Mechanical and dielectric properties of SiCf/SiC composites fabricated by PIP combined with CIP process

2D KD-1 SiC fiber fabrics were employed to fabricate SiC_f/SiC composites by an improved polymer infiltration and pyrolysis (PIP) process, combined with cold isostatic pressing (CIP). The effect of CIP process on the microstructure, mechanical and dielectric properties of SiC_f/SiC composites was investigated. The infiltration efficiency was remarkably improved with the introduction of CIP process. Compared to vacuum infiltration, the CIP process can effectively increase the infiltrated precursor content and decrease the porosity resulting in a dense matrix. Thus SiC_f/SiC composites with high density of 2.11 g cm⁻³ and low porosity of 11.3% were obtained at 100 MPa CIP pressure, together with an increase of the flexural strength of the composites from 89 MPa to 213 MPa. Real part (ε′) and the imaginary part (ε″) of complex permittivity of SiC_f/SiC composites increase and vary from 11.7-i9.7 to 15.0-i12.8 when the CIP pressure reaches 100 MPa.     

Fatigue of a SiC/SiC ceramic composite with an ytterbium-disilicate environmental barrier coating at elevated temperature*

Tension-tension fatigue performance of a SiC/SiC composite with an ytterbium-disilicate environmental barrier coating (EBC) was investigated at 1200°C in air and steam. The composite is reinforced with Hi-Nicalon™ SiC fibers and has a melt-infiltrated matrix processed by chemical vapor infiltration of SiC with subsequent infiltration with SiC particulate slurry and molten silicon. The EBC consists of a Si bond coat and an Yb₂Si₂O₇ top coat applied via air plasma spraying. Tensile properties were evaluated at 1200°C. Tension-tension fatigue was examined for maximum stresses of 110-140 MPa. To assess the efficacy of EBC, experimental results obtained for the coated composite are compared to those for a control uncoated composite. Surface grit-blasting inherent in the EBC application process degrades tensile strength of the composite. However, the EBC effectively protects the composite from oxidation embrittlement during cyclic loading in air or steam. Fatigue runout set to 200 000 cycles (55.6 hours at a frequency of 1.0 Hz) was achieved at 110 MPa in air and steam. Retained properties of pre-fatigued specimens were characterized. Composite microstructure, along with damage and failure mechanisms were investigated. Damage and failure of the composite are attributed to the growth of cracks originating from numerous processing defects in the composite interior.     

Evaluation of mechanical properties of a dense SiC/SiCN composite produced via PIP process

The material behavior of Polymer Infiltration and Pyrolysis based SiC/SiCN composites is studied and the characteristic thermal and mechanical properties in on- (0/90 °) and off-axis (±45 °) direction are summarized. The tensile properties are determined at room temperature and 1300 °C. Based on the ratio of Young’s modulus and strength between on- and off-axis loading, a new approach for the classification of Weak Matrix Composites (WMC) and Weak Interface Composites (WIC) is proposed, which seems to be reasonable for various CMCs. Even without fibre coating mechanical behavior of SiC/SiCN is similar to that of WIC. In order to explain this, a microstructure model is developed and confirmed by analysis of fracture surface. The effect of temperature on the tensile properties is investigated through analysis of residual thermal stresses. Even though at 1300 °C the strength is slightly lower, the fracture strain increased significantly from RT to 1300 °C.     

Theoretical prediction on structure evolution and optimal properties of silicon modified hexagonal boron nitride as interphase in SiCf/SiC composite

To predict the effects of Si doping on hexagonal boron nitride (h-BN) and to achieve a balance between mechanical and oxidation properties for the interphase modification in SiC_f/SiC composites, we herein calculate and analyze the crystal structures and mechanical properties of (BN)₆₄Si_x (x = 4, 8, 16, 32) models by means of density functional theory (DFT) calculations and ab initio molecular dynamics (aiMD) simulations. The possible trends of crack deflection and self-healing ability are discussed. The modeling shows an obvious transition of (BN)₆₄Si_x from the layered crystal structure and anisotropic mechanical property to amorphous structure and isotropic mechanical property as the Si doping content up to 36.1 wt%. Regarding to the application of interphase in SiC_f/SiC composites, (BN)₆₄Si₁₆ model structure possess the highest debonding potential according to Cook and Gordon’s criteria and illustrates the higher self-healing capacity at elevated temperature.     

