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.     

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.     

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.     

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.     

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.     

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.     

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.     

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.     

A comparison of the colloidal stabilization of aqueous titanium carbide suspensions using anionic and cationic dispersants

The aqueous colloidal stability of titanium carbide (TiC) suspensions has been assessed using both anionic and cationic dispersants. The zeta potential of TiC suspensions, both without and with polyelectrolyte addition, is examined as a function of pH and the relative responses of the polyelectrolytes are compared. Without a dispersant, the TiC powder used shows an isoelectric point at ~ pH 2.6. The use of an anionic polyelectrolyte, an ammonium salt of polymethacrylate (PMA-NH₄) does not significantly alter the isoelectric point. Conversely, the addition of a cationic dispersant, polyethylenimine (PEI) with a molecular weight of either 1800 or 10,000, significantly alters the isoelectric point. The rheological behaviour of the TiC suspensions was examined using a concentric cylinder geometry. In each case a shear thinning response is observed, and a transition to shear thickening is seen on all the PMA-NH₄ trials, and some, but not all, of the PEI experiments at high shear rates (~ 600 s^− 1). The PMA-NH₄ was found to produce optimum slip stability at lower concentrations, (~ 0.02 wt.%) versus the PEI, which obtained the same slip stability at concentrations of ~ 0.30 wt.%. However, increasing the PMA-NH₄ concentration does not provide increased stability; above this point it begins to degrade the slip properties through increasing viscosity. Conversely, the PEI does not exhibit a plateau and subsequent drop off of the slip stability with increasing concentration for the dispersant range studied. For TiC, both polyelectrolytes appear to be suitable dispersants for processing at their respective regions of the pH scale. The PMA-NH₄ provides sufficient stability at ~ pH 8.5, and the PEI provides essentially equal stability in the pH 4.5 region for the concentrations examined.     

Fine grinding of silicon wafers: a mathematical model for the chuck shape

Fine grinding of silicon wafers is a patented technology to manufacture super flat semiconductor wafers cost-effectively. Two papers on fine grinding were previously published in this journal, one discussed its uniqueness and special requirements, and the other presented the results of a designed experimental investigation. As a follow up, this paper presents a study aiming at overcoming one of the technical barriers that have hindered the widespread application of this technology, namely, the difficulty and uncertainty in chuck preparation. Although the chuck shape is critically important in fine grinding, there are no standard procedures for its preparation. Furthermore, the information on the relation between the set-up parameters and the resulting chuck shape is not readily available. In this paper, a mathematical model for the chuck shape is first developed. Then the model is used to predict the relations between the chuck shape and the set-up parameters. Finally, the results of the pilot experiments to verify the model are discussed.     

电冶碳化钨钢结合金在螺纹钢丝轧辊上的应用

介绍了用废弃的粉末冶金碳化钨基钢结合金作原料,采用电冶熔铸工艺制备出新型的电冶碳化钨基钢结合金,并将其用在冷拔轧螺纹钢丝轧辊上。结果表明,电冶钢结合金组织致密、强度高、韧性好,尤其是具有高的抗磨损性能,用其所制的钢丝轧辊成本低、使用寿命高。     

Application of phase diagram calculations to development of new ultra-high temperature structural materials

ln-situ refractory metal intermetallic composites（RMICs） based either on （Nb, Si） or （Mo, Si, B） are candidate materials for ultra-high temperature applications （〉1 400℃）. To provide a balance of mechanical and environmental properties, Nb-Si composites are typically alloyed with Ti and Cr, and Mo-Si-B composites are alloyed with Ti. Phase diagrams of Nb-Cr-Ti-Si and Mo-Si-B-Ti, as prerequisite knowledge for advanced materials design and processing development, are critically needed. The phase diagrams in the metal-rich regions of multicomponent Nb-Cr-Ti-Si and Mo-Si-B-Ti were rapidly established using the Calphad （Calculation of phase diagram） approach coupled with key experiments. The calculated isotherms, isopleths, and solidification paths were ：validated by experimental work. The important heterogeneous multiphase equilibria in both quaternary systems identified will offer engineers the opportunity to develop materials with a balance of properties for high-temperature applications.     

Effect of carbide formers on microstructure and thermal conductivity of diamond-Cu composites for heat sink materials

Diamond-copper composites were prepared by powder metallurgy, in which the diamond particles were pre-coated by magnetic sputtering with copper alloy containing a small amount of carbide forming elements (including B, Cr, Ti, and Si). The influence of the carbide forming element additives on the microstructure and thermal conductivity of diamond composites was investigated. It is found that the composites fabricated with Cu-0.5B coated diamond particles has a relatively higher density and its thermal conductivity approaches 300 W/(m·K). Addition of 0.5%B improves the interfacial bonding and decreases thermal boundary resistance between diamond and Cu, while addition of 1%Cr makes the interfacial layer break away from diamond surface. The actual interfacial thermal conductivity of the composites with Cu-0.5B alloy coated on diamond is much higher than that of the Cu-1Cr layer, which suggests that the intrinsic thermal conductivity of the interfacial layer is an important factor for improving the thermal conductivity of the diamond composites.