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.

The large-scale CT system GULLIVER was recently put into operation at the Rheinland-Pfälzische Technische Universität (RPTU) in Kaiserslautern (Germany). The project, which was launched in 2019 as a result of a competition between various German universities and research institutions, aims to use Computed Tomography (CT) to examine real-scale building components under the most realistic load conditions possible, as is customary in materials testing. The CT measurement is intended to provide new insights into the fatigue dynamics inside these concrete structures, which are up to 6 m long and 1 m wide, by detecting minimal cracks of up to 100 microns in size at the point of load application. The special design of the system and the components installed, open up completely new fields of application for high-energy CT that were previously not available. Particularly noteworthy is the system's gantry-type manipulation unit, whose use has so far been limited primarily to medical diagnostics, as well as the X-ray components used, which open up completely new fields of application for CT in terms of energy and resolution. But also, the processing of the resulting huge data of approx. 10,000 × 10,000 × 2,000 voxels generated in the system represents a particular challenge for the image processing and evaluation to be carried out following the measurement. In this publication, we present the project funded by the German Research Foundation (DFG) and its development containing the measurement results achieved during the current completion of the system as well as the status of the processing procedures developed. In addition, the future measurement campaigns planned with the system are presented and the possibilities to access the innovative testing system for own research activities are explained.

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.

For the fundamental understanding and the technological development of the ammonothermal method for the synthesis and crystal growth of nitrides, an in situ monitoring technique for tracking mass transport of the nitride throughout the entire autoclave volume is desirable. The feasibility of using high-energy computed tomography for this purpose was therefore evaluated using ex situ measurements. Acceleration voltages of 600 kV were estimated to yield suitable transparency in a lab-scale ammonothermal setup for GaN crystal growth designed for up to 300 MPa operating pressure. The total scan duration was estimated to be in the order of 20 to 40 min, which was sufficient given the comparatively slow crystal growth speed in ammonothermal growth. Even shorter scan durations or, alternatively, lower acceleration voltages for improved contrast or reduced X-ray shielding requirements, were estimated to be feasible in the case of ammonoacidic growth, as the lower pressure requirements for this process variant allow for thinned autoclave walls in an adapted setup designed for improved X-ray transparency. Promising nickel-base and cobalt-base alloys for applications in ammonothermal reactors with reduced X-ray absorption in relation to the maximum operating pressure were identified. The applicability for the validation of numerical simulations of the growth process of GaN, in addition to the applicability of the technique to further nitride materials, as well as larger reactors and bulk crystals, were evaluated.

In this study we report on the first continuous records of three dimensional firn structure reconstructions using archive pieces of firn cores that cover the whole depth range of firn starting from surface down to the transition to bubbly ice. The CT-measurements have been performed on 1m-core segments with the means of the AWI-X-ray-computer tomograph especially designed for ice applications. Flyby recording in helical mode under a time-optimized measurement protocol enabled us to reduce the scanning time to 25 minutes per meter firn. The reconstructed volumes have a spatial resolution of 120 µm, giving about 1 million cross-section images per firn core. The analytical work flow includes three steps of pre-processing with denoising, image segmentation and a manual check for outliers at break positions and a layer-wise (5.5 mm thick) calculation of several geometrical parameters like density, ice and pore cluster sizes, intercept lengths, autocorrelation functions, structural anisotropy, Euler number (connectivity), coordination number, bubble number density, closed and open porosity.The method was applied to archive pieces of EGRIP-S6 (firn air pumping site, 2018, North-East-Greenland, 75.6°N ,35.9°W), B40 (Kohnen station, 2013, Dronning Maud Land, East Antarctica, 75.0°S, 0.1°E) and B51 (CoFi-Traverse 2013, Dronning Maud Land, East Antarctica, 75.1°S ,15.4°E). Temperature and accumulation rates at the different core sites vary between -30°C and -50°C and 130 mm w.eq./a and 40 mm w.eq./a respectively. The selected sites cover a wide range of recent environmental conditions of polar regions.In this contribution we present several fundamental relationships between the derived geometrical parameters. The evolution of firn structure with depth will be discussed in respect to the dominant processes acting at different sintering/densification stages. The potential value for densification modelling, gas transport and enclosure modelling will be highlighted.

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.