Evolution of microstructure and tensile strength of Cansas-II SiC fibers under air oxidizing atmosphere

The influence of oxidation on the microstructure and tensile strength of Cansas-II SiC fibers at 900–1500 ℃ in the air was investigated in depth. The growth of β-SiC grains ordering as well as the increase of the size of free carbon in the SiC core occurred due to the thermal exposure. The thickness of the amorphous SiO₂ layer increases with the temperature, starting to transform to cristobalite at 1200 ℃. The activation energy in the ambient air is determined as 148KJ/mol, similar to that of Hi-Niaclon fibers (107∼151 KJ/mol). With the growth of the SiO₂ layer, lots of bubbles appeared in the SiO₂ layer due to the release of excess CO gas. Moreover, many cracks occurred on the fiber surface caused by the residual stress. The mean tensile strength decreased from initial 2.7 GPa to 0.3 GPa after the treatment at 1500 ℃, which could be mainly attributed to the SiO₂ layer.     

Protecting nuclear graphite from liquid fluoride salt and oxidation by SiC coating derived from polycarbosilane

Modification process has been conducted on commercial nuclear graphite IG-110 (Toyo Tanso Co., Ltd., Japan) by impregnation and pyrolysis of polycarbosilane (PCS) solution for getting the modified IG-110 (M-IG-110) coated by dense SiC coating for molten salt reactor. The microstructure and properties of graphite were systematically investigated and compared before and after the modification process. Results indicated that the M-IG-110 possessed of more excellent integrated properties including molten salt barrier property and oxidation resistance than bare IG-110 due to the filling effect of SiC particles in the pores of M-IG-110 and dense SiC coating adhering to the surface of M-IG-110. The fluoride salt infiltration amount of M-IG-110 under 5 atm was only 1.1 wt%, which was much less than 14.9 wt% for bare IG-110. The SiC coating derived from PCS exhibited remarkable compatibility with graphite substrate under high temperature and gave rise to excellent oxidation resistance of M-IG-110.     

Influence of tensile pre-fatigue stress on residual strength of SiC/(PyC/SiC)2/SiC minicomposites

The tensile-tension fatigue behavior of minicomposite SiC/(PyC/SiC)2/SiC at room temperature was studied, and the residual mechanical properties of specimens were tested after 10⁶ pre-fatigue cycles under different levels of stress. The results show that the residual strength first increases owing to the release of stress concentration and then decreases owing to excessive fiber wear. In addition, it is worth noting that the tensile curve of pre-fatigue specimens deflects twice; the first occurrence correlates with matrix crack reopening, and the second occurs when the uniaxial tensile load exceeds the pre-fatigue stress, and the degree of deflection also gradually decreases or almost disappears.     

In-situ formation of Ti3SiC2 interphase in SiCf/SiC composites by molten salt synthesis

Titanium silicon carbide (Ti₃SiC₂) film was synthesized by molten salt synthesis route of titanium and silicon powder based on polymer-derived SiC fibre substrate. The pre-deposited pyrolytic carbon (PyC) coating on the fibre was utilized as the template and a reactant for Ti₃SiC₂ film. The morphology, microstructure and composition of the film product were characterized. Two Ti₃SiC₂ layers form the whole film, where the Ti₃SiC₂ grains have different features. The synthesis mechanism has been discussed from the thickness of PyC and the batching ratio of mixed powder respectively. Finally, the obtained Ti₃SiC₂ film was utilized as interphase to prepare the SiC fibre reinforced SiC matrix composites (SiC_f/Ti₃SiC₂/SiC composites). The flexural strength (σ_F) and fracture toughness (K_IC) of the SiC_f/Ti₃SiC₂/SiC composite is 460 ± 20 MPa and 16.8 ± 2.4 MPa?m^1/2 respectively.     

Tensile behaviors of ECR-glass and high strength glass fibers after NaOH treatment

ECR-glass and high strength glass (S-glass) fibers were treated in 2 mol/l NaOH solution up to 5 h. The strength maintenance ratio and mass loss ratio of the fibers after treatment were investigated. The surface morphologies were characterized using scanning electron microscopy, and changes of chemical composition were analyzed by energy dispersive X-ray spectroscopy and Fourier transform infrared spectrometry. The alkali resistance and tensile strength of the S-glass fibers are higher compared to those of the ECR-glass fibers as they received less alkaline attack because of the more compact SiO₂ network and the formation of a protective layer on the S-glass fiber surface. The S-glass fibers have a higher mass loss due to the smaller diameter and thinner corrosion layer.     

