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.     

High mechanical performance SiC/SiC composites by NITE process with tailoring of appropriate fabrication temperature to fiber volume fraction

Unidirectional SiC/SiC composites are prepared by nano-powder infiltration and transient eutectic-phase (NITE) process, using pyrolytic carbon (PyC)-coated Tyranno-SA SiC fibers as reinforcement and SiC nano-powder with sintering additives for matrix formation. The effects of two kinds of fiber volume fraction incorporating fabrication temperature were characterized on densification, microstructure and mechanical properties. Densification of the composites with low fiber volume fraction (appropriately 30 vol%) was developed even at lower fabrication temperature of 1800 °C, and then saturated at 3rd stage of matrix densification corresponding to classic liquid phase sintering. Hence, densification of the composites with high volume fraction (above 50 vol%) became restricted because the many fibers retarded the infiltration of SiC nano-powder at lower fabrication temperature of 1800 °C. When fabrication temperature increased by 1900 °C, densification of the composites was effectively enhanced in the intra-fiber-bundles and simultaneously the interaction between PyC interface and matrix was strengthened. SEM observation on the fracture surface revealed that fiber pull-out length was accordingly changed with fabrication temperature as well as fiber volume fraction, which dominated tensile fracture behaviors. Through NITE process, SiC/SiC composites with two fracture types were successfully developed by tailoring of appropriate fabrication temperature to fiber volume fraction as follows: (1) high ductility type and (2) high strength type.     

Stress-dependence and time-dependence of the post-fatigue tensile behavior of carbon fiber reinforced SiC matrix composites

The major objective of this paper is to phenomenally report the stress-dependence and time-dependence of fatigue damage to C/SiC composites, and to tentatively discuss the effects of the fatigue stress levels and the fatigue cycles on the post-fatigue tensile behavior. Results show that compared with the virgin strength of the as-received C/SiC specimens, the tensile strengths of the as-fatigued specimens after 86,400 cycles were increased by 8.47% at the stresses of 90 ± 30 MPa, 23.47% at 120 ± 40 MPa, and 9.8% at 160 ± 53 MPa. As cycles continued, however, the post-fatigue strength of the composites gradually decreased after the peak of 23.47%, at which the optimal strength enhancement was obtained because the mean fatigue stress of 120 MPa was the closest to thermal residual stress (TRS), and caused TRS relieve largely during the fatigue. Most interestingly, there was a general inflexion appeared on the post-fatigue tensile stress-strain curves, which was just equal to the historic maximum fatigue stress acted upon the as-fatigued specimens. Below this inflexion stress the tensile curves revealed the apparent linear behavior with little AE response, and above that nonlinearity with new damage immediately emitted highly increase rate of AE activities. This ‘stress memory’ characteristic was strongly relevant to damaged microstructures of the as-fatigued composites in the form of the coating/matrix cracks, interface debonding/wear, and fiber breaking, which resulted undoubtedly in reduction of modulus but in proper increase of strength via TRS relief.     

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.%.     

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.     

Creep of Nextel™720/alumina–mullite ceramic composite at 1200 °C in air,argon, and steam

The tensile creep behavior of an oxide–oxide continuous fiber ceramic composite was investigated at 1200 °C in laboratory air, in steam and in argon. The composite consists of a porous alumina–mullite matrix reinforced with laminated, woven mullite/alumina (Nextel™720) fibers, has no interface between the fiber and matrix, and relies on the porous matrix for flaw tolerance. The tensile stress–strain behavior was investigated and the tensile properties measured at 1200 °C. The elastic modulus was 74.5 GPa and the ultimate tensile strength was 153 MPa. Tensile creep behavior was examined for creep stresses in the 70–140 MPa range. Primary and secondary creep regimes were observed in all tests. Creep run-out (set to 100 h) was achieved in laboratory air for creep stress levels ?91 MPa. The presence of either steam or argon accelerated creep rates and reduced creep lifetimes. Composite microstructure, as well as damage and failure mechanisms were investigated.     

