Model for SiC fiber strength after oxidation in dry and wet air

The strengths of oxidized SiC fibers were modeled from the effects of SiO₂ scale residual stress on fracture. Surface tractions from scale residual stress were determined for SiC surface flaws. The residual stress was the sum of the growth stress from oxidation volume expansion, thermal stress from SiO₂-SiC thermal expansion mismatch, and stress from phase transformations in crystallized scale. The partial relaxation of tensile residual stress from scale cracking was also calculated. Scale thicknesses were determined using Deal-Grove oxidation kinetics for glass and crystalline scales. Kolmogorov-Johnson-Mehl-Avrami (KJMA) kinetics was used to determine scale crystallization rates. Strengths of fibers with glass and with crystalline scales formed by oxidation in dry and wet air between 600° and 1400°C were modeled. The effects of partially crystallized scales were calculated using Weibull statistical methods. Modeled strengths were compared with measurements. Slight strength increases after glass scale formation, large decreases that accompany scale crystallization, and some differences between dry and wet air oxidation were accurately modeled. This suggests that under some conditions the scale residual stress dominates the changes in strength after SiC fiber oxidation. However, modeled strengths were significantly higher than those measured for some fibers oxidized in wet air, which suggests another degradation mechanism is active for these conditions. Modeling assumptions and implications for SiC fiber strength after oxidation for long times are discussed.     

Oxidation of 3D-printed SiC in air and steam environments

The high-temperature oxidation of additively manufactured and chemically vapor infiltrated (3D-printed SiC) has been compared to chemical vapor deposited (CVD) SiC. 100-h isothermal exposures were conducted at 1425° and 1300°C at 1 atm under both dry air and steam environments. A SiC reaction tube was utilized to reduce silica volatility. After steam oxidation at 1425° and 1300°C, on the 3D-printed SiC surface, which was intrinsically rougher than the CVD surface, scales were 70%–90% thicker at the convex regions compared to concave/flat regions. In the convex regions, large cracks perpendicular to the oxidizing interface were observed. After dry air oxidation, scale thicknesses were comparable between 3D-printed SiC and CVD SiC, regardless of geometry. Finite element modeling, conducted to elucidate the relationship between SiC geometry and ß- to α-cristobalite transformation stress, determined cristobalite transformation tensile stresses to be on the order of 10³ MPa during cool down, assuming a 6 vol% reduction. Compared to flat SiC substrates, tensile transformation stresses were elevated at concave regions and relaxed at convex regions. Combined with specimen mass gain (accounting for the rougher surface) of 3D-printed SiC being 15%–32% higher for 3D-printed SiC after 1300°C and 1425°C steam oxidation, the work presented concludes that the increased oxidation of 3D-printed SiC is primarily caused by tensile hoop stresses driven by oxidation volume expansion. Lastly, the efficacy of the 3D-printing method is demonstrated through the production of tristructural isotropic imbedded 3D-printed SiC fuel forms.     

SiOC modified carbon-bonded carbon fiber composite with SiC nanowires enhanced interfibrous junctions

Carbon-bonded carbon fiber (CBCF) composites are promising lightweight and high efficient thermal insulators to be applied in aerospace area, but their practical applications are usually restricted by the low mechanical performance and poor oxidation resistance. To overcome these drawbacks, many efforts have been made in the fabrication of ceramic coated CBCF composites. However, the densities of these modified composites are usually very high, which would result in the reduction in their thermal insulation performance. Herein, we prepared a CBCF composite with SiC nanowires enhanced interfibrous junctions and SiOC ceramic coated carbon fibers (SiCNWs-SiOC-CBCF). Similar to CBCF, the SiCNWs-SiOC-CBCF exhibits a low density of 0.35 g/cm³ and an anisotropic and highly porous architecture. The SiCNWs-SiOC-CBCF possesses a compressive strength of 3.8 MPa and a compression modulus of 195.7 MPa in the X (or Y) direction, ~26.7% and 150% higher than those of CBCF respectively. It can also suffer from an isothermal treatment in air at 900°C for 120 minutes. The combination of these properties makes the SiCNWs-SiOC-CBCF a good candidate for thermal insulator to be applied in extreme conditions.     