Microstructure and tensile behavior of (BN/SiC)n coated SiC fibers and SiC/SiC minicomposites

Interphase plays an important role in the mechanical behavior of SiC/SiC ceramic-matrix composites (CMCs). In this paper, the microstructure and tensile behavior of multilayered (BN/SiC)_n coated SiC fiber and SiC/SiC minicomposites were investigated. The surface roughness of the original SiC fiber and SiC fiber deposited with multilayered (BN/SiC), (BN/SiC)₂, and (BN/SiC)₄ (BN/SiC)₈ interphase was analyzed through the scanning electronic microscope (SEM) and atomic force microscope (AFM) and X-ray diffraction (XRD) analysis. Monotonic tensile experiments were conducted for original SiC fiber, SiC fiber with different multilayered (BN/SiC)_n interfaces, and SiC/SiC minicomposites. Considering multiple damage mechanisms, e.g., matrix cracking, interface debonding, and fibers failure, a damage-based micromechanical constitutive model was developed to predict the tensile stress-strain response curves. Multiple damage parameters (e.g., matrix cracking stress, saturation matrix crack stress, tensile strength and failure strain, and composite’s tangent modulus) were used to characterize the tensile damage behavior in SiC/SiC minicomposites. Effects of multilayered interphase on the interface shear stress, fiber characteristic strength, tensile damage and fracture behavior, and strength distribution in SiC/SiC minicomposites were analyzed. The deposited multilayered (BN/SiC)_n interphase protected the SiC fiber and increased the interface shear stress, fiber characteristic strength, leading to the higher matrix cracking stress, saturation matrix cracking stress, tensile strength and fracture strain.     

Interface modification of carbon fibers with TiC/Ti2AlC coating and its effect on the tensile strength

A uniform TiC/Ti₂AlC gradient coating was obtained on carbon fibers via an in-situ reaction in molten salts. The results indicated that in-situ growth of TiC/Ti₂AlC coating caused strong interfacial bonding and surface defects. In this case, evident stress concentration was induced and cracks penetrated the fiber easily during tensile loading. Thus the tensile strength of carbon fibers was dramatically decreased to 78?±?13?MPa. In order to improve the performance of the as-prepared TiC/Ti₂AlC-coated carbon fibers, a pyrolytic carbon layer was pre-fabricated on carbon fibers. By introducing pyrolytic carbon layer, the interfacial bonding strength and surface defects were reduced accordingly. These improvements lead to a decrease of stress concentration and cracks propagation, and facilitate the interfacial debonding during tensile loading. As a result, the tensile strength of the fiber was significantly increased to 550?±?72?MPa. This fact indicates that pre-fabricating a pyrolytic carbon layer on carbon fibers is an effective method to improve the reliability of the TiC/Ti₂AlC-coated carbon fibers. The present work also provides a feasible way to fabricate TiC/Ti₂AlC interphase for high-performance Cf/SiC composites.     

Evolution of the structure and mechanical performance of Cansas-II SiC fibres after thermal treatment

Herein, an in-depth analysis of the effect of heat treatment at temperatures between 900 and 1500 °C under an Ar atmosphere on the structure as well as strength of Cansas-II SiC fibres was presented. The untreated fibres are composed of β-SiC grains, free carbon layers, as well as a small amount of an amorphous SiC_xO_y phase. As the heat-treatment temperature was increased to 1400 °C, a significant growth of the β-SiC grains and free carbon layers occurred along with the decomposition of the SiC_xO_y phase. Moreover, owing to the decomposition of the SiC_xO_y phase, some nanopores formed on the fibre surface upon heating at 1500 °C. The mean strength of the Cansas-II fibres decreased progressively from 2.78 to 1.20 GPa with an increase in the heat-treatment temperature. The degradation of the fibre strength can be attributed to the growth of critical defects, β-SiC grains, as well as the residual tensile stress.     

