Microstructures and improved wear resistance of 3D needled C/SiC composites with graphite filler

Three-dimensional (3D) needled carbon/carbon (C/C) composites with a lowest porosity of 15.6% were achieved after 1 cycle of impregnation by phenolic resin slurry containing graphite filler, hot-pressing curing and pyrolysis. Carbon/silicon carbide (C/SiC) composites were obtained by liquid silicon infiltrating C/C composites. The aim was to incorporate cost effectiveness and excellent performance of C/SiC braking material. Using filler content not exceeding 30 wt% in the slurry promised undamaged C/C segments in C/SiC composites. The linear wear rate of C/SiC using 30 wt% filler was 0.33 μm side⁻¹ cycle⁻¹ and displayed a fourfold decrease; its weight wear rate was 2.46 mg side⁻¹ cycle⁻¹ and minus 171%, compared with the previously reported values of C/SiC without filler, at a braking velocity of 28 m/s. Its friction coefficients and friction stability coefficients appeared relative insensitive to changes in braking velocities and displayed higher values at high braking velocities compared with the previous values.     

Porous carbon nanofibers with narrow pore size distribution from electrospun phenolic resins

Phenolic resin-based porous carbon nanofibers (PCNFs) with large surface area and narrow pore size distribution have been successfully prepared using novolac-type phenolic resin as precursor. The high molecular weight precursor was first synthesized in this study, then was dissolved in methanol. The PCNFs were finally obtained through electrospinning the phenolic resin polymer solution followed by successive curing and carbonization without activation. The N₂ adsorption/desorption isotherms reveal that the PCNFs have high specific surface area about 812 m²/g, the pore size falls in the range of 0.4-0.7 nm and the pore volume is 0.91 cm³/g. The vapor adsorption testing demonstrated that PCNFs exhibited different adsorption performance for ethanol and water.     

Fabrication and characterization of novel hydroxyapatite/porous carbon composite scaffolds

Novel hydroxyapatite (HA)/porous carbon composite scaffolds were prepared by applying sonoelectrodeposition and a subsequent hydrothermal treatment to previous carbonized phenolic resin coated polyurethane sponges. The interconnected pore network and morphology of HA/porous carbon composite scaffolds were determined by scanning electron microscope (SEM), and the whole surface of porous carbons were evenly coated with the deposited HA layer which was confirmed by EDS and XRD. The porosity (83.5 ± 0.3%) and the bulk density (0.297 ± 0.009 g·cm⁻³) of HA/porous carbon scaffolds were detected by the Archimedes method. The compressive and flexural strength of the scaffolds is 1.187 ± 0.064 MPa and 0.607 ± 0.268 MPa, respectively. Compared with the polymeric surface of 24-well cell culture plates, these novel scaffolds significantly promote the proliferation of human osteoblast-like MG-63 cells, indicating that this novel HA/porous carbon composite scaffold could be used for in vitro 3D culture of osteoblasts.     

Fabrication of SiCf/SiC composites by chemical vapor infiltration and vapor silicon infiltration

Three-dimensional (3D) silicon carbide fiber reinforced silicon carbide matrix (SiC_f/SiC) composites, employing KD-1 SiC fibers (from National University of Defense Technology, China) as reinforcements, were fabricated by a combining chemical vapor infiltration (CVI) and vapor silicon infiltration (VSI) process. The microstructure and properties of the as prepared SiC_f/SiC composites were studied. The results show that the density and open porosity of the as prepared SiC_f/SiC composites are 2.1 g/cm³ and 7.7%, respectively. The SiC fibers are not severely damaged during the VSI process. And the SiC fibers adhere to the matrix with a weak interface, therefore the SiC_f/SiC composites exhibit non-catastrophic failure behavior with the flexural strength of 270 MPa, fracture toughness of 11.4 MPa·m^1/2 and shear strength of 25.7 MPa at ambient conditions. Moreover, the flexural strength decreases sharply at the temperature higher than 1200 °C. In addition, the thermal conductivity is 10.6 W/mk at room temperature.     

