Growth Of SiC Research Articles

Improvement of curing efficiency and heat resistance of CFRP by the growth of SiCNWs on CF

Carbon fiber-reinforced polymer composites are widely used in modern industry. However, poor heat transfer between layers of carbon fiber cloth during the curing process leading to poor curing of the substrate, long curing cycles, and excessive heat accumulation has become an urgent problem to be solved. A common approach is dispersing highly thermally conductive fillers in the polymer matrix to improve the curing efficiency of the composites. Different from adding fillers, we report a novel method of in situ growth of SiC nanowires (SiCNWs) on the surface of carbon fiber (CF) by the chemical vapor deposition (CVD) method and study the effects of CVD deposition time on curing efficiency and thermal stability of the composites. The results indicate that the nano bridge effect of SiCNWs significantly improves the curing efficiency of the composites. Compared with pure CF/epoxy composites, the curing efficiency can be increased by 38.72%. The cross-linking point between SiCNWs and the resin matrix enhances the thermal stability of the composites and increases the heat resistance index ( T HRI) by 8.4°C.

Effect of boron on phase, nanostructure, and thermal stability of polycarbosilane-derived SiC ceramics

The current study explores the formation, evolution, and thermal stability of polymer-derived SiBC at high temperatures. It focuses on the phase evolution of SiBC ceramics derived from the doping of boron in an allyl-containing polycarbosilane preceramic polymer after 1200 °C to 1600 °C pyrolysis. Different SiBC ceramic monoliths have been obtained. Boron is incorporated into the carbon phase at lower pyrolysis temperatures but into both the carbon phase and the SiC lattice structure at high pyrolysis temperatures. B–C bonds form in SiBC and hinder the growth of graphitic carbon and SiC. Boron improves the densification and thermal stability of the SiBC ceramics. This work provides an improved understanding of boron effects in polymer-derived SiC nanostructures at high temperatures.

Effect of Fe-Co catalysis on the temperature field distribution during the growth of 3C-SiC fibers synthesised by microwave heating

Microwave heating produce local hot spots on materials, which result in uneven heating and other issues. Regulate the microwave temperature field using different catalyst combinations such as Fe (NO3)3·9H2O and Co (NO3)2·6H2O. The electromagnetic and temperature field distributions of 3C–SiC fibers and the molecular dynamics of the SiC interfacial growth process and interfacial oxidation reaction during microwave heating in the presence of a catalyst were simulated and calculated respectively. The results show that the combination of Fe and Co at 9 wt% catalyst concentration can effectively improve the electromagnetic loss capability of SiC fibers. The Fe and Co bimetallic catalysed synthesis of 3C–SiC fibers follows a vapor–liquid–solid growth mechanism. The Fe–Si and Fe–Co–Si alloy phases can induce 3C–SiC growth along (111) crystal faces. The simultaneous exothermic reactions provide a highly catalytically active growth environment that facilitates the enhancement of microwave temperature field uniformity. This phenomenon facilitated the synthesis of 3C–SiC fibers.

Determination of Thermal Properties of Carbon Materials above 2000 °C for Application in High Temperature Crystal Growth

AbstractThis work reports on the determination of the heat conductivity of high temperature stable carbon materials in the temperature range well above 2000 °C where classic material characterization methods fail. Dense graphite (DG) materials as well as rigid and soft felt isolation (RFI/SFI) components have been investigated which are used during crystal growth of SiC by the physical vapor transport method (PVT) in the temperature regime of 2000 and 2400 °C. The applied materials characterization methods include low temperature physical heat conductivity measurements using laser flash analysis (LFA) in the temperature range 25–1200 °C, data extrapolation to elevated temperatures up to 2400 °C, and a correlation of heating processes and computer simulation of the temperature field of different hot zone designs. Using this approach, the calculated temperatures and experimentally determined values with an error of less than ± 2% at 2400 °C can be merged.

Li2O addition as a means of achieving low-temperature densification of SiC ceramic