Molten salt synthesis of a SiC coating on graphite flakes for application in refractory castables

A silicon carbide coating was formed on the surface of graphite flakes by reaction of molten Si with carbon at 1100–1300 °C in a 95%KCl-5%NaF molten salt under Ar atmosphere. The effect of temperature and Si/graphite ratio in the initial mixture on the quality and the amount of SiC were investigated by XRD and SEM/EDS analyses. Also, the water wettability, oxidation resistance and zeta potential of un-coated and coated graphite were examined by TGA analysis and sedimentation test. The results show the amount of coating to increase in the coated flakes with increasing temperature and Si/graphite ratio. The SiC coating improves water wettability of graphite and acts as a protective layer to enhance oxidation resistance. The zeta potential of coated graphite was also increased which indicated a better dispersion in water based systems. These improvements in both the water dispersivity and oxidation resistance of SiC coated graphite would make it as promising candidate raw materials for application in C-containing refractory castables.     

Synthesis of photoluminescent polycrystalline SiC nanostructures via a modified molten salt shielded method

Polycrystalline SiC (3C-, 6H-, 24R- and 27H-) nanostructures are synthesized via a modified molten salt shielded synthesis method (m-MS³) in open air using Si and carbon black as the starting materials. The influences of salt species and their amount, and the sintering temperature, are discussed and optimized. Well crystalline SiC nanopowders composed of bountiful microstructures (nanoparticles, nanowires, nanosheets and nanoblocks) are successfully synthesized by m-MS³ at 1250 °C, with KCl and NaCl as the shielding salt. The polycrystalline SiC powders showed excellent photoluminescence property at an excitation wavelength of 330 nm and relatively small band gaps of 2.57–2.74 eV, which are quite attractive among reports for SiC-based materials. The investigation in this paper may provide a prototype strategy for protection-free synthesis of nanostructured SiC powders applicable for ultraviolet luminescence devices.     

Strength degradation of SiC fibers with a porous ZrB2-SiC coating: Role of the coating porous structure

ZrB₂-SiC coatings with varied porous structures were deposited on SiC fiber tows using the sol-gel method and cured at 1400 ℃ in vacuum. Tensile strength of the coated SiC fibers were much lower than that of the uncoated fibers. The bimodal distribution in the Weibull plot of the coated SiC fibers demonstrated that the fracture of the coated fiber can be attributed to two types of defects: the porous structure of the coating and the fiber defects. Detailed morphology and microstructure characterization of the coating and fiber combined with strength calculation were carried out to investigate the individual contribution of the fiber defects and the porous coating layer respectively. The results revealed that apart from the fiber damage during the coating process the porous structure of the fiber coating has a non-negligible effect on the fiber strength, presumably due to a relatively strong bonding between the fiber and coating.     

Development of oriented morphology and tensile properties upon superdawing of solution-spun fibers of ultra-high molecular weight poly(acrylonitrile)

The uniaxial drawing of UHMW-PAN fibers spun from a dilute solution into methanol coagulation baths at different temperatures and the resultant structure and tensile properties of the drawn products were studied. Although the initial morphology of the fibers and the deformation mode in a lower draw ratio (DR_t) range were significantly dependent on the temperatures of the coagulation bath, the tensile properties at a given DR_t, as well as the maximum achieved ones, were comparable. Both the tensile modulus and strength increased steadily with the DR_t and reached 35 and 1.8 GPa, respectively, at the highest DR_t of ∼80. These tensile properties are among the highest ever reported for PAN fibers. The achievement of such high tensile properties for extremely drawn fibers is ascribed to the conformational changes of crystalline chains from the 3/1 helix to the planar-zigzag with increasing DR_t, the improvement in the uniformity of the fiber diameter along the fiber axis, and the decrease in fiber diameter. Indeed, the tensile strength of fibers prepared from a dilute solution and having comparable moduli increased with a decrease in the fiber diameters. The reciprocal of the strength was proportional to the square root of the diameter as suggested by the Griffith theory. Extrapolation to a zero diameter yielded an ultimate tensile strength of 2.4±0.1 GPa for a fiber having a maximum achieved tensile modulus of 35±1 GPa.     

