Homogeneous nanocrystalline cubic silicon carbide films prepared by inductively coupled plasma chemical vapor deposition

Silicon carbide films with different carbon concentrations x(C) have been synthesized by inductively coupled plasma chemical vapor deposition from a SiH(4)/CH(4)/H(2) gas mixture at a low substrate temperature of 500?°C. The characteristics of the films were studied by x-ray photoelectron spectroscopy, x-ray diffraction, scanning electron microscopy, high-resolution transmission electron microscopy, Fourier transform infrared absorption spectroscopy, and Raman spectroscopy. Our experimental results show that, at x(C) = 49?at.%, the film is made up of homogeneous nanocrystalline cubic silicon carbide without any phase of silicon, graphite, or diamond crystallites/clusters. The average size of SiC crystallites is approximately 6?nm. At a lower value of x(C), polycrystalline silicon and amorphous silicon carbide coexist in the films. At a higher value of x(C), amorphous carbon and silicon carbide coexist in the films.     

Low-dimensional SiC nanostructures: Fabrication, luminescence, and electrical properties

Nanostructured silicon carbide has unique properties that make it useful in microelectronics, optoelectronics, and biomedical engineering. In this paper, the fabrication methods as well as optical and electrical characteristics of silicon carbide nanocrystals, nanowires, nanotubes, and nanosized films are reviewed. Silicon carbide nanocrystals are generally produced using two techniques, electrochemical etching of bulk materials to form porous SiC or embedding SiC crystallites in a matrix such as Si. Luminescence from SiC crystallites prepared by these two methods is generally believed to stem from surface or defect states. Stable colloidal 3C-SiC nanocrystals which exhibit intense visible photoluminescence arising from the quantum confinement effects have recently be produced. The field electron emission and photoluminescence characteristics of silicon carbide nanostructures as well as theoretical studies of the structural and electronic properties of the materials are described.     

金刚石/碳化硅复合梯度膜制备研究

采用微波等离子化学气相沉积(MW-PCVD)制备金刚石/碳化硅复合梯度膜.工作气体为H₂,CH₄和Si[CH₃]₄(四甲基硅烷,TMS),其中H₂∶CH₄=100∶0.6,Si[CH₃]₄为0％-O.05％,沉积压力为3300Pa,基体温度为700℃,微波功率为700W.基体为单晶硅,在沉积前用纳米金刚石颗粒处理.沉积后的样品经扫描电子显微镜(SEM),电子探针显微分析(EPMA),X射线能量损失分析(EDX)表明:沉积膜中的碳化硅含量是随Si[CH₃]₄流量的变化而改变.通过改变Si[CH₃]₄的流量可以制备金刚石/碳化硅复合梯度膜,且梯度膜中金刚石与复合膜过渡自然平滑.     

Mechanical behavior of SiCf/SiC composites with alternating PyC/SiC multilayer interphases

In order to tailor the fiber–matrix interface of continuous silicon carbide fiber reinforced silicon carbide (SiC_f/SiC) composites for improved fracture toughness, alternating pyrolytic carbon/silicon carbide (PyC/SiC) multilayer coatings were applied to the KD-I SiC fibers using chemical vapor deposition (CVD) method. Three dimensional (3D) KD-I SiC_f/SiC composites reinforced by these coated fibers were fabricated using a precursor infiltration and pyrolysis (PIP) process. The interfacial characteristics were determined by the fiber push-out test and microstructural examination using scanning electron microscopy (SEM). The effect of interface coatings on composite mechanical properties was evaluated by single-edge notched beam (SENB) test and three-point bending test. The results indicate that the PyC/SiC multilayer coatings led to an optimum interfacial bonding between fibers and matrix and greatly improved the fracture toughness of the composites.     

A facile synthesis of silicon carbide nanoparticles with high specific surface area by using corn cob

Corn cob, which possesses low ash and high carbon contents, is a common waste material that accounts for a large amount of agricultural waste. This paper reports about a facile method to synthesize silicon carbide (SiC) nanoparticles with high specific surface area by using corn cob as a carbon source. The method is accomplished by carbothermal reduction at 1350?°C using corn cob as carbon source and silicon monoxide as silicon source. Fourier transform infrared (FT-IR) and Raman spectra results confirmed the formation of synthesized SiC particles. X-ray diffraction (XRD) results indicated the major phases of 3C-SiC. Scanning electron microscopy (SEM) and transmission electron microscopy (TEM) images showed that the SiC particle size is in the range of 40–100?nm and mainly composed of sphere-shaped nanoparticles. The Brunauer–Emmett–Teller (BET) specific surface area of samples is 80.25?m²/g. In addition, we proposed the formation mechanism of SiC nanoparticles with high specific surface area by adsorption and vapor–solid mechanism. This facile method for synthesizing SiC nanoparticles provides a new idea for high-value application of corn cobs and new raw material for the preparation of silicon carbide.     