Effects of CVI SiC amount and deposition rates on properties of SiCf/SiC composites fabricated by hybrid chemical vapor infiltration (CVI) and precursor infiltration and pyrolysis (PIP) routes

The SiC_f/SiC composites have been manufactured by a hybrid route combining chemical vapor infiltration (CVI) and precursor infiltration and pyrolysis (PIP) techniques. A relatively low deposition rate of CVI SiC matrix is favored ascribing to that its rapid deposition tends to cause a ‘surface sealing’ effect, which generates plenty of closed pores and severely damages the microstructural homogeneity of final composites. For a given fiber preform, there exists an optimized value of CVI SiC matrix to be introduced, at which the flexural strength of resultant composites reaches a peak value, which is almost twice of that for composites manufactured from the single PIP or CVI route. Further, this optimized CVI SiC amount is unveiled to be determined by a critical thickness t₀, which relates to the average fiber distance in fiber preforms. While the deposited SiC thickness on fibers exceeds t₀, closed pores will be generated, hence damaging the microstructural homogeneity of final composites. By applying an optimized CVI SiC deposition rate and amount, the prepared SiC_f/SiC composites exhibit increased densities, reduced porosity, superior mechanical properties, increased microstructural homogeneity and thus reduced mechanical property deviations, suggesting a hybrid CVI and PIP route is a promising technique to manufacture SiC_f/SiC composites for industrial applications.     

In situ growth of one-dimensional carbon-rich SiC nanowires in porous Sc2Si2O7 ceramics with excellent microwave absorption properties

For enhancing the absorption ability of dielectric and electromagnetic wave (EMW), C-rich SiC NWs /Sc₂Si₂O₇ ceramics are successfully fabricated through in-situ growth of SiC nanowires (NWs) into porous Sc₂Si₂O₇ ceramics by precursor infiltration and pyrolysis (PIP) at 1400?°C in Ar. SiC NWs are in-situ formed in the pore channels via a vapor-liquid-solid (VLS) mechanism, the relative complex permittivity increases notably with the content of absorber (C-rich SiC NWs), which tune the microstructure and dielectric property of C-rich SiC NWs/Sc₂Si₂O₇ ceramics. Meanwhile, the minimum reflection coefficient (RC) of C-rich SiC NWs/Sc₂Si₂O₇ ceramic decreases from ?9.5?dB to ??35.5?dB at 11?GHz with a thickness of 2.75?mm, and the effective absorption bandwidth (EAB) covers the whole X band (8.2–12.4?GHz) when the content of absorber is 24.5?wt%. The results indicate that Sc₂Si₂O₇ ceramics decorated with SiC NWs and nanosized carbon have a superior microwave-absorbing ability, which can be contributed to the Debye relaxation, interfacial polarization and conductivity loss enhanced by in-situ formed SiC NWs and nanosized carbon phases. The C-rich SiC NWs /Sc₂Si₂O₇ ceramics can be a promising microwave absorbing materials within a broad bandwidth.     

On the mechanical,thermophysical and dielectric properties of Nextel™ 440 fiber reinforced nitride matrix (N440/Nitride) composites

The Nextel? 440 fiber reinforced nitride matrix (N440/Nitride) composites were fabricated by precursor infiltration and pyrolysis (PIP) route. The results demonstrated that the original N440 fiber had a phase composition of amorphous SiO₂ and γ-Al₂O₃. Its single filament tensile strength was 3.03 GPa (at room temperature), while it dropped to 72.6% and 35.1% at 1200 °C and 1400 °C, respectively. The phase content of N440/Ntride composites was mainly γ-Al₂O₃ and amorphous BN, as well as mullite phase (formed at > 1100 °C). The composites owned a flexural strength up to 76.0 MPa at room temperature. The stair-stepping decrease in the load-displacement curve and fiber pull-outs in the fracture surface indicated a good fiber/matrix interface and toughness. By heating at 1400 °C, the composites still possessed 67.4% of original bending strength. It was found that the high temperatures caused strong fiber-matrix bonding and severe fiber degradation. The specific heat, CTE and thermal conductivity of the composites were 0.325–0.586 J g^?1 K^?1, (3.2–4.0) × 10^?6 K^?1 and 0.78–3.47 W m^?1 K^?1, respectively. The composites possessed a dielectric constant of 4.25–4.35 and loss tangent of 0.004–0.01 at 8–12 GHz. The good overall performances enabled the N440/Nitride composites advanced high-temperature wave-transparent applications.     