Oxidation kinetics strength of Hi‐NicalonTM‐S SiC fiber after oxidation in dry and wet air

Hi‐Nicalon?‐S SiC fiber strengths and Weibull moduli were measured after oxidation for up to 100 hours between 700°C and 1400°C in wet and dry air. SiO₂ scale thickness and crystallization extent were measured by TEM. The effect of furnace environment on trace element levels in the SiO₂ scales was characterized by secondary ion mass spectroscopy. Crystallization kinetics and Deal‐Grove oxidation kinetics for glass and crystalline scale, and the transition between them, were modeled and determined. Crystallization retards oxidation kinetics, and scale that formed in the crystalline state was heavily deformed by the growth stress accompanying SiC oxidation volume expansion. Glass scales formed in dry air slightly increased fiber strength. Glass scales formed in wet air did not increase strength, and in some cases significantly decreased strength. Scales more than 200 nm thick were usually partially or completely crystallized, which degraded fiber strength. Contamination of scales by trace impurities such as Al and Ca during heat treatment inhibited crystallization. The oxidation kinetics and the strengths of oxidized Hi‐Nicalon?‐S fibers are compared with previous studies on SiC fibers, bulk SiC, and single‐crystal SiC. Empirical relationships between oxidation temperature, time, scale thickness, and strength are determined and discussed.     

Effect of BN nanoparticle content in SiC matrix on microstructure and mechanical properties of SiC/SiC composites

BN-nanoparticle-containing SiC-matrix-based composites comprising SiC fibers and lacking a fiber/matrix interface (SiC/BN + SiC composites) were fabricated by spark plasma sintering (SPS) at 1800°C for 10 min under 50 MPa in Ar. The content of added BN nanoparticles was varied from 0 to 50 vol.%. The mechanical properties of the SiC/BN + SiC composites were investigated thoroughly. The SiC/BN + SiC composites with a BN nanoparticle content of 50 vol.%, which had a bulk density of 2.73 g/cm³ and an open porosity of 5.8%, exhibited quasiductile fracture behavior, as indicated by a short nonlinear region and significantly shorter fiber pullouts owing to the relatively high modulus. The composites also exhibited high strength as well as bending, proportional limit stress, and ultimate tensile strength values of 496 ± 13, 251 ± 30, and 301 MPa ± 56 MPa, respectively, under ambient conditions. The SiC fibers with contents of BN nanoparticles above 30 vol.% were not severely damaged during SPS and adhered to the matrix to form a relatively weak fiber/matrix interface.     

Stress rupture of SiC/SiC composite tubes under high-temperature steam

SiC-fiber–reinforced SiC matrix composite cladding for light water reactor fuel elements must withstand high-temperature steam oxidation in a loss-of-coolant accident scenario (LOCA). Current composite designs include an outer monolithic SiC layer, in part, to increase steam oxidation resistance. However, it is not clear how such a structure would behave under high-temperature steam in the case when the monolithic layer cracks and carbon interphases and SiC fibers are exposed to the environment. To fill this knowledge gap, stress-rupture tests of prototypic SiC composite cladding at 1000°C under steam and inert environments were conducted. The applied stress was ∼120 MPa, which was beyond the initial cracking stress. The failure lifetime under steam was 400–1300 s, while 75% of the composite specimens did not fail after 3 h of total exposure under inert gases. Microstructural observations suggest that steam oxidation activated slow crack growth in the fibers, which led to failure of the composite. The results from this study suggest that stress rupture in steam environments could be a limiting factor of the cladding under reactor LOCA conditions.     

