HAL is a multi-disciplinary open access archive for the deposit and dissemination of scientific research documents, whether they are published or not. The documents may come from teaching and research institutions in France or abroad, or from public or private research centers. L’archive ouverte pluridisciplinaire HAL, est destinée au dépôt et à la diffusion de documents scientifiques de niveau recherche, publiés ou non, émanant des établissements d’enseignement et de recherche français ou étrangers, des laboratoires publics ou privés. Kinetics of the 3C-6H polytypic transition in 3C-SiC single crystals: a diuse X-ray scattering study D. Dompoint, Alexandre Boulle, I. Galben-Sandulache, D. Chaussende, L. Hoa, T. Ouisse, D. Eyidi, J. L. Demenet, M. Beaufort, J. Rabier

demonstrated that the transformation implies the multiplication and ordering of double and triple stacking faults (SFs). The transformation level and root-mean-squared strains associated with the dislocations are determined from the simulations. The defect structure formed during the transition can be rationalized by considering the relative energies of the SFs. Using an axial next-nearest-neighbor Ising interaction model we show that single SFs are not energetically favored, whereas the simultaneous occurrence of double and triple SFs implies that their relative energy difference remains below a critical value (∼8–9%).

The 3C-6H polytypic transition in 3C-SiC single crystals is studied by means of diffuse X-ray scattering (DXS) coupled with numerical simulations. It is shown that the presence of spatially correlated stacking faults (characteristic of this type of re-stacking transition) gives rise to extended diffuse scattering in the reciprocal space perpendicularly to the fault plane. The simulation of the diffuse intensity allows to determine both the volume fraction of transformed material and the transformation level within these regions. It is further shown that the evolution with time and temperature of the transition implies the multiplication and glide of partial dislocations, the kinetics of which are quantified by means of DXS. (C) 2011 Elsevier B.V. All rights reserved.

The 3C-6H polytypic transition in 3C-SiC single crystals is studied by means of diffuse X-ray scattering (DXS) coupled with transmission electron microscopy (TEM). TEM reveals that the partially transformed SiC crystals contain regions of significantly transformed SiC (characterized by a high density of stacking faults) co-existing with regions of pure 3C-SiC. The simulation of the diffuse intensity allows to determine both the volume fraction of transformed material and the transformation level within these regions. It is further shown that the evolution with time and temperature of the transition implies the multiplication and glide of partial dislocations, the kinetics of which are quantified by means of DXS.

In this work, the kinetics of the 3C-6H polytypic transition in 3C-SiC single crystals are studied in details by means of diffuse x-ray scattering (DXS) coupled with numerical simulations and transmission electron microscopy and optical birefringence microscopy. Upon high-temperature annealing, spatially correlated stacking faults (SFs), lying in the {111} planes, are generated within the crystal and tend to form bands of partially transformed SiC. It is shown that the numerical simulation of the DXS curves allows to unambiguously deduce the transformation level within these bands, as well as the volume fraction corresponding to these bands. Increasing annealing time results (1) in the growth of the partially transformed regions by the glide of the partial dislocations bounding the SFs and (2) in the generation of new SFs within the crystal by means of a double-cross slip motion. The kinetics of each of these mechanisms are presented and discussed with respect to the annealing temperature, the initial SF density and crystalline quality.

Free carrier absorption (FCA) and picosecond light-induced transient grating (LITG) techniques were applied to study the photoelectrical properties of 3C-SiC(111) homoepitaxial layers grown by CVD method on VLS (vapour-liquid-solid) grown seeds. The thickness of the CVD layers was ~10.5 µm with non-intentional type doping of n (~ 1017 cm-3) or p (<1015 cm-3). The carrier lifetime and the diffusion coefficient were measured as the function of the sample temperature, the injected excess carrier density at different growth parameters. At room temperature the ambipolar diffusion coefficient was Da=2.5-3 cm2/s, while the lifetime was in the range of 12-18 ns. The best structural and electrical properties were obtained for a CVD layer grown at high, 1600 °C temperature.

The X-ray scattering of partially transformed 3C-SiC single crystals is considered in detail. Extended diffuse scattering streaks, originating from stacking faults (SFs) lying in the {111} planes, are clearly observed in the wide-range reciprocal-space maps. The intensity distribution along the diffuse streaks is simulated with a model including the contributions of the diffuse scattering originating from the SFs [based on the pioneering theoretical description given by Kabra, Pandey & Lele (1986). J. Mater. Sci. 21 , 1654–1666], the coherent scattering emanating from untransformed areas of the crystals and all θ-dependent terms that affect the scattered intensity (the layer structure factor, the irradiated volume and the polarization of the beam). The quantitative simulation of the diffuse streaks reveals that the transformation occurs through the glide of partial dislocations and allows one to derive the transformation level. It is shown that the 3C polytype is indeed unstable at high temperature. However, it is further shown that defect-free 3C-SiC single crystals remain stable at temperatures where 3C-SiC is known to be usually unstable (2173 K). The origin of this apparent stability is very likely of kinetic nature, i.e. the lack of crystalline defects inhibits the transformation.

The stability of (001)‐oriented 3C silicon carbide crystals is studied by a method coupling high resolution x‐ray diffraction and numerical simulations. The analysis of the diffuse scattering intensity distribution along selected directions in reciprocal space allows us to obtain qualitative and quantitative informations regarding the 3C‐6H transition. Our latest results concerning the influence of the initial crystal quality (presence of defects) and of annealing time on the 3C‐6H transition are presented in this article.

Stacking faults (SFs) and the 3C‐6H polytypic transition in thick (001)‐oriented 3C‐SiC crystals are studied by means of diffuse X‐ray scattering. The presence of SFs lying in the {111} planes gives rise to streaked reciprocal lattice points with the streaks being parallel to the directions. In the case of low SF densities the defects are uncorrelated and the simulation of the diffuse intensity distribution allows to derive the SF density. In partially transformed crystals, the SFs are spatially correlated which gives rise to an intense and asymmetric diffuse scattering distribution. Its simulation allows to determine both the transformation mechanism and the transformation level.

6H-SiC and 3C-SiC single crystals were simultaneously irradiated at room temperature with 100 keV Fe ions at fluences up to 4 × 1014 cm−2 (∼0.7 dpa), i.e. up to amorphization. The disordering behaviour of both polytypes has been investigated by means of Rutherford backscattering spectrometry in the channelling mode and synchrotron x-ray diffraction. For the first time, it is experimentally demonstrated that the general damage build-up is similar in both polytypes. At low dose, irradiation induces the formation of small interstitial-type defects. With increasing dose, amorphous domains start to form at the expense of the defective crystalline regions. Full amorphization of the irradiated layer is achieved at the same dose (∼0.45 dpa) for both polytypes. It is also shown that the interstitial-type defects formed during the first irradiation stage induce a tensile elastic strain (up to ∼4.0%) with which is associated an elastic energy. It is conjectured that this stored energy destabilizes the current defective microstructure observed at low dose and stimulates the formation of the amorphous nanostructures at higher dose. Finally, the disorder accumulation has been successfully reproduced with two models (namely multi-step damage accumulation and direct-impact/defect-stimulated). Results obtained from this modelling are compared and discussed in the light of experimental data.