Preparation and R-curve properties of laminated Si/SiC ceramics from paper

Laminated Si/SiC ceramics were synthesized from paper via impregnation with phenolic resin, followed by lamination and carbonization of the paper–resin laminates and subsequent infiltration and reaction with liquid silicon at a temperature of 1550 °C for 10–90 min. Due to the capillarity infiltration and in situ reaction with liquid silicon, intrinsic micro- and macrostructure in the carbon preform was retained within the final ceramics. The XRD, TGA, and microscopy analysis indicated that the final material exhibited a distinguished laminar structure with alternating arrangement of SiC and silicon layers. The thick SiC layer was composed of beta-SiC and a little of free silicon and un-reacted carbon. Studies on the evaluation of R-curves behavior by the indentation-strength method indicated a strong R-curve behavior for the Si/SiC composites.     

Novel method to produce β-TCP scaffolds

The production of ceramic scaffolds by a novel method was reported in this work. The method comprised the mixture of colloidal silica and β-tricalcium phosphate (β-TCP) powder, where paraffin microspheres were further added to provide the porosity in the scaffold after firing. Thermo-gravimetric analysis showed that the paraffin was completely degraded before 550 °C, where the heat treatment at 1100 °C was enough to remove the paraffin and provide porosity and mechanical strength. The scaffold had an open porosity, but with poor pore interconnection. The density of the scaffold was 1.11 ± 0.03 g/cm³ with a porosity of 64.98 ± 1.1%, and the compression strength was 5.02 ± 1.2 MPa.     

Interfacial control of uni-directional SiCf/SiC composites based on electrophoretic deposition and their mechanical properties

Interfacial control of uni-directional SiC_f/SiC composites were performed by EPD, and their mechanical properties at room temperature were evaluated. The effect of the thickness of carbon interphase on SiC fibers by EPD on mechanical properties of uni-directional SiC_f/SiC composites was also investigated. The average thickness of carbon coating on SiC fibers increased from 42 nm to 164 nm with an increase in the concentration of colloidal graphite suspension for EPD. Dense SiC_f/SiC composites were achieved and their fiber volume fraction was 47–51%. The SiC_f/SiC composites had a bending strength of 210–240 MPa. As the thickness of carbon coating was below 100 nm, the SiC_f/SiC composites (SC01 and SC02) fractured in almost brittle manner. In contrast, the SiC_f/SiC composites (SC03) showed a pseudo-ductile fracture behavior with a large number of fiber pullout as the thickness of carbon coating was above 100 nm. The fracture energy of SC03 was 3–4 times as high as those of SC01 and SC02 and the value was about 1.7 kJ/m². In consideration of the results of mechanical properties, the thickness of carbon coating on SiC fibers should be at least 100 nm to obtain high-performance SiC_f/SiC composites. The fabrication process based on EPD method is expected to be an effective way to control the interfaces of SiC_f/SiC composites and to obtain high-performance SiC_f/SiC composites.     

Friction and wear properties of TiCN coatings sliding against SiC and steel balls in air and water

The TiCN coatings were deposited on WC cemented carbides using enhanced cathodic arc magnetron sputtering. The topography of TiCN coatings were observed using scanning electron microscopy (SEM), the composition and structure of TiCN coatings were analyzed by energy dispersive spectroscopy (EDS) and X-ray diffraction (XRD). The friction and wear properties of TiCN coatings sliding against SiC and steel balls in air and water were investigated using ball-on-disk tribometer. The results showed that the TiCN coatings had a strong (111) preferred orientation. The friction coefficient and the specific wear rates of the TiCN/SiC tribopairs in air were higher than those in water. When the TiCN coatings slid against SiC balls in water, the friction coefficient and the specific wear rates first decreased, and then increased with the normal load, but decreased linearly with the sliding velocity. The lowest friction coefficient of 0.171 was obtained at 3 N and 0.4 m/s, while the lowest specific wear rate of the TiCN coatings was 2.3 × 10^− 6mm³/Nm at 6 N and 0.1 m/s. The TiCN coatings were worn out when the normal loads were higher than 6 N. When the TiCN coatings slid against the SUJ2 and SUS440C balls in water, the friction coefficient increased to 0.271 and 1.026 respectively. The EDS analysis showed that Fe and O elements existed on the wear track. This indicated that the tribochemical reaction occurred at the friction contact area.     