Investigations on continuous-wave laser and pulsed laser induced controllable ablation of SiCf/SiC composites

To lay a foundation for the feasibility exploration of laser-induced ablation-assisted machining for SiC_f/SiC composites, combined with numerical simulation and experiments, the laser-induced ablation mechanism of SiC_f/SiC composites was studied, and the relationship between laser parameters and ablation depth was analyzed. The laser-induced ablation products of SiC_f/SiC composites mainly consisted of recrystallized 3C-SiC and amorphous SiO₂, which were powdery and porous. According to the stratification characteristic, the ablation products were divided into attached smoke dust layer, sublimate recrystallization layer, heat-affected layer, and unaffected layer from the surface to the inside of the material. By adjusting the laser parameters (significant factors were the scanning speed and the scanning spacing), the depth of laser-induced ablation was adjustable and controllable. The ablation depth was greater in continuous-wave (CW) mode due to the continuous energy input. Therefore, CW laser is more suitable for generating larger and various ablation depths to match various cutting allowances.     

Dielectric properties of polymer-derived ceramic reinforced with boron nitride nanotubes

The electrical and dielectric properties of boron nitride nanotubes (BNNTs) reinforced ceramic composites using the polymer-derived ceramic (PDC) processing route were investigated in this work. The electrical resistivity of the pristine PDC increases from 10⁶ to 10⁸ Ω m after the addition of BNNTs. When the BNNT loading was increased to 5 wt%, the average real relative permittivity of the PDC decreased from 2.94 to 2.80, while the quality factor (Q) of the PDC increased from 134.40 to 176.77. The BNNTs can increase the Q factor of the PDC due to the reduction in the porosity cause by the introduction of the BNNTs. Further increasing the BNNT content decreases the real relative permittivity of the nanocomposites and increases the Q factor at high frequency. The average real relative permittivity decreases to 2.29, while the average Q factor increases to 208.60 when the BNNT content is increased to 30 wt%. The dielectric loss after the addition of high fraction of BNNTs can be explained by the Lorentz resonance relaxation process. Results of this work showed that PDC-BNNT nanocomposites are satisfactory electromagnetic transparent materials when the BNNT fraction is less than 10 wt%.     

In-situ tensile damage and fracture behavior of PIP SiC/SiC minicomposites at room temperature

In-situ tensile damage and fracture behavior of original SiC fiber bundles, processed and uncoated SiC fiber bundles, SiC fiber bundle with PyC interphase, SiC/SiC minicomposites without/with PyC interphase are analyzed. Relationships between load-displacement curves, stress-strain curves, and micro damage mechanisms are established. A micromechanical approach is developed to predict the stress-strain curves of SiC/SiC minicomposites for different damage stages. Experimental tensile stress-strain curves of two different SiC fiber reinforced SiC matrix without/with interphase are predicted. Evolution of composite’s tangent modulus, interface debonding fraction, and broken fiber fraction with increasing applied stress is analyzed. For the BX™ and Cansas-3303™ SiC/SiC minicomposite with interphase, the composite’s tangent modulus decreased with applied stress especially approaching tensile fracture; the interface debonding fraction increased with applied stress, and the composite’s tensile fracture occurred with partial interface debonding; and the broken fiber fraction increased with applied stress, and most of fiber’s failure occurred approaching final tensile fracture.     