Preparation of silicon carbide using bamboo charcoal as carbon source

Silicon carbide (SiC) was prepared by carbothermal reduction with amorphous silica sol as silicon source and bamboo charcoal powder as carbon source. The compositions and microstructure of prepared SiC were investigated by using X-ray diffraction (XRD), scanning electron microscopy (SEM) and Energy Dispersive X-ray Spectroscopy (EDS). XRD of prepared SiC showed that the major phase of prepared SiC was hexagonal 6H-SiC with the existence of some 4H-SiC. SEM showed that SiC particle was granular, rod-like and of tower-shape, and it inherited the shape of bamboo charcoal. EDS showed that prepared SiC was pure without being doped by the mineral elements from bamboo charcoal.     

Preparation and microwave absorbing properties of SiC microtubes

Using cotton as carbon source and template, SiC microtubes were prepared by the carbothermal reduction of a cotton-contained precursor, which was obtained by impregnating cotton in tetraethyl orthosilicate solution. To characterize the product, X-ray diffraction, scanning electron microscopy, transmission electron microscopy, and network analyzer were used. The results show that the SiC microtubes with surfaces composed of villus-like β-SiC nanowires have a length of tens to hundreds of micrometers and a diameter of several to 20 μm. SiC microtubes achieve a reflection loss below −10 dB (90% absorption) at different frequencies, and the minimum value is −23.9 dB at 17.5 GHz when its thickness is 1 mm.     

Interlaminar shear strength of SiC matrix composites reinforced by continuous fibers at 900 °C in air

To reveal the shear properties of SiC matrix composites, interlaminar shear strength (ILSS) of three kinds of silicon carbide matrix composites was investigated by compression of the double notched shear specimen (DNS) at 900 °C in air. The investigated composites included a woven plain carbon fiber reinforced silicon carbide composite (2D-C/SiC), a two-and-a-half-dimensional carbon fiber-reinforced silicon carbide composite (2.5D-C/SiC) and a woven plain silicon carbon fiber reinforced silicon carbide composite (2D-SiC/SiC). A scanning electron microscope was employed to observe the microstructure and fracture morphologies. It can be found that the fiber type and reinforcement architecture have significant impacts on the ILSS of the SiC matrix composites. Great anisotropy of ILSS can be found for 2.5D-C/SiC because of the different fracture resistance of the warp fibers. Larger ILSS can be obtained when the specimens was loaded along the weft direction. In addition, the SiC fibers could enhance the ILSS, compared with carbon fibers. The improvement is attributed to the higher oxidation resistance of SiC fibers and the similar thermal expansion coefficients between the matrix and the fibers.     

Synthesis of β-SiC nanostructures via the carbothermal reduction of resorcinol–formaldehyde/SiO2 hybrid aerogels

The novel resorcinol–formaldehyde/SiO₂ (RF/SiO₂) hybrid aerogels were chosen to synthesize the cubic silicon carbide (β-SiC) nanostructures via a carbothermal reduction route. In this process, the in situ polymerized RF/SiO₂ aerogels were used as both the silicon and carbon sources. The morphologies and structures of SiC nanostructures were characterized by X-ray diffraction (XRD), scanning electron microscope (SEM), and high-resolution transmission electron microscope (HRTEM) equipped with EDS. The effects of C/Si atomic ratios in RF/SiO₂ aerogels and heat treatment temperatures on the formation of SiC nanomaterials were investigated in detail. It was shown that β-SiC nanowhiskers with diameters of 50–150 nm and high crystallinity were obtained at the temperatures from 1400 to 1500 °C. The role of the interpenetrating network of RF/SiO₂ hybrid aerogels in the carbothermal reduction was discussed and a possible mechanism was proposed.     

Effects Associated with Nanostructure Fabrication Using In Situ Liquid Cell TEM Technology

Nano-Micro Letters - We studied silicon, carbon, and SiC x nanostructures fabricated using liquid-phase electron-beam-induced deposition technology in transmission electron microscopy systems....     