Direct comparison between monofilament and multifilament tow testing for evaluating the tensile strength distribution of SiC fibers

The tensile strength distributions of five types of silicon carbide (SiC) fiber, namely, Nicalon, Hi-Nicalon, Hi-Nicalon TypeS, Tyranno ZMI and Tyranno SA, were evaluated by monofilament and multifilament tow tensile testing with the estimated Weibull parameters being compared from each method. Whereas values for the Weibull scale parameter were found to be similar for both the monofilament and multifilament test methods, the Weibull shape parameter obtained from multifilament tow testing tended to be greater than that obtained from monofilament testing. The effect of diameter variation within individual fibers on the multifilament tow test results was investigated by Monte-Carlo simulations. In contrast with the experimentally obtained results, the shape parameters calculated by Monte-Carlo simulation exhibited good agreement with the monofilament test results.     

Effects of fabrication processes on the properties of SiC/SiC composites

Precursor infiltration and pyrolysis (PIP) and chemical vapor infiltration (CVI) were used to fabricate SiC/SiC composites on a four-step 3D SiC fibre preform deposited with a pyrolytic carbon interface. The effects of fabrication processes on the microstructure and mechanical properties of the SiC/SiC composites were studied. Results showed the presence of irregular cracks in the matrix of the SiC/SiC composites prepared through PIP, and the crystal structure was amorphous. The room temperature flexural strength and modulus were 873.62 MPa and 98.16 GPa, respectively. The matrix of the SiC/SiC composites prepared through CVI was tightly bonded without cracks, the crystal structure had high crystallinity, and the room temperature bending strength and modulus were 790.79 MPa and 150.32 GPa, respectively. After heat treatment at 1300 °C for 50 h, the flexural strength and modulus retention rate of the SiC/SiC composites prepared through PIP were 50.01% and 61.87%, and those of the composites prepared through CVI were 99.24% and 96.18%, respectively. The mechanism of the evolution of the mechanical properties after heat treatment was examined, and the analysis revealed that it was caused by the different fabrication processes of the SiC matrix. After heat treatment, the SiC crystallites prepared through PIP greatly increased, and the SiOxCy in the matrix decomposed to produce volatile gases SiO and/or CO, ultimately leading to an increase in the number of cracks and porosity in the material and a decrease in the material load-bearing capacity. However, the size of the SiC crystallites prepared through CVI hardly changed, the SiC matrix was tightly bonded without cracks, and the load-bearing capacity only slightly changed.     

Effects of laser surface remelting on the molten salt corrosion resistance of yttria-stabilized zirconia coatings

In the present study, atmospheric plasma-sprayed yttria-stabilized zirconia coatings were post-remelted by a continuous diode laser to improve the hot corrosion resistance for as-sprayed coatings. The coating surfaces were covered with a salt mixture (V₂O₅ and Na₂SO₄) and then subjected to a hot corrosion test at 1100?°C in air. The influence of laser parameters including power and scanning rate on the coating microstructure and corrosion resistance was investigated. Results showed that the hot corrosion resistance can be improved by producing a dense and smooth surface and reducing the coating permeability to the molten salt. The transformation of the hot corrosion mechanisms was clarified on the basis of the observed corrosion behaviors. A laser power of 1500?W and scanning rate of 9?mm/s can produce minimal surface roughness with few segmented cracks, which can provide improved performance of the hot corrosion resistance.     

Theoretical design and preparation of SiC whiskers catalyzed by Fe-oxides on carbon fibers

This work reported an in-situ vapor-liquid-solid (VLS) preparation method of SiC whiskers (SiC_w) catalyzed by Fe-oxides on carbon fibers, which could provide a method for preparing SiC_w/carbon fiber composites. The mechanism of the SiC_w was theoretically designed and then experimentally validated using XRD, SEM, and TEM. Fe₂O₃ was chosen as a Fe-oxide catalyst and directly loaded on carbon fibers by the impregnation process. The results showed that SiC_w were successfully prepared on carbon fibers at 1600 °C under the protection of flowing nitrogen, utilizing quartz and graphite as gas-phase generation sources. The prepared SiC_w were β-SiC and grew along the (111) crystal plane, with spherical droplets on top formed by Fe₂O₃ catalysts. SiC_w were microstructurally observed to have widths of 500–1000 nm and lengths of more than 15 μm, respectively.     

