Processing and mechanical properties of porous silica-bonded silicon carbide ceramics

A simple processing route for manufacturing highly porous, silica-bonded SiC ceramics with spherical pores has been developed. The strategy adopted for making porous silica-bonded SiC ceramics entails the following steps: (i) fabricating a formed body through a combination of SiC and polymer microbeads (employed as sacrificial templates) and (ii) sintering the formed body in air. SiC particles are bonded to each other by oxidation-derived SiO₂ glass. By controlling the microbead content and the sintering temperature, it was possible to adjust the porosity such that it ranged from 19 to 77%. The flexural and compressive strengths of the porous silica-bonded SiC ceramics with ≈40% porosity were ≈65 MPa and ≈200 MPa, respectively. The superior strengths were attributed to the homogeneous distribution of small (≤30 μm), spherical pores with dense struts in the porous silica-bonded SiC ceramics.     

Damage-free machining of monocrystalline silicon carbide

Cutting tests of monocrystalline SiC, on the surface of which an amorphous layer was preformed by ion implantation, were performed. Ductile-mode machining was observed at a depth of cut smaller than 60 nm. At a depth of cut larger than 60 nm, cracks were observed on the work surface. However, transmission electron micrographs show that crack propagation was obstructed at the interface between the amorphous and crystalline layers even under brittle-mode machining, and no subsurface damage extended into the crystalline layer. The results suggest that the damage-free machining of monocrystalline SiC is possible by surface modification to an amorphous structure.     

Shape adaptive grinding of CVD silicon carbide

Because of the direct relationship between removal rate and surface roughness in conventional grinding, ultra-precision finishing of hard coatings produced by chemical vapour deposition (CVD) usually involves several process steps with fixed and loose abrasives. In this paper, an innovative shape adaptive grinding (SAG) tool is introduced that allows finishing of CVD silicon carbide with roughness below 0.4 nm Ra and high removal rates up-to 100 mm³/min. The SAG tool elastically complies with freeform surfaces, while rigidity at small scales allows grinding to occur. Since material removal is time dependent, this process can improve form error iteratively through feed moderation.     

Magnetic properties of vanadium-doped silicon carbide nanowires

This study reports the magnetic properties of vanadium (V) doped single crystalline silicon carbide nanowires. The first principle calculation indicated that the V-doped cubic SiC phase can exhibit half-metallic ferromagnetic properties that are essential for the realization of spintronic devices. Based on this calculation, V-doped SiC nanowires were fabricated in a chemical vapor deposition process. The single crystalline β-SiC nanowires, which are doped with ca. 4 at.% of V, had diameters of < 100 nm and a length of several μm. High-resolution transmission electron microscopy observations revealed vanadium carbide (VC) phases in the nanowires, even at this low concentration of dopants. Magnetic characterization implies that the nanowires are a mixture of the diamagnetic phase of VC and ferro- or paramagnetic phases of V-doped SiC. These results suggest that the doping of transition metal having high solubility to the SiC phase can lead to the realization of dilute magnetic semiconductor behavior at very low temperature.     

Influence of silicon carbide chills on solidification process and shrinkage porosity of castings made of nickel based superalloys

The paper presents the manufacturing methodology of IN713C castings by application of investment casting method and silicon carbide (SiC) chills.

On the basis of numerical simulation and conducted microstructure analysis, it was established that the application of SiC chills results in significant decrease in shrinkage porosity, in comparison to castings without chills. The temperature measurement was carried out, and the influence of chills on the kinetics of solidification process was established. It was determined that the application of SiC chills causes the increase in cooling rate (～0·1 K s^?1), in comparison to the casting without chills. The authors carried out numerical optimisation with the use of ProCAST software and established which parameters have the largest influence on the solidification process of castings with and without chills. In addition to SiC, the graphite and Al₂O₃ were analysed as chill material in terms of influence on the predicted kinetics of cooling process and the shrinkage porosity of castings. The conditions of solidification process for castings, which are equipped with chills and are free from shrinkage porosity, were determined on the basis of obtained results.     

