The investigation of the interplay of experimental crystal growth runs and computer simulations of the physical vapor transport (PVT) growth process of silicon carbide (SiC) strongly supports the development of the growth technology toward larger crystalline diameters. To apply computer-aided designs of the growth process, a material database is developed that enables quantitative calculations of the temperature distribution inside the growth setup. The model utilizing COMSOL Multiphysics is validated by experimental means using five 100 mm SiC crystal growth runs, two measurement runs in a 100 mm PVT setup, and one SiC crystal growth run in a 75 mm PVT setup, varying in power, pressure, coil position, and reactor geometry. Material data are varied and the impact on the thermal gradients is investigated to trace out critical and noncritical parameters for the accuracy of the simulation. The influence of ambient pressure on the isolation's performance is studied experimentally and this correlation is implemented into the model. Beyond the state of the art, this work presents a modeling approach and handling of material properties for a true scale up of the current 100 mm and 150 mm SiC sublimation growth technologies to 200 mm.
Two 75mm 4H-SiC single crystals are grown by the physical vapor transport (PVT) technique, using different insulation materials. The insulation material of higher thermal conductivity led to an increased radial temperature gradient. The evolution of the growth front was monitored using the in-situ computed tomography (CT). A slightly bent growth interface and a bigger facet are formed during the growth applying a lower radial temperature gradient while a smaller facet and steeper crystal flanks are formed in the case of the larger radial temperature gradient. Micropipes are deflected laterally by large surface steps on the steep crystal flanks and a reduction of threading edge dislocations by 60% is revealed by KOH defect etching.
In this study, the change of mass distribution in a source material is tracked using an in situ computer tomography (CT) setup during the bulk growth of 4H- silicon carbide (SiC) via physical vapor depostion (PVT). The changing properties of the source material due to recrystallization and densification are evaluated. Laser flash measurement showed that the thermal properties of different regions of the source material change significantly before and after the growth run. The Si-depleted area at the bottom of the crucible is thermally insulating, while the residual SiC source showed increased thermal conductivity compared to the initially charged powder. Ex situ CT measurements revealed a needle-like structure with elongated pores causing anisotropic behavior for the heat conductivity. Models to assess the thermal conductivity are applied in order to calculate the changes in the temperature field in the crucible and the changes in growth kinetics are discussed.
Computed tomography using X‐rays is applied during the bulk growth of silicon carbide (SiC) to investigate growth kinetics in situ during the physical vapor transport process. In addition to the standard SiC source material, in particular, a pure solid source SiC block is used. It is found that the growth rate is lowered as the sublimation of gaseous species is limited to the top part of the solid source. The morphological changes in the source area during growth differ significantly compared with the process when conventional powder is used. The formation of multiple growth centers on the surface of the seed is monitored in situ with a computed tomography system. In a series of experiments, the influence of the supersaturation on the growth is examined. The in situ computed tomography shows that the curvature of the growth interface is stronger influenced by the thermal field at higher pressures. A high supersaturation leads to the formation of rather smooth surface morphologies, whereas the formation of large steps on the surface is induced at lower supersaturations.
Today the physical vapor transport process is regularly applied for the growth of bulk SiC crystals. Due to the required high temperature of up to 2400 °C, and low gas pressure of several Mbar inside the crucible, the systems are encapsulated by several layers for heating, cooling and isolation inhibiting the operator from observing the growth. Also, the crucible itself is fully encapsulated to avoid impurities from being inserted into the crystal or disturbing the temperature field distribution. Thus, once the crucible has been set up with SiC powder and the seed crystal, the visible access to the progress of growth is limited. In the past, X-ray radiography has allowed this limitation to be overcome by placing the crucible in between an X-ray source and a radiographic film. Recently these two-dimensional attenuation signals have been extended to three-dimensional density distribution by the technique of computed tomography (CT). Beside the classic X-ray attenuation signal dominated by photoelectric effect, Compton effect and Rayleigh scattering, X-ray diffraction resulting in the crystalline structure of the 4H-SiC superimposes the reconstructed result. In this contribution, the achievable material contrast related to the level of X-ray energy and the absorption effects is analyzed using different CT systems with energies from 125 kV to 9 MeV. Furthermore the X-ray diffraction influence is shown by the comparison between the advanced helical-CT method and the classical 3D-CT.
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