Interfacial load transfer in carbon nanotube/ceramic microfiber hybrid polymer composites

Growing carbon nanotubes (CNTs) on the surface of fibers has the potential to modify fiber–matrix interfacial adhesion, enhance the composite delamination resistance, and possibly improve its toughness and any matrix-dominated elastic property as well. In the present work aligned CNTs were grown upon ceramic fibers (silica and alumina) by chemical vapor deposition (CVD) at temperatures of 650 °C and 750 °C. Continuously-monitored single fiber composite (SFC) fragmentation tests were performed on pristine as well as on CNT-grown fibers embedded in epoxy. The critical fragment length, fiber tensile strength at critical length, and interfacial shear strength were evaluated. Significant increases (up to 50%) are observed in the fiber tensile strength and in the interfacial adhesion (which was sometimes doubled) with all fiber types upon which CNTs are CVD-grown at 750 °C. We discuss the likely sources of these improvements as well as their implications.     

Reinforcing potential of micro- and nano-sized fibers in the starch-based biocomposites

Starch-based biocomposites reinforced with jute (micro-sized fiber) and bacterial cellulose (BC) (nano-sized fiber) were prepared by film casting. Reinforcement in the composites is essentially influenced by fiber nature, and amount of loading. The optimum amount of fiber loading for jute and bacterial cellulose in each composite system are 60 wt% and 50 wt% (of starch weight), respectively. Mechanical properties are largely improved due to the strong hydrogen interaction between the starch matrix and cellulose fiber together with good fiber dispersion and impregnation in these composites revealed by SEM. The composites reinforced with 40 wt% or higher bacterial cellulose contents have markedly superior mechanical properties than those reinforced with jute. Young’s modulus and tensile strength of the optimum 50 wt% bacterial cellulose reinforced composite averaged 2.6 GPa and 58 MPa, respectively. These values are 106-fold and 20-fold more than the pure starch/glycerol film. DMTA revealed that the presence of bacterial cellulose (with optimum loading) significantly enhanced the storage modulus and glass transition temperature of the composite, with a 35 °C increment. Thermal degradation of the bacterial cellulose component occurred at higher temperatures implying improved thermal stability. The composites reinforced with bacterial cellulose also had much better water resistance than those associated with jute. In addition, even at high fiber loading, the composites reinforced by bacterial cellulose clearly retain an exceptional level of optical transparency owing to the effect of the nano-sized fibers and also good interfacial bonding between the matrix and bacterial cellulose.     

Dynamic compressive behavior of unidirectional IM7/5250-4 laminate after thermal oxidation

Fiber reinforced high temperature polymer matrix composites are currently gaining wide usage in aircraft structures, especially in airframe and engine inlet casing. The failure of composites in worst-case operational conditions mandates the extensive investigation of the mechanical behavior, and the durability in long-term performance and service life under thermal oxidation. In this work, unidirectional IM7 carbon fiber reinforced high-temperature BMI resin composite (IM7/5250-4) were isothermally aged in air for 2 months at 195 °C and 245 °C, respectively. The dynamic behavior of thermally aged composites was investigated on a split Hopkinson pressure bar (SHPB) in three principal directions. The results indicate that thermal oxidation leads to significant reduction in both stiffness and strength of the composites. Optical micrographs of fracture surface and failure pattern of composite after SHPB impact reveals oxidation induced debonding along the fiber–matrix interface due to oxygen diffusion under long-term exposure to elevated temperatures.     

Covalent functionalization of graphene with organosilane and its use as a reinforcement in epoxy composites

Functionalized graphene nanosheets (f-GNSs) produced by chemically grafting organosilane were synthesized by a simple covalent functionalization with 3-aminopropyl triethoxysilane. The f-GNSs showed a larger thickness, but smaller width and than the un-treated graphene. The covalent functionalization of graphene with silane was favorable for their homogeneous dispersion in the polymer matrix even at a high nanofiller loading (1 wt.%). The initial thermal degradation temperature of epoxy composite was increased from 314 °C to 334 °C, at a f-GNS content of 1 wt.%. Meanwhile, the addition of 1 wt.% f-GNSs increased the tensile strength and elongation to failure of epoxy resins by 45% and 133%, respectively. This is believed to be attributed to the strong interfacial interactions between f-GNSs and the epoxy resins by covalent functionalization. The experimentally determined Young’s modulus corresponded well with theoretical simulation under the hypothesis that the graphene sheets randomly dispersed in the polymer matrix.     

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.     