In order to achieve low-temperature densification of SiC ceramic, β-SiC nanopowder was doped with Li2O together with Y2O3–Al2O3–MgO as sintering aids, and then spark plasma sintered at temperatures ranging from 1450 °C to 1600 °C for 30 min under 30 MPa pressure in argon. The densities, microstructures and mechanical properties of SiC ceramics were systematically investigated, in comparison to the counterparts sintered with Y2O3–Al2O3–MgO additives. Since Li2O has a low melting point, Li2O addition effectively decreased the formation temperature of liquid secondary phase, enabling SiC ceramics to obtain higher density and lower porosity after low-temperature sintering (T ≤ 1550 °C). Besides, Li2O addition was found to decrease the viscosity of liquid phase and enhance grain growth of SiC through dissolution-reprecipitation process. When sintered at 1550 °C, Li2O addition led to a remarkable increase of density from 3.03 g/cm3 to 3.21 g/cm3 for SiC ceramic. Meanwhile, the SiC ceramic with Li2O addition exhibited a high Vickers hardness of 22.75 ± 0.35 GPa and a good fracture toughness of 3.83 ± 0.27 MPa m1/2. The research results are expected to benefit the low-cost fabrication of SiC ceramics based on pressure-assisted sintering and alleviate the thermal damage of SiC fiber in hot-pressed SiCf/SiC composites.

Effects of diamond as a main carbon source on the fabrication and mechanical properties of reaction-bonded SiC

RBSC with a low residual Si less than 5 vol% was fabricated using SiC–C preform with diamond as a main carbon source by a conventional reaction sintering process at the temperature range between 1500 °C and 1800 °C. The diamond content in the SiC–C preform varied from 10 wt% to 17 wt%. The diamond as the main carbon source used in SiC–C preform effectively minimized the residual Si in RBSC by increasing the reaction of diamond due to the enhanced Si melt infiltration even in SiC–C preform with high carbon content. The Si melt infiltration should be performed above 1600 °C for the complete reaction of diamond particles with size of 0.5 μm because of the relatively low dissolution rate of diamond in Si melt. The flexural strength of RBSC with residual Si content less than 7 vol% exceeded 400 MPa. The flexural strength of RBSC was increased with decreasing residual Si content, but sharply decreased by the residual carbon accompanying pores in RBSC. RBSC with low residual Si content displayed moderate flexural strengths around 200 MPa even above Si melt temperature because of the formation of continuous SiC structure in RBSC by the enhanced grain growth of SiC. Vickers hardness of RBSC was steadily increased from 17.7 GPa to 24.6 GPa with decreasing residual Si.

(Invited) Application of 3D in-Situ X-Ray Visualization to Track the Formation of Dislocation Clusters during PVT Growth of SiC

SiC has become the key player among wide bandgap semiconductors for power electronic applications. Since the first description of the physical vapour transport (PVT) growth process of SiC by Tairov and Tsvetkov (J. Crystal Growth, 43, 209(1978)), there has been steady progress in SiC-based crystal growth, epitaxy and device processing. The success of SiC compared to Si is related to its superior material properties such as extremely high electrical breakdown field and high thermal conductivity compared to the standard silicon counterpart. In addition, SiC device processing utilises much of the standard Si processing equipment. A major reason for the success of SiC in power electronic applications compared to other wide bandgap counterparts such as GaN, Ga2O3 and diamond is related to the availability of large diameter SiC wafer materials (150mm = standard, 200mm = developped). Bulk SiC growth is now a very well developed process with comparatively high yields. The extraordinary physical properties also include obstacles related to the strong chemical bonding and complex phase diagram of the material, which pose challenges to the growth process. Therefore, there are still a number of open questions related to the nucleation, progression and termination of the bulk growth process that require fundamental research in materials science and technology.The aim of this presentation is (i) to give an overview of the state-of-the-art PVT growth process and (ii) to discuss a current research topic dealing with the early stage of the growth process and the defect formation that can occur during the initial nucleation of SiC. We have applied 3D in-situ visualisation of the growth process using X-ray computed tomography to visualise island formation on the large seeding area. These data are related to growth process instabilities such as temperature variations during the seeding process and axial doping level changes from the seed to the newly grown crystal. Both process instabilities induce mechanical stress on the SiC lattice and act as sources for dislocation generation and multiplication. We will show a series of growth processes with varying growth parameters that shed light on the initial growth stage of SiC.As the crystal diameter of SiC increases from 150 mm to 200 mm, the results of this study become increasingly important.

Growth of SiC, AlN, and GaN Films on Silicon Parts of Arbitrary Geometry for Microelectromechanical Applications

Growth of SiC, AlN, and GaN Films on Silicon Parts of Arbitrary Geometry for Microelectromechanical Applications

Evaluation of critical supersaturation ratios during epitaxial growth of hexagonal SiC {0001} under carbon- and hydrogen-rich conditions

Critical supersaturation ratios α crit during epitaxial growth on 6H-SiC (0001) and (000) under carbon- and hydrogen-rich conditions were formerly estimated by assuming disc-shaped critical nuclei whose side surfaces were terminated with silicon and carbon atoms, respectively. Since this assumption contradicts the atomic configurations of possible hexagonal-prism-shaped critical nuclei, we evaluated α crit by using the reported surface free energies for hydrogen-passivated 3C-SiC surfaces. To account for the observed α crit being much larger on 6H-SiC (0001) than on 6H-SiC (000), we considered that silicon atoms on the side surfaces of hexagonal-prism-shaped critical nuclei be terminated not by carbon but by hydrogen atoms.