Fabrication and characterization of some novel reaction-bonded silicon carbide materials

Attempts have been made to produce modified reaction-bonded silicon carbide (RBSC) ceramics by incorporating a dispersion of other phases into the initial powder mix. ZrC, TiC, TaC and B₄C were chosen as additives together with TiB₂ as a phase likely to produce microcrack toughening in the final compact. During fabrication an important factor appears to be the possible reactions of the added phase with liquid silicon during the infiltration stage of the process. Thus, while all the carbides react with liquid silicon to form refractory silicides and new silicon carbide, this only significantly affected the reaction-bonding process if the dissolution/reaction kinetics were so fast as to disrupt the formation of the new silicon carbide framework which grows epitaxially to bond the existing silicon carbide particles together. As with conventional RBSC, the initial SiC grits play no part in any reaction except to act as nucleation sites for the new SiC. The microstructures of the various new materials have been characterized by reflected light microscopy, scanning electron microscopy, energy dispersive X-ray analysis and X-ray diffraction. This has led to an appraisal of the high-temperature reactions observed to have occurred and the unreliability of the high-temperature thermochemical data used to predict their occurrence. The mechanical properties of the new materials have been investigated by indentation testing (hardness and fracture toughness), including temperature-variant tests. Results are presented and the possibility for improving the properties of RBSC are discussed.     

Heteropolytype structures with SiC quantum dots

Epitaxial silicon carbide layers of 3C-SiC polytype with an array of nanodimensional SiC quantum dots (QDs) have been obtained for the first time using an improved method of sublimation epitaxy in vacuum. The X-ray topography and X-ray diffraction data unambiguously confirm the formation of a 3C-SiC epilayer with twinned regions on the surface of a 6H-SiC substrate. The surface topography of epilayers was studied by atomic force microscopy (AFM), and the microstructure of a near-surface layer of the deposit was investigated by transmission electron microscopy (TEM). Using the AFM and TEM data, the presence of QDs (representing SiC nanoislands) is established, and their average dimensions and concentration are evaluated.     

Formation of SiC nanowhiskers by carbothermic reduction of silica with activated carbon

The silicon carbide (SiC) nanowhiskers were obtained by a carbothermic reduction of silica (SiO₂) with activated carbon at 1450 °C. The products were characterized by X-ray diffraction (XRD), Fourier transformed infrared spectroscopy (FT-IR), field emission scanning electron microscopy (FE-SEM) and high resolution transmission electron microscopy (HR-TEM). The SiC nanowhiskers were grown as crystalline β-SiC with the diameter ranging from 20 to 150 nm grew along (111) direction with the length up to several tens of micrometers. Yield of β-SiC is very high with the moderate amount of un-reacted SiO₂. This is the first report on the synthesis of high yield of β-SiC by simple direct heating method.     

Novel silicon carbide/polypyrrole composites; preparation and physicochemical properties

Novel silicon carbide/polypyrrole (SiC/PPy) conducting composites were prepared using silicon carbide as inorganic substrate. The surface modification of SiC was performed in aqueous solution by oxidative polymerization of pyrrole using ferric chloride as oxidant. Elemental analysis was used to determine the mass loading of polypyrrole in the SiC/PPy composites. Scanning electron microscopy showed the surface modification of SiC by PPy. PPy in composites was confirmed by the presence of PPy bands in the infrared spectra of SiC/PPy containing various amounts of conducting polymer. The conductivity of SiC/PPy composites depends on PPy content on the surface. The composite containing 35 wt.% PPy showed conductivity about 2 S cm⁻¹, which is in the same range as the conductivity of pure polypyrrole powder prepared under the same conditions using the same oxidant. PPy in the composites was clearly detected by X-ray photoelectron spectroscopy (XPS) measurements by its N1s and Cl2p peaks. High resolution scans of the C1s regions distinguished between silicon carbide and polypyrrole carbons. The fraction of polypyrrole at the composite surface was estimated from the silicon and nitrogen levels. The combination of XPS and conductivity measurements suggests that the surface of the SiC/PPy composites is polypyrrole-rich for a conducting polymer mass loading of at least 12.6 wt.%.     

Structure of a silicon carbide film synthesized by r.f. reactive ion plating

Silicon carbide films were easily synthesized on silicon (111) surfaces and tantalum plates by r.f. reactive ion plating. Silicon was evaporated from an evaporation source using an electron beam gun in an acetylene discharge atmosphere at a pressure of the order of 10^-4 Torr. Film structures were studied using reflection high energy electron diffraction and scanning electron microscopy. Cubic silicon carbide (β-SiC) single crystals were observed on the silicon (111) surfaces at 1000°C. The synthesis mechanism of SiC film formation in the r.f. reactive ion-plating system appears to be different from that in an ordinary reactive evaporation system. The r.f. plasma excitation in reactive ion plating is considered to be effective in the synthesis process.     