Passive oxidation kinetics for glass and cristobalite formation on Hi‐Nicalon™‐S SiC fibers in steam

Parabolic rate constants for SiO₂ glass ( B _G ) and cristobalite ( B _C ) scale formation during passive oxidation of SiC in steam were determined. Cristobalite scale that originally formed as glass and as scale that formed afterward, directly as cristobalite, was distinguished by TEM. A method to determine B _G and B _C from many thickness measurements of the 2 different scale layers was developed. The method was applied to Hi‐Nicalon?‐S SiC fiber oxidation in Si(OH)₄ saturated steam between 500 and 1600°C. At 1500°C and lower temperatures, glass scale formed more rapidly than cristobalite scale. B _G and B _C had activation energies of 80 ± 5 kJ/mol and 95 ± 5 kJ/mol, respectively. At 1600°C, cristobalite scales formed much faster than glass scales. Many scales spheroidized after oxidation at temperatures beneath 1000°C, and continuous scales that did form had wide variation in thickness. This made kinetics analysis after low temperature steam oxidation problematic.     

Na2SO4 deposit-induced hot corrosion of SiC fibers relevant for SiC CMCs

Hi Nicalon, Hi Nicalon S, Sylramic, and Sylramic iBN SiC fibers were exposed to ~60 μg/cm² of Na₂SO₄ in a 0.1% SO₂/O₂ gaseous environment for times between 0.75 and 24 h at 1000°C. After exposure, the corrosion products were characterized using SEM, EDS, ICP-OES, TEM, and EFTEM to determine their high-temperature resistance to Na₂SO₄ and key reaction mechanisms. All SiC fiber types tested in this work exhibited little resistance to Na₂SO₄ deposit-induced attack relative to their behavior in dry O₂ environments. It was found that Hi-Nicalon displayed the least resistance to Na₂SO₄ deposit-induced attack due to excess carbon content resulting in the formation of a highly porous crystalline oxide and promotion of basic corrosion conditions. All fiber types formed a crystalline SiO₂ reaction product, either cristobalite or tridymite. Sylramic and Sylramic iBN formed a crystalline SiO₂ reaction layer containing TiO₂ needles due oxidation of TiB₂ particles. Additionally, Na₂SO₄ deposits resulted in pitting of all fiber surfaces.     

Synthesis and thermal shock evaluation of porous SiC ceramic foams for solar thermal applications

Reticulated porous ceramics with structural features spanning across multiple length scales are emerging as the primary media in a variety of demanding mass and heat transfer applications, most notably solar-assisted synthetic fuel processing. In this study, we focus on engineering of the open pore silicon carbide (SiC)-based foams in such catalytic applications. We evaluate the mechanical integrity and thermal stability of these porous structures. X-ray tomography analyses of the 3D structures reveal the presence of dual pore size distribution different by up to an order of magnitude in length scale. We further study the effect of thermal shock—induced via water quenching—on the SiC structures and we conclude that the mechanical properties of the ceramic foams are significantly reduced after thermal stress. Comparison of SEM micrographs—before and after thermal shock—reveals that needle-like features appear inside the foam matrix. These elongated defects may be responsible for structural and mechanical weakening.     

低压化学气相渗透法制备2.5维SiCf/SiC复合材料

采用低压化学气相渗透法制备了具有和不具有热解炭界面层的2.5维连续SiC纤维增强的SiC复合材料(SiCf/SiC).SiC纤维的体积分数为30%和41%.所制备复合材料的气孔率为20%左右.当纤维为30%时,沉积有0.1 μm热解炭界面层的复合材料的弯曲强度由未加热解炭界面层的232MPa增加到328MPa,而且材料由灾难性断裂转变为非灾难性断裂.在同一制备条件下,纤维体积分数为41%的SiCf/SiC比30%的SiCf/SiC具有更高的气孔率.纤维为41%时,热解炭界面层厚度为0.1 μm的SiCf/SiC的弯曲强度只有244MPa,但是它具有更高的韧性和更长的纤维拔出长度.     