Effect of SNNWS content on the microstructure and properties of SNNWS/Si-C-N ceramic composites via PIP

Si-C-N ceramic composites containing well distributed silicon nitride nanowires (SNNWs) were fabricated by die-pressing and precursor infiltration and pyrolysis process at a low temperature. The structure, composition, mechanical and thermophysical properties of the composites were investigated. The results show that the composites consisted of amorphous SiCN, α-Si₃N₄ and α-cristobaslite. The composites with different contents of SNNWs possessed a density of 2.02–2.07 g cm^?3 and open porosity of 7.9–9.9%. SNNWs can effectively restrain the contraction of matrix with a decrease by 25% in linear shrinkage. The composites with 3 wt% SNNWs owned the highest flexural strength (83.7 MPa) and elastic modulus (54.0 GPa) at room temperature, which increase by 13.2% and 62.3% respectively, compared with pure SiCN ceramics. The SNNWs displayed good reinforcement function at high temperature due to the fact that the composites with 7 wt% SNNWs had a 96.8% retention rate of bending strength at 1200 °C. The composites had relatively low coefficient of thermal expansion and thermal diffusivity which were less than 2.2 × 10^?6 K^?1 and 0.62 mm² s^?1, respectively.     

Effect of in situ grown SiC nanowires on microstructure and mechanical properties of C/SiC composites

Hexagonal-shaped SiC nanowires were in situ formed in C/SiC composites with ferrocene as catalyst in the densification process of polymer impregnation and pyrolysis. The effect of SiC nanowires on microstructure and properties of the composites were studied. The results show that the in situ formed SiC nanowires were hexagonal, mostly with diamer of about 250 nm, and grew by the vapor–liquid–solid (VLS) mechanism. The C/SiC composite with nanowires shows higher bulk density and flexural strength than the one with no SiC nanowires, and the high temperature flexural strength behavior of C/SiC composites with SiC nanowires was evaluated.     

Effects of heat treatment on the mechanical properties at elevated temperatures of plain-woven SiC/SiC composites

The effects of heat treatment on the mechanical properties of plain-woven SiC/SiC composites at 927 °C and 1200 °C in argon were evaluated through tensile tests at room temperature and at elevated temperature on the as-received and heat-treated plain-woven SiC/SiC composites, respectively. Heat treatment can improve the mechanical properties of composites at room temperature due to the release of thermal residual stress. Although heat treatment can damage the fiber, the effect of this damage on the mechanical properties of composites is generally less than the effect of thermal residual stress. Heat treatment will graphitize the pyrolytic carbon interface and reduce its shear strength. Testing temperature will affect the expansion or contraction of the components in the composites, thereby changing the stress state of the components. This study can provide guidance for the optimization of processing of ceramic matrix composites and the structural design in high-temperature environments.     

Preparation and tensile behavior of SiCf/SiC mini composites containing different types and thicknesses of interphase

SiC fiber-reinforced SiC matrix (SiC_f/SiC) composites are promising materials for high-temperature structural applications. In this study, KD-II SiC fiber bundles with a C/Si ratio of approximately 1.25 and an oxygen amount of 2.53%, were used as reinforcement. PyC interphase, PyC-SiC co-deposition interphase I and II, with different thicknesses, and SiC matrix were deposited into the SiC fiber bundles by using chemical vapor infiltration (CVI) to form SiC_f/SiC mini composites. When the thickness of the interphase is approximately 1000 nm, the ultimate tensile stress and strain of SiC_f/SiC mini composites with PyC-SiC co-deposition interphase I can reach 1120.0 MPa and 0.72%, respectively, which are significantly higher than those of SiC_f/SiC mini composites with a PyC interphase (740.0 MPa, 0.87%) and PyC-SiC co-deposition interphase II (645.0 MPa, 0.54%). The effect of thicknesses and types of interphase on tensile fracture behavior of mini composites and then the fracture mechanism are discussed in detail.     

纳米SiO2对先驱体浸渍裂解法制备SiCf/SiC复合材料力学性能的影响

以纳米SiO2为填料,采用先驱体浸渍裂解法制备2.5D-SiCf/SiC（D为维数,SiCf为SiC纤维）复合材料,研究了前驱液中纳米SiO2含量对复合材料力学性能的影响。结果表明,纳米SiO2的添加能有效抑制先驱体裂解过程中的体积收缩,提高致密度,但过量引入易导致浸渍液黏度过高,浸渍效率降低。纳米SiO2含量对材料力学性能有较大影响,添加纳米SiO2后材料的抗弯强度和断裂韧性均高于没有添加的样品,材料抗弯强度随纳米SiO2含量的增加先增大后降低。当浸渍液中纳米SiO2含量为6%时,复合材料具有优异的力学性能,抗弯强度达到211.1MPa。     

