Papers by Author: Roland Madar

Abstract: The development of 3C-SiC crystals from <0001> oriented hexagonal seed has always suffered from the systematic twinning which appears during the nucleation step of the layer. Using the continuous feed – Physical Vapour Transport (CF-PVT) growth process, we succeeded in growing single domain 3C-SiC crystals. To explain that, we propose in this work, a model based on the interaction between the lateral expansion anisotropy of 3C-SiC nuclei and the step flow growth front. Depending on the step edges direction, we can obtain one 3C orientation developing simultaneously with the vanishing of the other one. This model is confirmed by cross sectional HRTEM observation of the α-β interface.

Abstract: The growth of 3C-SiC polycrystal and 6H-SiC homoepitaxial layers from Metal-Si alloys is carried out as function of temperature and propane partial pressure. Based on the vapourliquid- solid mechanism, we present a new configuration for the growth of SiC which could allow first to simplify the liquid handling at high temperature and second to precisely control the crystal growth front. 3C-SiC crystals exhibiting well-faceted morphology are obtained at 1100-1200°C with outstanding deposition rates, varying from 1 to 1.5 mm/h in Ti-Si melt. At 1200-1300°C, thick homoepitaxial 6H-SiC layers were successfully obtained in Co-Si melts, with growth rates up to 200 ,m/h. Details on the experiments will be given and the potentialities of such process for the growth of bulk crystals will be discussed..

Abstract: AlN is considered as the most suitable substrate material for further development of high quality and high performance nitride-based micro- and opto-electronics. AlN ingots are often grown on SiC seeds. To solve the formation of cracks due to the difference in lattice parameters between seed and crystal we chose to “adapt” the lattice mismatch by a buffer layer of the (AlN)x(SiC)1-x solid solution. This paper gives some inputs on the growth of AlN and the solid solution by the sublimation technique, in terms of materials compatibility, hetero- and homo-epitaxial growth of AlN and on the preparation of crack-free solid solution single crystals.

Abstract: Recently, in some silicon carbide single crystals, some micropipes associated with screw dislocation have been observed by X-ray topography and the strain field around them produced images similar to those of screw dislocations with a very large Burgers vector, about 667 nm. The radius of the hole in the centre of the micropipe is less than 10 'm. This value and the theoretical predictions by Frank (about 7.8 mm) using the Burgers vector magnitude show a large discrepancy. In this paper we present Atomic Force Microscopy experiments around this kind of defects. The Burgers vector magnitude of the screw dislocation and the value of the radius have been measured by this technique. Not only one dislocation, but several have been observed around the micropipe. We concluded that it is in better agreement with the Frank theory modified by Cabrera and Levine concerning kinetic effects during the growth.

Abstract: The growth of SiC crystals or epilayers from the liquid phase has already been reported for many years. Even if the resulting material can be of very high structural quality and the possibility to close micropipes was demonstrated, handling the liquid phase still is a challenge. Moreover, it is highly difficult to stabilize the C dissolution front and then to stabilize the growth front over a long growth time. Based on the Vapour-Liquid-Solid mechanism, we present a new configuration for the growth of SiC single crystal which should allow first to simplify the liquid handling at high temperature and second to precisely control the crystal growth front. The process consists in a modified top seeded solution growth method, in which the liquid is held under electromagnetic levitation and fed from the gas phase. In a Co-Si solution fed from a propane flow at 1350°C, thick epitaxial layers of 4H-SiC have been grown at 28 0m/h. The potentiality of this new process will be discussed in the paper.

Abstract: Because of the formation of DPB (Double Positioning Boundary) when starting from a hexagonal <0001> seed, DPB-free 3C-SiC single crystals have never been reported up to now. In a recent work we showed that, using adapted nucleation conditions, one could grow thick 3C-SiC single crystal almost free of DPB [1]. In this work we present the results of a multi-scale investigation of such crystals. Using birefringence microscopy, EBSD and HR-TEM, we find evidence of a continuous improvement of the crystal quality with increasing thickness in the most defected area, at the sample periphery. On the contrary, in the large DPB-free area, the SF density remains rather constant from the interface to the surface. The LTPL spectra collected at 5K on the upper part of samples present a nice resolution of multiple bound exciton features (up to m=5) which clearly shows the high (electronic) quality of our 3C-SiC material.

Abstract: The transfer by wafer-bonding of single-crystalline SiC thin films to a polycrystalline SiC support to obtain a “quasi-wafer” is an attractive way for lowering the cost of silicon carbide wafers. Such a process needs high quality polycrystalline substrates, with controlled and high-level bulk properties (thermal conductivity, electrical resistivity) and with very low surface roughness and surface bowing. Currently, polycrystalline SiC wafers which are available are siliconized SiC or CVD processed SiC wafers. Siliconized ceramic wafers are very heterogeneous (mixture of 3C, 6H, 15R and silicon), while CVD ones are of better quality (homogeneous and textured 3C). However neither the siliconized SiC nor the CVD SiC can be CMP polished with low roughness over large dimension. In this paper, wafers with large and textured grains (> 1cm) are processed and characterized. The polishing of such structures is studied and optimized to obtain low surface roughness. To meet these requirements high temperature processes used for single crystal growth were selected. Structural investigations performed on the grown ingots showed an important influence of the used seed since no preferential crystallographic orientation was observed during the growth. The final polishing quality was of high level but step heights were observed between grains.

Abstract: The development of the Continuous Feed Physical Vapour Transport (CF-PVT) process requires a perfect control of each phenomenon in the growth cell. Along this line, the present paper gives some inputs on the CF-PVT mass transfer regimes with respect to the process parameters, both from qualitative and quantitative viewpoints. For example, two boundary cases have been evidenced depending on the temperature. At low temperature, the growth is limited by the sublimation step between the source and the seed. In this case, the CF-PVT process can be roughly assimilated to the classical seeded sublimation technique. At high temperature, the process is limited by the feeding step, i.e. the CVD deposition and infiltration on the lower part of the source. Measurements are correlated to in-situ X-ray imaging. The ability of the X-ray imaging to in-situ qualify and quantify the mass transfer is discussed.

Abstract: QuaSiC TM substrates can be obtained by transferring a single crystal SiC layer onto a poly SiC substrate using the Smart Cut TM technology. The structure evolution of metal bonding (W-Si silicide) layer has been investigated by Transmission Electron Microscopy and X-ray diffraction. Results indicate that the metal bonding film is made of W5Si3. The film is discontinuous and strained. Annealing releases stress at least partially.

Abstract: Thick (111) oriented β-SiC layers have been grown by hetero-epitaxy on a (0001) a-SiC substrate with the Continuous Feed-Physical Vapour Transport (CF-PVT) method. The growth rate was 68 µm/h at a pressure of 2 torr and a temperature of 1950°C. The nucleation step of the β-SiC layer during the heating up of the process was studied in order to manage first the a to b heteropolytypic transition and second the selection of the b-SiC orientation. With a adapted seeding stage, we grew a 0.4mm thick layer almost free of Double Positioning Boundaries on a 30mm diameter sample. First observations of the layer by cross-polarised optical Microscopy are presented both in planar view and in cross section geometry.