High-throughput thermodynamic study of SiC high-temperature chemical vapor deposition from TMS-H2

A systematic study on the tetramethylsilane-hydorgen (TMS-H2) system by high-throughput thermodynamic method is conducted with a large experimental condition range (500 ∼ 2700 K, 0 ∼ 75 kPa, and H2:TMS ratio of 0.1 to 10000) towards the deposition of pure single-crystal SiC by high-temperature chemical vapor deposition (HTCVD) method. The temperature, pressure and H2:TMS ratio dependence phase diagrams are calculated to describe the deposition condition of single-phase “gas + SiC” region. Due to the etching effect of hydrogen on graphite, the increasing temperature and pressure could suppress the formation of graphite and favor the growth of SiC in the H2:TMS ratio above 1000, however, excessive H2:TMS ratio could reduce the TMS consumption efficiency. TMS consumption efficiency maps focusing on the gas + SiC region based on the phase diagrams have been carried out to balance the deposition parameters, SiC mole fraction and TMS consumption efficiency. When H2:TMS ratio > 1000, an accepted window for preparing single-phase SiC with a high TMS consumption efficiency (>90%) is provided, and this window could expand furtherly with increasing the ratio. TMS consumption efficiency maps offer the theoretic basis and guidance for improving the quality and cost of industrial production of single-crystal SiC by HTCVD method.

Comparative studies of nanoscale columnar AlxGa1-xN/AlN heterostructures grown by plasma-assisted molecular-beam epitaxy on cSi, porSi/cSi and SiC/porSi/cSi substrates

Problems of the growth of nanoscale columnar AlxGa1-xN/AlN heterostructures on hybrid substrates involving porous silicon and silicon carbide layers by molecular beam epitaxy technique with plasma-activated nitrogen are discussed in this study. The epitaxial growth of nanoscale columnar AlxGa1-xN/AlN heterostructure is shown to be specified by the layer of silicon carbide, which is formed by atomic substitution technique, and a porous silicon sublayer predetermines the oriented growth of SiC. The performed complex of structural-spectroscopic analysis demonstrated that epitaxial growth of the nuclear AlN layer on all types of the substrates in N-enriched conditions resulted in the formation of AlxGa1-xN/AlN heterostructures with Ga-polar surface. At the same time it was found that the layer of ordered AlxGa1-xN alloy was formed only on the hybrid SiC/porSi/cSi substrate. The layer of AlxGa1-xN on the substrates of cSi and porSi/cSi is present in the state of disordered alloy with an excess content of gallium atoms. Nanocolumns of AlxGa1-xN/AlN grown on the hybrid SiC/porSi/cSi substrate have two types of preferential azimuthal orientation that affects not only their structural and optical properties but also the value of elastic deformation in the heterostructure nanoscale layers. For the first time, azimuthal dependence of intensity of E1(TO) and E2high photon modes was detected in the Raman spectra. The observed periodicity angle in micro-Raman scattering coincides with the characteristic swivel of nanoscale columns of AlxGa1-xN/AlN around c-axis according to the data of XRD pole figure measurements. Results obtained in our work show promising capabilities in the use of SiC/porSi/сSi substrates for integration of silicon technology and technology of synthesis of the nanoscale columnar AlxGa1-xN heterostructures by molecular-beam epitaxy with plasma-activated nitrogen.

Microstructure evolution, interface and mechanical properties of SiCp/2A14 joint during laser keyhole welding

Welding problems have restricted the applications of lightweight SiCp/Al composites in aerospace. In this work, the controllability of the keyhole mode, nucleation mechanism, and mechanical properties of the laser-welding process are studied in detail. The extrusion effect formed by the open keyhole pushes SiC particles to the bottom of the molten pool. To observe the nucleation and growth mechanism of the Al4C3 of keyhole laser-welded SiC/2A14Al composites, the dissolution–precipitation behavior of the SiC particles and growth behavior of the Al4C3 tip were observed. Owing to its high chemical properties, Al4C3 mainly begins nucleating from the open edges of the SiC particles and its formation is mainly distributed along the direction of Al grains. Al4C3 was the main crack source and propagation path while the small-sized SiC particles hindered the crack propagation. This work innovatively regulates the keyhole mode to achieve ‘small damage breakdown’ laser welding, greatly reducing the volume fraction of Al4C3. It also provides new insight into fusion welding of SiC particle-reinforced Al matrix composites.