Models Proposed to Explain the Electrical Conductivity of Polymer‐Derived Silicon Carbide Fibers

Two types of silicon carbide fibers (SiC_f) were prepared employing different pyrolysis techniques. The relationship between the microstructure and the electrical resistivity of the fibers was investigated. The results indicated that the carbon layer present on the fiber surface acted as the main conductive phase in the SiC_f obtained by direct pyrolysis, whereas a free carbon phase determined the conductivity of the SiC_f prepared by the preheated pyrolysis method. A core‐shell model and a general effective media (GEM) theory were proposed to explain the conductivity of different types of SiC_f. Quantitative analysis based on these models indicated an electrical resistivity of ~10^?2 Ω·cm for the carbon layer on the surface of SiC_f obtained by direct pyrolysis. The electrical resistivity and the percolation threshold of the free carbon in SiC_f prepared by the preheated pyrolysis method were 10^?1 Ω·cm and 11.3% respectively.     

Effects of SiC whisker addition on mechanical,thermal, and permeability properties of porous silica-bonded SiC ceramics

The effects of SiC whisker addition into nano-SiC powder-carbon black template mixture on flexural strength, thermal conductivity, and specific flow rate of porous silica-bonded SiC ceramics were investigated. The flexural strength of 1200°C-sintered porous silica-bonded SiC ceramics increased from 9.5 MPa to 12.8 MPa with the addition of 33 wt% SiC whisker because the SiC whiskers acted as a reinforcement in porous silica-bonded SiC ceramics. The thermal conductivity of 1200°C-sintered porous silica-bonded SiC ceramics monotonically increased from 0.360 Wm^–1K^–1 to 1.415 Wm^–1K^–1 as the SiC whisker content increased from 0 to 100 wt% because of the easy heat conduction path provided by SiC whiskers with a high aspect ratio. The specific flow rate of 1200°C-sintered porous SiC ceramics increased by two orders of magnitude as the SiC whisker content increased from 0 to 100 wt%. These results were primarily attributed to an increase in pore size from 125 nm to 565 nm and secondarily an increase in porosity from 49.9% to 63.6%. In summary, the addition of 33 wt% SiC whisker increased the flexural strength, thermal conductivity, and specific flow rate of porous silica-bonded SiC ceramics by 35%, 133%, and 266%, respectively.     

The effects of adding nano-alumina filler on the properties of polymer-derived SiC coating

In this paper, SiC coating was prepared using the polymer-derived ceramic method; then the effect of nano-alumina as a filler material was studied. First of all, polycarbosilane(PCS) was dissolved in xylene; after that, different amounts of nano-alumina particles were added to the solution. The coating was deposited on the alumina substrate using the dip-coating method; this was followed by sintering at 1200℃. The phase content and microstructure of the samples were studied by X-ray diffraction and scanning electron microscope methods, respectively. Nanohardness, Young's modulus, and coating adhesion were investigated by a nanoindentation method. The sheet resistance was evaluated using the four-point probe technique; also, the wear resistance of the coating was studied by applying the pin-on-disk method. It was found that the addition of the nano-alumina filler up to 20 wt% drastically improved the adhesion and wear resistance of the SiC coating.     

Microstructure and Mechanical Properties of Three-Dimensional Textile Hi-Nicalon SiC/SiC Composites by Chemical Vapor Infiltration

Three-dimensional textile Hi-Nicalon SiC-fiber-reinforced SiC composites were fabricated using chemical vapor infiltration. The microstructure and mechanical properties of the composite materials were investigated under bending, shear, and impact loading. The density of the composites was 2.5 g·cm⁻³ after the three-dimensional SiC perform was infiltrated for 30 h. The values of flexural strength were 860 MPa at room temperature and 1010 MPa at 1300°C under vacuum. Above the infiltration temperature, the failure behavior of the composites became brittle because of the strong interfacial bonding and the mismatch of thermal expansion coefficients between fiber and matrix. The fracture toughness was 30.2 MPa·m^1/2. The obtained value of shear strength was 67.5 MPa. The composites exhibited excellent impact resistance, and the dynamic fracture toughness of 36.0 kJ·m⁻² was measured using Charpy impact tests.     

