applications, however, the 4H-SiC polytype is the favored material, because it offers greater electron mobility. In this paper we present the growth of 4H-Si13C single crystals with up to 60% of 13C concentration. From a physical point of view we present first results on phonons as well as the fundamental bandgap energy shift due to 13C incorporation into the SiC lattice.

Development of a KOH Defect Etching Furnace with Absolute In-Situ Temperature Measurement Capability

Etching temperature and time are important parameters in the etching of SiC single crystals in molten KOH for defect studies. However, comparison of results of different research groups is difficult because of the way temperature measurements are being carried out. Until now the temperature of the melt has been measured indirectly with a temperature sensor placed outside the melt on the outer walls of the crucible of the etching furnace, resulting in varying etching conditions for varying setup designs. In this paper we developed an etching furnace with the capability of measuring the absolute temperature in-situ directly in the KOH melt. A new thermoelement, resistant to hot molten KOH was developed. Temperature profile measurements of the molten KOH were carried out and a calibration curve of the furnace was obtained. Based on our temperature measurements, we found that etching at 530 °C for 5 minutes was optimal for defect characterisation, both for defect statistics and for distinguishing between the etch pit morphologies. At 550 °C the etch pits become too large, overlap each other and the etching is no longer defect selective.

Impact of Compensation on Optical Absorption Bands in the Below-Bandgap Region in n-Type (N) 6H-SiC

We present an optical method for the determination of the charge c ri r concentration as well as the compensation level based on absorption measurements at roo m temperature in n-type 6H-SiC. Below band-gap absorption bands (BBGA) are best fitted by a Fano like shape. Calibration plots are provided for evaluation of the charge carrier concentration f rom the peak area of the BBGA. The compensation level is derived from the comparison of th e peak area of the BBGA and the absolute peak value.

Impact of n-Type versus p-Type Doping on Mechanical Properties and Dislocation Evolution during SiC Crystal Growth

The origin of dislocation evolution during SiC crystal growth is usually related to lattice relaxation mechanisms caused by thermal stress. In this paper we discuss dislocation generation and dislocation propagation related to doping and suppression of basal plane dislocations, the latter being of particular interest for bipolar electronic devices. We have prepared alternating p-/n-/pdoped SiC crystals using the donor nitrogen and the acceptors aluminum or boron. In addition we determined the mechanical properties of n-type and p-type SiC; in particular we measured the critical shear stress by nano-indentation on c-plane and a-plane 6H-SiC surfaces. A considerably lower basal plane dislocation density is found in aluminum as well as in boron doped p-type SiC compared to nitrogen doped n-type SiC. It is concluded that the explanation of the reduced basal plane dislocation density in p-type SiC needs the consideration of electronic as well as mechanical effects.

Bulk Growth of SiC

The paper reviews the basics of SiC bulk growth by the physical vapor transport (PVT) method and discuss current and possible future concepts to improve crystalline quality. In-situ process visualization using x-rays, numerical modeling and advanced doping techniques will be briefly presented which support growth process optimization. The “pure” PVT technique will be compared with related developments like the so called Modified-PVT, Continuous-Feeding-PVT, High-Temperature-CVD and Halide-CVD concepts. Special emphasis will be put on dislocation generation and annihilation and concepts to reduce dislocation density during SiC bulk crystal growth. The dislocation study is based on a statistical approach. Rather than following the evolu-tion of a single defect, statistic data which reflect a more global dislocation density evolution are interpreted. In this context a new approach will be presented which relates thermally induced strain during growth and dislocation patterning in networks.

Efficient Image Segmentation for Detection of Dislocations in High Resolution Light Microscope Images of SiC Wafers

The determination of dislocation density and in particular the dislocation distribution in SiC wafers is of particular interest for SiC crystal growth development and production. We present an image recognition tool allowing the wafer analysis with specific needs for SiC. In the first stage of expansion, micropipes are selected and counted from SiC wafers that have been etched by KOH.