Temperature Dependence of 3С-SiC Growth During Rapid Vacuum Thermal Silicon Treatment

The paper presents the results of a study of the structure, phase composition, and growth kinetics of silicon carbide epitaxial layers on silicon substrates during their rapid vacuum thermal treatment. Transmission electron microscopy revealed the formation of layers of the cubic polytype SiC (3C-SiC) on silicon during carbidization in the temperature range of 1000–1300 °C. It was found that the formation of SiC layers proceeds in two stages, characterized by different activation energies. In the lower temperature range from 1000 to 1150 °C, the activation energy of the SiC growth process is Ea = 0.67 eV, while in the temperature range from 1150 to 1300 °C, the activation energy increases by almost an order of magnitude (Ea = 6.3 eV), which indicates a change in the limiting physical process. It has been established that the type of conductivity and the orientation of the substrate affect the thickness of the formed SiC layers. In this case, the greatest thickness of silicon carbide layers is achieved on silicon substrates with (111) orientation of p-type conductivity.

Kinetic Monte Carlo simulation study of the early stages of epitaxial SiC (0001) growth

A kinetic Monte Carlo (kMC) simulation with a cluster-multiple labeling technique was carried out to study the dynamic behavior of Si-C clusters during the early stage of epitaxial growth. In the model, a crystal lattice was established to fix the physical location of atoms and interatomic bonding. Events, such as adatoms adsorption, diffusion on the planar surface, and attachment to and detachment from clusters of adatoms were considered in the model. The Si and C atoms were treated individually to achieve more elaborate information for dynamic behavior of the clusters in the crystal surface. Moreover, a cluster multiple labeling technique, also known as the Hoshen - Kopelman algorithm was used to identify Si-C clusters. Then the properties of the clusters were calculated and analyzed by the algorithm. The simulation results showed that the number of Si-C clusters gradually decreases with increasing substrate temperature and decreasing deposition rate, and that the average size of Si-C clusters at high temperatures is much larger than that at low temperatures. Furthermore, the Si:C ratio on the growing surface has a significant effect on the surface morphology. At Si-rich conditions, the cluster density is relatively high, and the cluster shape is not homogeneously distributed. While with the increase of C mole fraction, the cluster density gradually decreases and the cluster shape becomes more uniform. Therefore, a higher concentration of C in deposition flux is beneficial to the early stage of nucleation. These findings are consistent with predictions for the case of the epitaxial growth of SiC.

Transient and in situ Growth of Nanostructured SiC on Carbon Fibers toward Highly Durable Catalysis

AbstractCarbon is ubiquitously used as catalyst supports in various clean energy technologies, particularly emerging electrocatalysis, yet it often suffers slow oxidation and corrosion along with performance degradation. The harmonious combination of refractory silicon carbide (SiC, chemically inert) with carbon is alluring but often a great challenge, particularly to achieve desirable nanostructures and strong interfaces. Herein, a shockwave‐type transient heating is designed (> 1750 °C for 1 s per pulse) for controllable growth of conformal SiC coating and massive SiC nanowires on carbon fibers (denoted as CF/SiC‐NW), which serves as a high surface area and durable support for catalysis under harsh environments. The transient heating in SiO vapor triggers in situ transformation of the carbon surface into a seamless SiC protective layer, while the following fast cooling is essential for the growth of numerous self‐assembled SiC nanowires. The CF/SiC‐NW exhibits excellent structural stability in the air at high temperatures, in concentrated acidic/alkaline solutions after electrochemical stressing for 2000 cycles, and in oxygen evolution reaction after 10 h of continuous operation. This strategy enables delicate structure control in refractory carbides and is also general for various carbon/carbide functional materials (e.g., C/TiC, C/WC) for electro‐ or electrified catalysis under harsh conditions.

Nucleation and growth of SiC at the interface between molten Si and graphite

In the present work, the evolution of the SiC layer formed at the interface between liquid silicon and solid carbon is studied using a diffusion couple configuration. Reaction conditions were isothermal, with a temperature of 1450 °C maintained from 2 min to 4 h. The rapid heating and cooling of the Si–C diffusion couple specimens were achieved using a Pulse-Electric Current Sintering system. Crystallographic, compositional, and phase distribution data obtained after different reaction times were used to develop a two-stage model for SiC growth at the interface between molten Si and C. Initially, the formation of SiC at the interface is governed by diffusion of C into the molten Si and dissolution/reprecipitation of formed SiC nuclei. These nuclei further grow into larger SiC grains at the Si–C interface and this initial stage is successfully modeled using the Johnson-Mehl-Avrami-Kolmogorov model. Once a continuous SiC layer forms at the Si–C interface, the growth of SiC is controlled by the diffusion of C through the SiC layer, which can be modeled using a power rate law. However, the nature of this diffusion is difficult to determine with certainty since the rate laws for both grain boundary and bulk diffusion fit experimental data equally well.