Effect of surface treatments on the thermal behavior and tensile strength of piassava (Attalea funifera) fibers

Piassava (Attalea funifera) fibers subjected to several surface chemical treatments and as‐received raw fibers were compared with respect to their thermal and tensile behaviors. The thermal degradation of the raw fibers was characterized by three main stages that corresponded to water release at low temperatures, decomposition of hemicellulose, and decomposition of α cellulose. Mercerization acted mainly on hemicellulose removal, and there was no change in the hydrophilic behavior of the fibers. The removal of hemicellulose split the fibers into microfibrils and favored the thermal decomposition of α cellulose. The same behavior was observed when the fibers were subjected to mercerization and acetylation. The fibers subjected to only acetylation showed thermal behavior similar to that of the raw fibers. With the acetylation treatment, a minor decrease in the hydrophilic character of the fibers was noted. Despite some differences in the thermal behavior, the tensile strengths of the raw and treated fibers were statistically equal. Complementary Fourier transform infrared and scanning electron microscopy analysis corroborated the thermogravimetric analysis/differential thermogravimetry results. © 2010 Wiley Periodicals, Inc. J Appl Polym Sci, 2011     

The relationship between microstructure and flexural strength of pressureless liquid phase sintered SiC ceramics oxidized at elevated temperatures

The oxidation behavior of pressureless liquid phase sintered SiC ceramics with Al₂O₃ and Y₂O₃ as sintering additives was investigated in the temperature range from 1000 °C to 1600 °C at the interval of 100 °C for 5 h. The relationship between residual flexural strength and microstructure was analyzed in detail. It was found that the SiC specimens suffered from mild oxidation below 1300 °C. The flexural strength of SiC specimens after oxidation at 1100 °C was the highest (90% of the original strength) due to the formation of dendritic grains, which filled pores and healed cracks. And the flexural strength was almost above 80% of the original flexural strength when the oxidation temperature was below 1300 °C. Meanwhile, the weight of specimens underwent steady increase. However, when the oxidation temperature was elevated to above 1400 °C, the specimens began to suffer from severe oxidation, which resulted in a lot of through pores and cracks on the surface, bringing about the sharp decrease of flexural strength to 30% of original strength when the oxidation temperature of 1600 °C was reached. And the weight of the specimens after huge increase began to show downtrend when the oxidation temperature was elevated to 1600 °C due to the spalling of oxidation products.     

Effects of oxidation on the strength of debound SiC parts by powder injection moulding

In order to increase the production efficiency of powder injection moulding for SiC parts, thermal debinding was performed in air furnace without gas shield. Bending tests were performed to evaluate the strength of samples debound under different temperatures. The effects of oxidation on debinding process were also analyzed. Analysis indicates that air could accelerate the debinding rate of green parts without defects occurring. The bending strength of debound samples increases from 6.55 MPa to 11.58 MPa as the pre-sintering temperature increases from 550 °C to 850 °C. On the other hand, the bending strength of the samples pre-sintered at 1200 °C in argon atmosphere is only 11.52 MPa. It was found that, blanks have enough strength for transport after being pre-sintered in air atmosphere at 850 °C. The technology could reduce the requirement for heating equipment and enhance the efficiency of debinding for SiC parts.     

Revealing the formation mechanism of the skin-core structure in nearly stoichiometric polycrystalline SiC fibers

The polymer-derived SiC fibers have broad application prospects in the fields of aerospace, nuclear industry and high-tech weapon. Oxygen plays an essential role in adjusting the composition, structure and tensile strength of SiC fibers. Our studies have found that introducing too much oxygen during air curing process will form the skin-core structure in nearly stoichiometric polycrystalline SiC fibers. In order to reveal the formation mechanism of the skin-core structure, gradient oxygen was introduced into the fibers. The morphologies, phase distributions and defects of the fibers were well characterized. By strictly controlling the introduction of oxygen, the polycrystalline product fiber exhibits intragranular fracture behavior and excellent high-temperature resistance. The retention rate of its tensile strength can reach up to 91% and 61% after exposure at 1800 °C for 1 h and 10 h, respectively. The present results give valuable insights into the structural optimization of the nearly stoichiometric polycrystalline SiC fibers.