Aluminum matrix composites based on preceramic-polymer-bonded SiC preforms

Polymethylsiloxane (PMS) was used as a binder to make self-supporting SiC preforms for pressurized aluminum melt infiltration. The SiC particles were coated with preceramic polymer by spray drying; this ensured a fine and homogeneous distribution coupled with a high yield of the binder. The conditioned SiC powder mixtures were processed into preforms by warm pressing, curing and pyrolysis. A polymer content of 1.25 wt.% conferred sufficient stability to the preforms to enable composite processing. Using this procedure, SiC preforms with various SiC particle size distributions were prepared. The resulting Al/SiC composites with SiC contents of about 60 vol.% obtained by squeeze casting infiltration exhibit a 4-point bending strength of ∼500 MPa and Young’s moduli of ∼200 GPa. These values are comparable to those of compositionally identical, but binder-free composites. It is thus shown that the PMS-derived binder confers the desired strength to the SiC preforms without impairing the mechanical properties of the resulting Al/SiC composites.     

Hot-pressed A12O3–SiC(–C) composites with polycarbosilane as the precursor

The processing and mechanical behavior of Al₂O₃–xSiC (–C) (x = 1, 2, 5, 10 wt.%, ASx and ASCx) composites prepared by in situ reaction synthesis SiC from polycarbosilane (PCS) were investigated. The composites were densified by hot pressing. The pyrolysis process of PCS, microstructure, phase structure and mechanical properties of sintered composites were analyzed. Fully dense structure was obtained, and it was found that the fracture toughness and strength were highly improved compared with monolithic Al₂O₃. The fracture toughness reached 5.1 MPa m^1/2 in 1 wt.%SiC composite ASC1. AS1 showed 516 MPa of flexural strength.     

Mechanical properties of 3D KD-I SiCf/SiC composites with engineered fibre-matrix interfaces

Three-dimensional (3D) silicon carbide (SiC) matrix composites reinforced with KD-I SiC fibres were fabricated by precursor impregnation and pyrolysis (PIP) process. The fibre-matrix interfaces were tailored by pre-coating the as-received KD-I SiC fibres with PyC layers of different thicknesses or a layer of SiC. Interfacial characteristics and their effects on the composite mechanical properties were evaluated. The results indicate that the composite reinforced with as-received fibre possessed an interfacial shear strength of 72.1 MPa while the composite reinforced with SiC layer coated fibres had a much higher interfacial shear strength of 135.2 MPa. However, both composites showed inferior flexural strength and fracture toughness. With optimised PyC coating thickness, the interface coating led to much improved mechanical properties, i.e. a flexural strength of 420.6 MPa was achieved when the interlayer thickness is 0.1 μm, and a fracture toughness of 23.1 MPa m^1/2 was obtained for the interlayer thickness of 0.53 μm. In addition, the composites prepared by the PIP process exhibited superior mechanical properties over the composites prepared by the chemical vapour infiltration and vapour silicon infiltration (CVI-VSI) process.     

Effect of carbon nanofibers (CNFs) content on thermal and mechanical properties of CNFs/SiC nanocomposites

Carbon nanofibers dispersed β-SiC (CNFs/SiC) nanocomposites were prepared by hot-pressing via a transient eutectic phase route at 1900 °C for 1 h under 20 MPa in Ar. The effects of additional CNFs content between 1 and 10 wt.% were investigated, based on densification, microstructure, thermal and mechanical properties. The CNFs/SiC nanocomposites by the CNFs contents below 5 wt.% exhibited excellent relative densities over 98% with well dispersed CNFs. However, the CNFs/SiC nanocomposites containing the CNFs of 10 wt.% possessed a relative density of 92%, accompanying CNFs agglomerates and many pores located inside the agglomerates. The three point bending strength gradually decreased with the increase of CNFs content, but the indentation fracture toughness increased to 5.7 MPa m^1/2 by the CNFs content of 5 wt.%. The thermal conductivity was enchanced with the increase of CNFs content and represented a maximum value of 80 W/mK at the CNFs content of 5 wt.%.     