High-performance composites based on all-aromatic liquid crystal thermosets

In this study, a new high-performance liquid crystal ester-based thermoset for composite applications was investigated. All-aromatic liquid crystalline thermosets (LCTs) are a promising class of polymers that offer a unique combination of properties such as solvent resistivity, high modulus, high strength, low coefficient of thermal expansion and high after cure glass-transition temperatures (T_g ? 150 °C). Fully cured LCTs offer superior thermo-mechanical properties over high-performance thermoplastic polymers such as PPS, PEEK and PEI. For this study we used a 9000 g mol⁻¹ ester-based LCT based on cheap and readily available monomers, i.e. 4-hydroxybenzoic acid (H), isophthalic acid (I) and hydroquinone (Q), abbreviated by us as HIQ-9. Composite panels prepared from T300 carbon fiber (5-harness satin weave) showed in-plane shear strength of 154 MPa and an in-plane shear modulus of 3.7 GPa. The tensile strength and modulus were measured to be 696 MPa and 57 GPa, respectively. A post-mortem inspection showed that the interfacial strength was excellent and no delamination was observed in the test specimen. Preliminary results show that LCT-based composites exhibit a better combination of (thermo) mechanical properties over PPS and PEI-based composites.     

Effects of particle size and distribution on the mechanical properties of SiC reinforced Al-Cu alloy composites

This paper studied the combined effects of particle size and distribution on the mechanical properties of the SiC particle reinforced Al-Cu alloy composites. It has been shown that small ratio between matrix/reinforcement particle sizes resulted in more uniform distribution of the SiC particles in the matrix. The SiC particles distributed more uniformly in the matrix with increasing in mixing time. It has also been shown that homogenous distribution of the SiC particles resulted in higher yield strength, ultimate tensile strength and elongation. Yield strength and ultimate tensile strength of the composite reinforced by 4.7 μm sized SiC particles are higher than those of composite reinforced by 77 μm sized SiC particles, while the elongation shows opposite trend with yield strength and ultimate tensile strength. Fracture surface observations showed that the dominant fracture mechanism of the composites with small SiC particle size (4.7 μm) is ductile fracture of the matrix, accompanied by the “pull-out” of the particles from the matrix, while the dominant fracture mechanism of the composites with large SiC particle size (77 μm) is ductile fracture of the matrix, accompanied by the SiC particle fracture.     

Structure and properties of highly oriented polyoxymethylene/multi-walled carbon nanotube composites produced by hot stretching

Highly-oriented polyoxymethylene (POM)/multi-walled carbon nanotube (MWCNT) composites were fabricated through solid hot stretching technology. With the draw ratio as high as 900%, the oriented composites exhibited much improved thermal conductivity and mechanical properties along the stretching direction compared with that of the isotropic samples before drawing. The thermal conductivity of the composite with 11.6 vol.% MWCNTs can reach as high as 1.2 W/m K after drawing. Microstructure observation demonstrated that the POM matrix had an ordered fibrillar bundle structure and MWCNTs in the composite tended to align parallel to the stretching direction. Wide-angle X-ray diffraction results showed that the crystal axis of the POM matrix was preferentially oriented perpendicular to the draw direction, while MWCNTs were preferentially oriented parallel to the draw direction. The strong interaction between the POM matrix and the MWCNTs hindered the orientation movement of molecules of POM, but induced the orientation movement of MWCNTs.     

Comparison of the thermal properties between composites reinforced by raw and amino-functionalized carbon materials

Carbon materials, such as graphite oxides, carbon nanotubes and graphenes, have exceptional thermal conductivity, which render them excellent candidates as fillers in advanced thermal interface materials for high density electronics. In this paper, these carbon materials were functionalized with 4,4′-diaminodiphenyl sulphone (DDS), to enhance the bonding between the carbon materials and the resin matrix. Their visibly different properties were investigated. It seems that DDS-functionalization can obviously improve the interfacial heat transfer between the carbon materials and the epoxy matrix. The thermal conductivity enhancement of D-Graphene composites (0.493 W/m K) was about 30% higher than that of D-MWNTs composites (0.387 W/m K) at 0.5 vol.% loading. The different effects among EGO, D-EGO, MWNTs, D-MWNTs and D-Graphene in polymer composites were also discussed. It was demonstrated that DDS-functionalized carbon materials had an obvious effect on the thermal performances of composite materials and were more effective in thermal conductivity enhancement.     