Evidence of a highly compressed nanolayer at the epitaxial silicon carbide interface with silicon

Through a novel methodology for evaluating layer-by-layer residual stresses in epitaxial silicon carbide films with resolution down to 10 nm, we indicate the existence of a highly compressed interfacial nanolayer between the films and their silicon substrates. This layer is consistently present underneath all types of silicon carbide films examined herein, regardless of the extent of residual tensile stress measured in the full thickness of the films, which varies from 300 up to 1300 MPa. We link this nanolayer to the carbonization step of the film growth process and we discuss in detail the implications in terms of fracture behaviour by bulge testing of micromachined membranes.     

High temperature oxidation of silicon carbide based materials

The process of high temperature oxidation of two silicon carbide based materials differing by methods of their production and properties has been studied up to 1500°C in air. The oxidation was performed under the isothermal conditions and at the programmed heat rate of 10° per minute. It was found that the oxidation resistance of the material was the function of the presence of extrinsic metals having close affinity for oxygen. It was also found that under heating up to 1500°C in air phase transitions occurred in the SiC surface layer.     

Effects of light-mass structural forms on silicon carbide mirror

To reduce the mass of the mirror, silicon carbide was used as the material and four light-mass structures were designed. The properties of SiC mirror open back structure with triangular cell, open back structure with hexagonal cell, sandwich structure with triangular cell, sandwich structure with hexagonal cell, were analyzed by using finite element method. The results of the static, dynamic, and thermal properties of the four kinds of SiC mirror indicate that the surface figures of the SiC mirrors are all satisfactory with the design requirements. The properties of the mirrors with sandwich structure are better than those with open back structure, except the high cost. And the mirror with triangular cell has better combination properties than the mirror with hexagonal cell. Considering the overall performance and the cost, open back structure with triangular cell is the most suitable for the SiC mirror.     

Room temperature process for chemical vapor deposition of amorphous silicon carbide thin film using monomethylsilane gas

The silicon carbide thin film formation process, which was completely performed at room temperature, was developed by employing a reactive silicon surface preparation using argon plasma and a chemical vapor deposition using monomethylsilane gas. Time-of-flight secondary ion mass spectrometry showed that silicon-carbon bonds existed in the obtained film, the surface of which could remain specular after exposure to hydrogen chloride gas at 800 °C. The silicon dangling bonds formed at the silicon surface by the argon plasma are considered to easily accept the monomethylsilane molecules at room temperature to produce the amorphous silicon carbide film thicker than monolayer. Thus, the entire silicon carbide thin film formation process at room temperature is possible.     

Slurry based multilayer environmental barrier coatings for silicon carbide and silicon nitride ceramics — I. Processing

Multilayer mullite/gadolinium silicate (Gd₂SiO₅) environmental barrier coatings (EBCs) were deposited on α-SiC (Hexaloy) and Si₃N₄ (SN282) substrates through cost-effective slurry based dip-coat processing. Coatings applied by two approaches, alcohol and sol-based slurries, were examined and optimized in terms of their recipes and air sintering temperatures. A significant increase in densification rates was found for the sol-based EBCs applied on both SiC and SN282 substrates due to the fine mullite particles formed during reaction sintering of well-mixed silica and alumina sols. Mechanical alloying of the starting powder mixtures instead of their simple rotary-blending was found to be beneficial in terms of enhanced coat sintering kinetics. Dense thick coatings that were well-bonded to the substrate were obtained.     