Pressure-pulsed chemical vapour infiltration of pyrolytic carbon into porous carbon or two-dimensional-carbon/SiC particulate preforms from C6H6–H2–N2

Pyrolytic carbon was infiltrated into porous carbon or two-dimensionally woven carbon fibre (2D-C)/SiC particulate preforms using pressure-pulsed chemical vapour infiltration from C6H6 (3–16%)–H2–N2 at 1273–1373 K. Residual porosity of porous carbon decreased from 29 to 10% after 1×104 pulses at 1323 K, and that of 2D-C/SiC particulate preform decreased from 30 to 7.5% after 4×104 pulses at 1273 K. Flexural strength of 2D-C/SiC preform reached about 150 MPa.     

Formation of microcrystalline SiC films by chemical transport with a high-pressure glow plasma of pure hydrogen

The formation of microcrystalline 3C-SiC films on Si substrates by the plasma-enhanced chemical transport method was investigated using a pure hydrogen glow plasma at 0.027 MPa. In this method, no source gas was necessary. Instead, the erosion products of a sintered 3C-SiC plate in a hydrogen plasma were used as the deposition source. By Fourier transform infrared (FT-IR) absorption gas analysis, the species generated by the hydrogen etching of sintered SiC were found to be SiH₄ and CH₄, which can serve as precursors for SiC film formation. The etch rate of sintered SiC by hydrogen plasma decreased with increasing source temperature. The maximum etch rate of the sintered SiC was 450 nm/min at an input power of 47 W/cm². Films prepared by this method at substrate temperatures (T_sub) of 600 and 1073 K were analyzed by FT-IR absorption spectroscopy. An absorption peak at 800 cm^- 1 related to Si-C bonds was clearly observed, but no significant hydrogen-related absorption peaks, such as C-H and Si-H, were observed in the prepared films. The deposition rate of SiC was about 8 nm/min, independent of T_sub. The SiC films had a columnar structure, and their surface morphologies revealed faceted growth. With decreasing T_sub, the lateral grain size became large. The current-voltage characteristics of a prepared SiC/Si heterojunction np diode showed rectifying behavior, demonstrating that the doping of an SiC film can be achieved without a doping gas source. The dopant distribution near the SiC/Si interface deduced from capacitance-voltage measurements suggests that the precise control of the initial growth stage is important to obtain a good SiC/Si interface.     

Preparation and microstructural evolution of carbon/carbon composites

Carbon/carbon (C/C) composites with characteristic matrix-crack pattern are key intermediate materials for preparation of carbon/silicon carbide (C/C–SiC) composites. The C/C composites were prepared by pyrolyzing carbon fiber/phenolic resin preform. The change of density, open porosity, mass loss and specially the microstructural evolution of the composites during pyrolysis at 200–900 °C was analyzed, which provided important information for preparation of C/SiC composites by infiltration of silicon. An increasing number of regular spacing cracks were formed above 400 °C. After pyrolysis at 900 °C, the pore volume was 0.17 cm³/g, and the pores in the radius range of 2.44–122.19 μm occupied 81% of the pore volume.     

Fracture behavior and mechanism of 2D C/SiC-BCx composite at room temperature

2D C/SiC composite was modified with partial BC_x matrix by low pressure chemical vapor infiltration technique (LPCVI), which was named as 2D C/SiC-BC_x composite. The flexural fracture behavior, mechanism, and strength distribution of 2D C/SiC-BC_x composite are investigated. The results indicate that the flexural strength, fracture toughness, and fracture work are 442.1 MPa, 22.84 MPa m^1/2, and 19.2 kJ m⁻², respectively. The flexural strength of C/SiC-BC_x composite decrease about 20% than that of C/SiC composite. However, the fracture toughness and fracture work increase about 19% and 18.5%, respectively. The properties varieties between C/SiC-BC_x composite and C/SiC composite can be attributed to the weak-bonding interface between BC_x/SiC matrices according to the results of detailed microstructure analysis. The strength distribution of 2D C/SiC-BC_x composite follows as Normal distribution or Weibull distribution with σ_u = 0, and m = 8.1393. The mean value of flexural strength for 2D C/SiC-BC_x composite is 443 MPa obtained by theory calculation, which is consistent with experiment result (442.1 MPa) very well.     