Pressureless fabrication of dense monolithic SiC ceramics from a polycarbosilane

This paper presents the pressureless preparation of dense and crack-free near stoichiometric SiC monoliths via cross-linking and pyrolysis of a polycarbosilane, followed by polymer-infiltration-pyrolysis cycles. The composition and the porosity of the samples strongly depend on the processing temperature. Thus, at 1050–1100 °C, the SiC monoliths are X-ray amorphous and exhibit low amounts of oxygen and excess carbon; their porosity was rather high (>10%). Higher processing temperatures induced the crystallization of β-SiC. The removal of oxygen and excess carbon due to CO release allowed for obtaining near-stoichiometric compositions at 1700 °C. However, the residual porosity of the samples increased. The use of the PIP technique led already after six cycles to dense monoliths (residual porosity ca. 0.5%).The present study emphasizes the potential of the polymer processing technique for the fabrication of near stoichiometric and dense SiC monoliths, which might be used for structural applications in harsh conditions.     

Tensile behavior of 2D-C/SiC composites at elevated temperatures: Experiment and modeling

In this paper, on-axis tensile behavior of a coated 2D-C/SiC composite at elevated temperatures was studied experimentally and theoretically. The measured data reveals that the tensile modulus and strength increase continuously with increasing temperature till 1273 K. Contrarily, the failure strains decrease sharply at high temperatures than the counterpart at room temperature, manifesting the significant influence of thermal residual stresses (TRS) on mechanical behavior of C/SiC composites. Simulation of stress-strain response is based on a two-scale analytical model, in which the plain-weave element is idealized as a cross-ply laminate and its macroscopic mechanical parameters are evaluated by shear-lag approach. The primary calculation was concentrated on TRS of the composite. And, a new crack evolution model was introduced to describe the stochastic cracking process. The total strain response including residual strain and elastic strain from the loading-unloading-reloading conception was finally formulated through micromechanical analysis involving the influence of TRS on matrix cracking and interface debonding. Additionally, a strength model was developed for plain-weave structures by using shear-lag theory, statistical theory and rule of mixture. Both of the proposed constitutive and strength models can give accurate predictions for 2D-C/SiC composites at elevated temperatures.     

Reaction kinetics and ablation properties of C/C-ZrC composites fabricated by reactive melt infiltration

Carbon/carbon-zirconium carbide (C/C-ZrC) composites were prepared by reactive melt infiltration. Carbon fiber felt was firstly densified by carbon using chemical vapor infiltration to obtain a porous carbon/carbon (C/C) skeleton. The zirconium melt was then infiltrated into the porous C/C at temperatures higher than the melting point of zirconium to obtain C/C-ZrC composites. The infiltration depth as a function of annealing temperature and dwelling time was studied. A model based on these results was built up to describe the kinetic process. The ablation properties of the C/C-ZrC were tested under an oxyacetylene torch and a laser beam. The results indicate that the linear and mass ablation rates of the C/C-ZrC composites are greatly reduced compared with C/SiC-ZrB₂, C/SiC, and C/C composites. The formation of a dense layer of ZrC and ZrO₂ mixture at high temperatures is the reason for high ablation resistance.     

Advances in modifications and high-temperature applications of silicon carbide ceramic matrix composites in aerospace: A focused review

This article is a detailed review of the measures to modify the high-temperature mechanical properties of silicon carbide ceramic matrix composites (SiC CMCs), namely toughness, high-temperature stability and wear resistance. Additionally, it briefly describes the common processing methods of the SiC CMCs and their application in the high-temperature field of aerospace. The advantages and disadvantages of various existing processing and molding methods for the SiC CMCs are also discussed. The high-temperature mechanical properties of the SiC CMCs are mainly affected by the properties of the matrix, added phase and interface. It is crucial to reduce the crystal defects of the matrix and select a suitable enhancement phase for an elevated performance. Moreover, it is important to improve the bonding at the interface between the enhancement phase and the matrix. This review is expected to provide useful information for the subsequent development of complex SiC CMCs for high-temperature applications.