Slurry based multilayer environmental barrier coatings for silicon carbide and silicon nitride ceramics — II. Oxidation resistance

In part I of this study, the dip-coat processing of mullite/gadolinium silicate (Gd₂SiO₅) environmental barrier coatings (EBCs) applied on α-SiC and SN282™ Si₃N₄ through alcohol based and sol based slurries was presented. Here, the performance of selected EBCs by evaluating their oxidation resistances during thermal cycling in simulated combustion (90% H₂O-balance O₂) environment between 1350 °C and RT for up to 400 cycles is being reported. Oxidation of un-coated α-SiC was severe, leading to aligned and layered porous silica scale formation (~ 17 μm thick) on its surface with frequent scale spallation when exposed to 100 cycles. Mullite/Gd₂SiO₅/B₂O₃ (83.5/11.5/5 wt.%) EBCs remained adherent to α-SiC substrate with an underlying porous silica layer formed at substrate/coating interface, which was ~ 12 μm after 100 cycles, ~ 16 μm after 200 cycles, and ~ 25 μm after 400 cycles. In contrast, α-SiC substrate coated with mullite/Gd₂SiO₅ (88/12 wt.%) EBC had only limited oxidation of ~ 10 μm even after 1350 °C/400 cycles. The sol based mullite/Gd₂SiO₅ (88/12 wt.%) EBC on α-SiC substrate after 400 cycles was adherent, but showed more interfacial damages (~ 20 μm after 400 cycles) though it had increased coating density. However, the mullite/Gd₂SiO₅ (88/12 wt.%) EBC (alcohol based) delaminated from the SN282™ Si₃N₄ substrate after 1350 °C/100 cycles, because of the formation of interconnected interfacial voids and hairline cracks. Parabolic growth kinetics for the underlying silica was observed for both the alcohol and sol based coated samples.     

Machining performance of silicon carbide ceramic in end electric discharge milling

A new process of machining silicon carbide (SiC) ceramic using end electrical discharge milling is proposed in this paper. The process is able to effectively machine a large surface area on SiC ceramic with good surface quality and low cost. The effects of machining conditions on the material removal rate, electrode wear ratio, and surface roughness have been investigated. The surface microstructures machined by the new process are examined with a scanning electron microscope (SEM), an energy dispersive spectrometer (EDS), and an X-ray diffraction (XRD). The results show that the SiC ceramic is removed by melting, evaporation and thermal spalling, the material from the tool electrode can transfer to the workpiece, and a combination reaction takes place during end electric discharge milling of the SiC ceramic.     

Plasma functionalization of silicon carbide crystalline nanoparticles in a novel low pressure powder reactor

In order to functionalize silicon carbide nanopowders with carboxylic groups, an r.f. (13.56 MHz) low pressure plasma reactor has been developed so that particles can be stirred during the processing to try to coat them on their whole surface. Coatings in an O₂/hexamethyldisilazane (HMDSN) mixture have first been optimized on flat substrates; X-ray Photoelectron Spectroscopy (XPS) analysis showed that the O₂/HMDSN gas mixture resulted in a coating evolving from a polymer-like structure to a more inorganic SiO_x-like structure as the oxygen ratio increased. For a large O₂/HMDSN value, carboxylic groups were detected on the sample surface. Silicon carbide nanoparticles have then been plasma processed in such a reactive atmosphere. XPS, Time of Flight Secondary Ion Mass Spectroscopy (ToF-SIMS) and Transmission Electron Microscopy (TEM) analyses evidenced the surface modification of the processed powder and confirmed the grafting of carboxylic groups.     

High-energy heavy ion beam annealing effect on ion beam synthesis of silicon carbide