Effect of frequency and environment on fatigue behavior of a CVI SiC/SiC ceramic matrix composite at 1200 °C

The fatigue behavior of a SiC/SiC CMC (ceramic matrix composite) was investigated at 1200 °C in laboratory air and in steam environment. The composite consists of a SiC matrix reinforced with laminated woven Hi-Nicalon™ fibers. Fiber preforms had boron nitride fiber coating applied and were then densified with CVI SiC. Tensile stress-strain behavior and tensile properties were evaluated at 1200 °C. Tension-tension fatigue tests were conducted at frequencies of 0.1, 1.0, and 10 Hz for fatigue stresses ranging from 80 to 120 MPa in air and from 60 to 110 MPa in steam. Fatigue run-out was defined as 10⁵ cycles at the frequency of 0.1 Hz and as 2 × 10⁵ cycles at the frequencies of 1.0 and 10 Hz. Presence of steam significantly degraded the fatigue performance. In both test environments the fatigue limit and fatigue lifetime decreased with increasing frequency. Specimens that achieved run-out were subjected to tensile tests to failure to characterize the retained tensile properties. The material retained 100% of its tensile strength, yet modulus loss up to 22% was observed. Composite microstructure, as well as damage and failure mechanisms were investigated.     

Microstructure and mechanical properties of ZrB2-SiC composites

A ZrB₂-based composite containing 20 vol.% nanosized SiC particles (ZSN) was fabricated at 1900 °C for 30 min under a uniaxed load of 30 MPa by hot-pressing. The microstructure and mechanical properties of the composite were investigated. It was shown that the grain growth of ZrB₂ matrix was effectively suppressed by submicrosized SiC particles located along the grain boundaries. In addition, the mechanical properties of ZSN composite were strongly improved by incorporating the nanosized SiC particles into a ZrB₂ matrix, especially for flexural strength (925 ± 28 MPa) and fracture toughness (6.4 ± 0.3 MPa•m^1/2), which was much higher than that of monolithic ZrB₂ and ZrB₂-based composite with microsized SiC particles, respectively. The formation of intragranular nanostructures plays an important role in the strengthening and toughening of ZrB₂ ceramic.     

Effects of laser scans on the diffusion depth and diffusivity of gallium in n-type 4H-SiC during laser doping

An n-type 4H-SiC substrate has been doped with gallium using a continuous wave Nd:YAG laser to heat the sample to high temperatures but below the peritectic temperature of SiC. Mathematical models have been presented for the temperature and Ga concentration distributions in the sample. The Ga atoms, which are produced due to the thermal decomposition of a metallorganic precursor, diffuse into the sample by the solid-phase diffusion process at high temperatures. This process is modeled by considering the temperature-dependent diffusion coefficient and the Ga concentration profile was measured by the secondary ion mass spectrometry (SIMS). The concentration of Ga (6.25 × 10²⁰ cm⁻³) at the substrate surface was found to exceed the solid solubility limit (1.8 × 10¹⁹ cm⁻³) of Ga in SiC. Comparing the SIMS data to the results of the diffusion model, the activation energy, pre-exponential factor and diffusion coefficient of Ga were determined for different doping conditions. Four doped samples were produced by scanning the samples with a laser beam for different number of passes. The sample prepared with four passes showed the highest diffusion coefficient of 5.53 × 10⁻⁷ cm²/s with activation energy 1.84 eV and pre-exponential factor 1.05 × 10⁻² cm²/s. The diffusion coefficient is five orders of magnitude higher than the typical diffusion coefficient of Ga in SiC. This indicates that the laser doping process enhances the diffusion coefficient of dopant significantly.     

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.%.