Bottom-Up Growth of Monolayer Honeycomb SiC.

The long theorized two-dimensional allotrope of SiC has remained elusive amid the exploration of graphenelike honeycomb structured monolayers. It is anticipated to possess a large direct band gap (2.5eV), ambient stability, and chemical versatility. While sp^{2} bonding between silicon and carbon is energetically favorable, only disordered nanoflakes have been reported to date. Here we demonstrate large-area, bottom-up synthesis of monocrystalline, epitaxial monolayer honeycomb SiC atop ultrathin transition metal carbide films on SiC substrates. We find the 2D phase of SiC to be almost planar and stable at high temperatures, up to 1200 °C in vacuum. Interactions between the 2D-SiC and the transition metal carbide surface result in a Dirac-like feature in the electronic band structure, which in the case of a TaC substrate is strongly spin-split. Our findings represent the first step towards routine and tailored synthesis of 2D-SiC monolayers, and this novel heteroepitaxial system may find diverse applications ranging from photovoltaics to topological superconductivity.

Modeling-Based Design of the Control Pattern for Uniform Macrostep Morphology in Solution Growth of SiC

In the solution growth of the SiC crystal, macrosteps with sufficient height on an off-axis substrate are required to reduce defects and achieve a high-quality grown layer. However, over-developed macrosteps can induce new defects and adversely affect the crystal quality. To better understand and control the behavior of macrosteps corresponding to the control parameters of the growth system, a simulation method that consists of a global two-dimensional computational fluid dynamic (CFD) model, a local three-dimensional CFD model near the growth front, and a kinetics model that describes the movement of macrosteps on the crystal surface is proposed. The simulation method is first applied to investigate the effect of the crystal rotation speed on macrostep morphology. Although the results indicate that a higher crystal rotation speed results in less step bunching, constantly rotating the crystal in one direction is demonstrated to be incapable of yielding a uniform macrostep distribution on the whole surface. Accordingly, a sophisticated control pattern is designed by periodically switching the flow direction underneath the crystal surface, where the proposed simulation method is critical to determine detailed control-parameter values. When the control pattern suggested by the simulation is used, a grown crystal with a uniform macrostep morphology and ideal step height on the whole surface is obtained in the practical experiment.

Growth of 4H-SiC epitaxial layers at temperatures below 1500 °C using trichlorosilane (TCS)

TCS (SiHCl3) is widely used in the rapid growth of SiC. However, in the study of using TCS to grow 4H-SiC, the growth temperature is mainly concentrated in 1550–1650 °C, and the research on lower growth temperature is lacking. In this study, TCS was used as the silicon precursor and epitaxial layers were grown in the temperature range of 1350–1500 °C. The results show that the single crystal type 4H-SiC epitaxial layer with good quality can be obtained at the growth temperature of 1450 ℃.

Characterization of epitaxial layers grown on 4H-SiC (0 0 0 −1) substrates

SiC is an excellent semiconductor material that can be used in power semiconductor devices. It has the advantages of high thermal conductivity, stable chemical properties, and high critical breakdown field strength. The active region of a SiC device is usually in the SiC epitaxial layer, so the growth of high-quality SiC epitaxial layers is extremely valuable. In this paper, we investigate the epitaxial growth of SiC on n-type 4° off-axis SiC (0 0 0–1) substrates. We used a horizontal hot-wall chemical vapor deposition apparatus for rapid epitaxy on SiC substrates, using C2H4, and SiHCl3 as precursors and H2 as carrier gas, respectively, and growing at 1350 °C,1400 °C,1450 °C,1500 °C, 1550 °C, 1600 °C for half an hour to get epitaxial layer. The effect of growth temperature on the surface morphology of SiC (0 0 0 –1) epitaxial layer was analyzed and epitaxial layers is characterized by optical microscope, scanning electron microscope, atomic force microscope and Raman scattering instrument, and the growth rate of epitaxial layer was obtained. It is found that the higher growth temperature is helpful to obtain the epitaxial layer with smooth surface and higher content of 4H-SiC under certain pressure, C/Si molar ratio, and following rate of precursor and carrier gas.