Localized mechanical property assessment of SiC/SiC composite materials

SiC fiber-reinforced SiC matrix composites (SiC/SiC) are under consideration as a structural material for a range of nuclear applications. While these materials have been studied for decades, recently new small scale materials testing techniques have emerged which can be used to characterize SiC/SiC materials from a new perspective. In this work cross section nanoindentation was performed on SiC/SiC composites revealing that both the hardness and Young’s modulus was substantially lower in the fiber compared to the matrix despite both being SiC. Using scanning electron microscopy it was observed that the grain growth of the matrix during formation was radially out from the fiber with a changing grain structure as a function of radius from the fiber center. Focused ion beam machining was used to manufacture micro-cantilever samples and evaluate the fracture toughness and fracture strength in the matrix as a function of grain orientation in the matrix. Additionally microstructural characterization techniques like Raman spectroscopy, X-ray diffraction, and microtomography were used to evaluate differences in the matrix and fibers of the composite.     

The effect on the tensile properties of PIP-processed SiC/SiC composite of a chemical vapor-infiltrated SiC layer overlaid on the pyrocarbon interface layer

A chemical vapor-infiltrated (CVI) SiC layer is often deposited on the pyrocarbon (PyC) fiber–matrix interface layer in SiC fiber-reinforced SiC matrix (SiC/SiC) composites. It is normally applied to protect the PyC layer from reacting with molten Si or sintering aids during manufacturing, and to guard against the effects of high temperature, oxidation and moisture during use. In this study, we investigated the effect of this SiC layer on the tensile properties of a composite. Tensile tests of our composite samples showed the SiC layer to have no noticeable effects on its ultimate load or fracture strain, whereas it decreased the load-to-strain ratio and proportional limit. The test results were analyzed by carrying out element tests on filaments and fiber bundle samples, fracture mirror analysis of pullout fibers, and finite element analysis (FEA) of residual thermal stress around the interface.     

Poly(vinyl alcohol) reinforced with large-diameter carbon nanotubes via spray winding

For practical application of carbon nanotube (CNT)/polymer composites, it is critical to produce the composites at high speed and large scale. In this study, multi-walled carbon nanotubes (MWNTs) with large diameter (∼45 nm) and polyvinyl alcohol (PVA) were used to increase the processing speed of a recently developed spraying winding technique. The effect of the different winding speed and sprayed solution concentration to the performance of the composite films were investigated. The CNT/PVA composites exhibit tensile strength of up to 1 GPa, and modulus of up to 70 GPa, with a CNT weight fraction of 53%. In addition, an electrical conductivity of 747 S/cm was obtained for the CNT/PVA composites. The good mechanical and electrical properties are attributed to the uniform CNTs and PVA matrix integration and the high degree of tube alignment.     

Correlation of elastic properties of melt infiltrated SiC/SiC composites to in situ properties of constituent phases

The ability to correlate the elastic properties of melt infiltrated SiC/SiC composites to properties of constituent phases using a hybrid Finite Element approach is examined and the influence of material internal features, such as the fabric architecture and intra-tow voids, on such correlation is elucidated. Tensile testing was carried out in air at room temperature and 1204 °C. Through-thickness compressive elastic modulus utilizing the stacked disk method was measured at room temperature. In situ moduli of constituent materials were experimentally evaluated using nano-indentation techniques at room temperature. A consistent relationship is observed between constituent properties and composite properties for in-plane normal and shear moduli and Poisson’s ratio at room temperature. However, experimental data for through-thickness compressive elastic modulus is lower than the calculated value. It is hypothesized that the existence of voids inside the fiber tows and their collapse under compressive loads is the cause of such discrepancy. Estimates for the change in elastic moduli of constituent phases with temperature were obtained from literature and used to calculate the elastic properties of the composites at 1204 °C. A reasonable correlation between the in-plane elastic moduli of the composite and the in situ elastic properties of constituent phases is observed.     

Tensile properties and damage behaviors of Csf/Mg composite at elevated temperature and containing a small fraction of liquid

The mechanical properties of magnesium matrix composites reinforced by pyrolytic carbon coated short carbon fiber at temperatures close to and above the solidus temperature were investigated by tensile tests for the first time. Microstructural observations and fractographic analysis were carried out in order to reveal the damage mechanisms of the composites with different fraction of liquid. Tensile strength of the composites decreased monotonously with temperature, an exponential equation relating the tensile strength to temperature and liquid fraction was derived. The elongation increases monotonously with temperatures from 400 °C to 428 °C (solidus temperature), and then decreases gradually with increasing fraction of liquid except a trough at 432 °C. The composites almost have no ductility and cannot sustain tensile stress when the fraction of liquid reaches 8%. The amount and distribution of liquid phase in the composites directly determines their mechanical properties and damage behavior.