Using grazing-incidence x-ray diffraction and scanning tunneling microscopy (STM), we show that the thermal decomposition of an electronic-grade wafer of 6H-SiC after annealing at increasing temperatures TA between 1080 and 1320 °C leads to the layer-by-layer growth of unconstrained, heteroepitaxial single-crystalline graphite. The limited width of the in-plane diffraction rod profiles of graphite reveals large terraces, with an average size larger than 200 Å and a very small azimuthal disorientation. The overlayer is unstrained and adopts the crystalline parameter of bulk graphite even at the smallest coverage studied, which corresponds to a single graphene plane, as inferred from the flat out-of-plane diffraction profile. By increasing TA, additional graphene planes can be grown below this graphite layer from the solid-state decomposition of SiC, forming the AB stacking of Bernal graphite. A C-rich precursor is evidenced in STM by an intrinsic (6×6) reconstruction made of ordered ring or starlike structures. The resulting epitaxial film is indistinguishable from a bulk graphite single crystal.
Phase contrast images of dislocation micropipe in SiC crystal are experimentally studied at various distances from the sample using synchrotron white beam. Computer simulation of these images enabled us to understand the peculiarities of image formation and measure the diameter of the micropipe. The phase contrast imaging of micropipes without monochromator is explained by the absorption of x rays in a thick (490μm) SiC crystal, effectively forming a high brilliance radiation spectrum with a pronounced maximum at 16keV.
Phase-sensitive synchrotron radiation (SR) radiography was combined with x-ray diffraction topography to study structural defects of SiC crystals. The particular bulk SiC crystals examined had a low micropipe density and a hexagonal habitus composed of prismatic, pyramidal, and basal faces well developed. X-ray diffraction topography images of the sliced (0001) wafers, which were formed due to the complex lattice distortions associated with defective boundaries, demonstrated the existence of two-dimensional defective boundaries in the radial direction, normal to the (0001) planes. In particular, those parallel to the 〈1120〉 directions extended rather far from the seed. On the other hand, by phase-sensitive SR radiography the effect of micropipe collection was detected. Micropipes grouped mostly in the vicinities of the defective boundaries but rarely appeared between groups. Some general remarks about possible reasons for the development of such peculiar defect structures were made.
Formation of pores at foreign polytype boundaries in bulk SiC crystals is studied by means of synchrotron radiation phase-sensitive radiography, optical and scanning electron microscopies, and color photoluminescence. It is demonstrated that pores are formed through coalescence of micropipes and extend along the polytype boundaries by means of micropipe absorption. A theoretical model is suggested, which describes the micropipe absorption by an elliptic pore nucleated at the boundary of a foreign polytype inclusion. It is shown that depending on the inclusion distortion, the pore can either be a separate micropipe, or grow up to a certain length, or occupy the whole facet of the inclusion.
The role of micropipes in pore formation in SiC crystals with foreign polytype inclusions is studied by means of synchrotron phase sensitive radiography, optical and scanning electron microscopies, and color photoluminescence. The pores at the inclusion boundaries are revealed, and their shapes and locations are analyzed. It is found that the pores arise due to the attraction of micropipes by the foreign polytype interfaces, followed by micropipe coalescence. The observed pores have tubular or slit shapes. Tubular pores nucleate at the inclusion corners, where the inclusion-associated stresses are concentrated. Slit pores spread between them and follow the shape of the inclusion boundaries. We explain the observations within a two-dimensional model of elastic interaction between micropipes and inclusion boundaries, which accounts for free surfaces of micropipes.
Synchrotron phase sensitive radiography, optical and scanning electron microscopies, and color photoluminescence have been used to study the interaction of micropipes with foreign polytype inclusions in 4H-SiC bulk crystals grown on 6H-SiC substrates. This combination of techniques confirms that micropipes agglomerate at the polytype inclusions and merge into pores. A mechanism for this phenomenon is suggested based on a three-dimensional theoretical model; the inclusion boundaries elastically interact with micropipes, causing them to migrate from the bulk to their equilibrium positions at the polytype boundaries. The turning of micropipes towards the inclusions is experimentally demonstrated, and the reduction of their density in nearby regions is revealed. Supported by experimental observations, our model helps to understand the pore formation and expansion in SiC bulk crystals.
We show that x-ray phase contrast images of some objects with a small cross-section diameter d satisfy a condition for a far-field approximation d ≪ r
1 where r
1 = (λz)1/2, λ is the x-ray wavelength, z is the distance from the object to the detector. In this case the size of the image does not match the size of the object contrary to the edge detection technique. Moreover, the structure of the central fringes of the image is universal, i.e. it is independent of the object cross-section structure. Therefore, these images have no detailed information on the object.
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