Oxidation Effects on the Mechanical Properties of a SiC-Fiber-Reinforced Reaction-Bonded Si3N4 Matrix Composite

The room-temperature mechanical properties of a SiC-fiberreinforced reaction-bonded silicon nitride composite were measured after 100 h treatment in nitrogen and oxygen environments to 1400°C. The composite heat-treated in nitrogen to 1400°C showed no appreciable loss in properties. In contrast, composites heat-treated in oxygen from 600° to 1000°C retained ∼65% and 35% of the matrix fracture and ultimate strength, respectively, of the as-fabricated composites, and those heat-treated from 1200° to 1400°C retained greater than 90% and 65% of the matrix fracture and ultimate strength, respectively, of the as-fabricated composites. For all nitrogen and oxygen treatments, the composite displayed strain capability beyond the matrix fracture strength. Oxidation of the fiber surface coating, which caused degradation of bond between the fiber and matrix and reduction in fiber strength, appears to be the dominant mechanism for property degradation of the composites oxidized from 600° to 1000°C. Formation of a protective silica coating at external surfaces of the composites at and above 1200°C reduced oxidation of the fiber coating and hence degrading effects of oxidation on their properties.     

Fatigue behavior and relation between fatigue resistance and tensile properties of poly(para-phenylene-co-3,4'-oxydiphenylene terephthalamide) fiber

The poly(para-phenylene-co-3,4′-oxydiphenylene terephthalamide) (PPODTA) fiber is one of the high strength organic fibers, and it has been reported that the PPODTA fiber has superior fatigue resistance. The high strength fibers are used in the applications to utilize their high mechanical properties in general. Therefore, the long-term durability of these fibers is also required. In this study, the fatigue tests were conducted for the PPODTA fibers. As a result, it was found that the PPODTA fibers were able to be fractured by the cyclic tensile stress, and the fatigue behavior was influenced by the stress conditions. In addition, the single fiber tensile tests were also conducted for the PPODTA fibers, and the relation between the tensile properties and the fatigue resistance of the PPODTA fiber was investigated. The fatigue resistance of the PPODTA fiber was increased with the decrease of the fiber diameter and the increase of the tensile modulus.     

Effect of Interface Mechanical Properties on Pullout in a SiC-Fiber-Reinforced Lithium Aluminum Silicate Glass-Ceramic

The pullout of fibers in the crack wake makes an important contribution to the toughness of ceramic-matrix composites. The pullout is, in turn, influenced by the properties of the fibers and by the sliding resistance of the interface. Basic relationships governing the pullout are developed analytically and investigated experimentally using a lithium aluminum silicate/silicon carbide (LAS/SIC) composite subjected to various heat treatments. The experiments involve determining the strengths of single fibers and then measuring the pullout distributions. The results are used to provide a consistent view of the pullout process and related changes in mechanical properties.     

Mechanical Behavior of a Continuous-SiC-Fiber-Reinforced RBSN-Matrix Composite

The results of a detailed study are presented on the toughening of reaction-bonded silicon nitride reinforced with large-diameter SiC monofilaments at ambient and elevated temperatures. Composite stiffness, strength, toughness, and R -curve behavior were investigated at ambient temperature, with strengths measured up to 1400°C. At elevated temperature, toughening mechanisms were explored by investigating crack initiation and growth under creep conditions. The results show that, at ambient temperature, the composite exhibited noncatastrophic failure with substantial toughening associated with contributions of both fiber pullout and elastic bridging of fibers in the crack wake, consistent with predictions using available models. Limited R -curve measurements suggest that large-scale bridging effects may be present. At elevated temperature, crack initiation occurred in the matrix at about 1000°C, but in the fiber at higher temperatures. Growth of cracks is governed by time-dependent bridging of unbroken fibers in the crack wake, consistent with a model based on fiber pullout by viscous sliding of fibers out of the matrix along amorphous interfacial layers.     

Tensile Rupture Strength and Fracture Defects of Sintered Silicon Carbide

The tensile strength distribution of sintered silicon carbide was measured at room temperature and 1300°C in air and fracture defects were characterized. The measured strength was compared with strength obtained from flaw characteristics and fracture toughness assuming a peripherally cracked spherical void model.