快速烧成连续碳化硅纤维的表面分析

以聚碳硅烷（PCS）为先驱体；经熔融纺丝、不熔化处理和快速烧成工艺制备出性能较好的连续碳化硅（SiC)纤维。采用XPS、SEM、TG等方法对所得SiC纤维的表面结构组成和热稳定性进行了分析，并探讨了快速烧成方式下引起纤维抗拉强度降低的主要原因。结果表明：快速烧成的SiC纤维表层有富含游离碳的热解沉积物，对纤维的热稳定性产生不利影响，采用超声清洗可以将其快速除去；表层缺陷是引起SiC纤维抗拉强度下降的主要原因。     

Carbon monoxide-silicon carbide interaction in HTGR fuel particles

The corrosion of the coating-layers of silicon carbide (SiC) by carbon monoxide (CO) was observed in irradiated Triso-coated uranium dioxide particles, used in high-temperature gas-cooled reactors, by optical microscopy and electron probe micro-analysis. The mechanical failure of the coating-layer of inner dense pyrolytic carbon (IPyC) was often observed beside the area of the SiC corrosion. The grain boundaries of the SiC seemed to be selectively corroded during early stages of corrosion. Silicon dioxide, or more stable (Si, Ce, Ba) oxide, was accumulated at the buffer-IPyC and IPyC-SiC interfaces on the cold side of the particles and the formation of (Pd, Rh, Ru, Tc, Mo) silicides was observed in the fuel kernels, which probably resulted from the vapour transport of silicon monoxide from the corroded areas.     

A microstructural study of silicon carbide fibres through the use of Raman microscopy

The microstructures of three different silicon carbide (SiC) fibres produced by CVD (chemical vapour deposition) have been examined in detail using Raman microscopy. Raman spectra were mapped out across the entire cross-sections of these silicon carbide fibres using an automated x-y stage with a spatial resolution of 1 m. The Raman maps clearly illustrate the variations in microstructure in such types of silicon carbide fibres. It appears that the SCS-type fibres contain carbon as well as SiC whereas the Sigma 1140+ fibre also contains free silicon. Furthermore, the differences in the detailed structures of the carbon and silicon carbide present in the fibres can also be investigated. Raman microscopy is demonstrated to be a very sensitive technique for characterising the composition and microstructure of CVD silicon carbide fibres prepared using different processing conditions.     

Optimizing the low-pressure carburizing process of 16Cr3NiWMoVNbE gear steel

Compared with the traditional atmospheric carburization, low-pressure carburization has the benefits of producing no surface oxidation and leaving fine, uniformly dispersed carbides in the carburized layer. However, the process parameters for low-pressure carburization of 16Cr3NiWMoVNbE steel have yet to be optimized. Thus, we use the saturation-value method to optimize these parameters for aviation-gear materials. Toward this end, the microstructure and properties of 16Cr3NiWMoVNbE steel after different carburization processes are studied by optical microscopy, scanning electron microscopy, transmission electron microscopy, and electron probe microanalysis. Considering the saturated austenite carbon concentration, we propose a model of carbon flux and an alloy coefficient for low-pressure carburization to reduce the carbon concentration in austenite and avoid the surface carbide network. At the early stage of carburization (˜30 s), the gas-solid interface has a higher concentration gradient. The averaging method is not ideal in practical applications, but the carbon flux measured by using the segmented average method is 2.5 times that measured by the overall average method, which is ideal in practical applications. The corresponding carburization time is reduced by 60%. By using the integral average method, the actual carburization time increases, which leads to the rapid formation of carbide on the surface and affects the entire carburization process. Nb and W combine with C to form carbides, which hinders carbon diffusion and consumes carbon, resulting in a sharp decrease in the rate of C diffusion in austenite (the diffusion rate is reduced by ˜52% for 16Cr3NiWMoVNbE steel). By changing the diffusion coefficient model and comparing the hardness gradient of different processes, the depth of the actual layer is found to be very similar to the design depth.     

平纹编织SiCf/SiC复合材料的中温蠕变断裂时间及损伤机制

碳化硅纤维增强碳化硅复合材料(SiC_f/SiC)是制造下一代航空发动机热结构件的关键材料,中等温度(～800℃)下,SiC_f/SiC的蠕变断裂时间t_u显著下降。为此,研究了平纹编织SiC_f/SiC (2D-SiC_f/SiC)在空气中500～1 000℃的蠕变性能及损伤机制,应力水平为100～160 MPa。利用SEM、TEM和EDS分析了断口形貌、微观组织和化学成分。结果表明：2D-SiC_f/SiC的t_u与温度和应力水平有关。相同温度下,2D-SiC_f/SiC的t_u随着应力增加而变短。当温度为800℃、蠕变应力大于基体开裂应力(PLS)时,2D-SiC_f/SiC发生中温脆化现象,其t_u下降。2D-SiC_f/SiC的中温脆化机制为基体开裂、BN界面氧化和SiO₂替代BN界面导致的强界面/基体结合。2D-Si...