Silicon carbide (SiC) is a superior material potentially replacing conventional silicon for high-power and high-frequency microelectronic applications. Ion beam synthesis (IBS) is a novel technique to produce large-area, high-quality and ready-to-use SiC crystals. The technique uses high-fluence carbon ion implantation in silicon wafers at elevated temperatures, followed by high-energy heavy ion beam annealing. This work focuses on studying effects from the ion beam annealing on crystallization of SiC from implanted carbon and matrix silicon. In the ion beam annealing experiments, heavy ion beams of iodine and xenon, the neighbors in the periodic table, with different energies to different fluences, I ions at 10, 20, and 30 MeV with 1-5 × 10¹² ions/cm², while Xe ions at 4 MeV with 5 × 10¹³ and 1 × 10¹⁴ ions/cm², bombarded C-ion in implanted Si at elevated temperatures. X-ray diffraction, Raman scattering, infrared spectroscopy were used to characterize the formation of SiC. Non-Rutherford backscattering and Rutherford backscattering spectrometry were used to analyze changes in the carbon depth profiles. The results from this study were compared with those previously reported in similar studies. The comparison showed that ion beam annealing could indeed induce crystallization of SiC, mainly depending on the single ion energy but not on the deposited areal density of the ion beam energy (the product of the ion energy and the fluence). The results demonstrate from an aspect that the electronic stopping plays the key role in the annealing.     

Fabrication and test of reaction bond silicon carbide for optical applications

1 Introduction Silicon carbide may be the best material available for mirror optics because of its outstanding combination of thermal and mechanical properties[1?3]. This material has remarkable dimensional stability even under the disturbances of tempera…     

Medium-range order in amorphous silicon investigated by constrained structural relaxation of two-body and four-body electron diffraction data

The structures of four types of amorphous silicon are examined by an experimentally constrained structural relaxation method (ECSR). Experimental selected area electron diffraction data and fluctuation electron microscopy normalized diffraction variance data were used as constraints to guide a Monte Carlo relaxation procedure towards best fit models. A Tersoff potential was also used to further restrict the space of possible solutions. The materials examined were self-ion-implanted silicon and pressure-amorphized silicon, both in their as-prepared and thermally annealed states. In the fitted models for these materials regions containing two types of medium-range order were identified. One type involves formation of paracrystallites with cubic and hexagonal structures, where both short-range crystalline and medium-range order are present. The other type of medium-range order appears in the form of extended crystalline planes without associated short-range crystalline order. These two types can coexist. It is observed that the best fit models for both as-prepared samples contain approximately 10-15% paracrystalline ordered regions, reducing to about 5-10% in the annealed materials. None of the models are true continuous random networks. We conclude that, with long computational times and with a suitable potential function, the ECSR procedure provides a powerful, although at present semi-quantitative, tool for determining the structural form of medium-range order in thin amorphous materials.     

SiC颗粒表面Mo涂层的制备与分析

采用磁控溅射法在碳化硅(SiC)颗粒表面成功制备了金属钼(Mo)涂层,分析了Mo涂层的成分和形貌;为改善初始涂层成分和形貌,对镀Mo改性SiC复合粉体进行了不同工艺的结晶化热处理,重点研究了热处理对SiC颗粒表面Mo涂层形貌和成分的影响。结果表明,磁控溅射法能够在SiC颗粒表面沉积Mo涂层,随磁控溅射时间的延长,SiC颗粒表面Mo涂层的粗糙度增大,但磁控溅射后SiC颗粒表面Mo涂层为非晶态。热处理能够有效改善SiC颗粒表面Mo涂层的成分、形貌及结晶状态,在600~1200℃之间结晶化热处理过程中,随热处理温度升高,SiC颗粒表面Mo涂层形貌主要经历了以下4个阶段变化:Mo涂层初步致密化—Mo的结晶致密化—Mo涂层的聚集长大—Mo与SiC之间化学反应;相应的Mo原子的存在状态也经历了如下变化:非晶态Mo原子—晶态Mo原子—Mo_2C和MoSi_2。其中800~900℃之间为最佳热处理温度,此时Mo涂层致密均匀包覆完整。SiC表面连续均匀致密的Mo涂层,有利于改善SiC颗粒增强金属基复合材料中基体与增强体之间的界面结合并控制不利界面反应,有利于复合材料综合性能的提高,必将扩大SiC颗粒作为增强体的应用范围。