High-temperature flexural strength of I-CVI processed Cf/SiC composites with variable interphases

The effect of single-layer pyrocarbon (PyC) and multilayered (PyC/SiC)_n=4 interphases on the flexural strength of un-coated and SiC seal-coated stitched 2D carbon fiber reinforced silicon carbide (C_f/SiC) composites was investigated. The composites were prepared by I-CVI process. Flexural strength of the composites was measured at 1200 °C in air atmosphere. It was observed that irrespective of the type of interphase, the seal coated samples showed a higher value of flexural strength as compared to the uncoated samples. The flexural strength of 470 ± 12 MPa was observed for the seal coated C_f/SiC composite samples with multilayered interphase. The seal coated samples with single layer PyC interphase showed flexural strength of 370 ± 20 MPa. The fractured surfaces of tested samples were analyzed in detail to study the fracture phenomena. Based on microstructure-property relations, a mechanism has been proposed for the increase of flexural properties of C_f/SiC composites having multilayered interphase.     

Oxidation behavior of 3D SiCf/SiBCN composites at 800–1200 °C

3D SiC_f/BN–SiC/SiBCN composites were fabricated via precursor impregnation and polymer infiltration pyrolysis (PIP). Oxidation behavior of the composites heated in air at 800 °C, 1000 °C and 1200 °C for 50 h was investigated. Following the oxidation treatment, it was found that the bending strength of the composites at different oxidation temperatures was degraded. The weight loss of the composites decreased gradually over the range of oxidation times of 1–50 h. In order to clarify the oxidation mechanism of the composites, reconstructed images, microstructures, phase compositions, the oxide layer formed on the composites and main chemical reactions were all analyzed. It was revealed that the degradation in the fracture strength of the composites was closely related to the oxidation of SiBCN matrix and BN-SiC interphase, whereas there was no signs of oxidation products about SiC fiber, which indicated that SiC fiber could be protected from oxygen by SiBCN matrix at 800?1200 °C in air.     

Properties and microstructure evolution of Cf/SiC composites fabricated by polymer impregnation and pyrolysis (PIP) with liquid polycarbosilane

In the present study, a novel liquid polycarbosilane (LPCS) with a ceramic yield as high as 83% was applied to develop 3D needle-punched C_f/SiC composites via polymer impregnation and pyrolysis process (PIP). The cross-link and ceramization processes of LPCS were studied in detail by FT-IR and TG-DSC; a compact ceramic was obtained when LPCS was firstly cured at 120 °C before pyrolysis. It was found that the LPCS-C_f/SiC composites possessed a higher density (2.13 g/cm³) than that of the PCS-C_f/SiC composites even though the PIP cycle for densification was obviously reduced, which means a higher densification efficiency. Logically, the LPCS-C_f/SiC composites exhibited superior mechanical properties. The shorter length and rougher surfaces of pulled-out fibers indicated the LPCS-C_f/SiC composites to possess a stronger bonding between matrix and PyC interphase compared with the PCS-C_f/SiC composites.     

Properties of Cf/SiC-ZrB2-TaxCy composite produced by reactive hot pressing and polymer impregnation pyrolysis (RHP/PIP)

C_f/SiC-ZrB₂-Ta_xC_y composite was synthesized by reactive hot pressing (RHP) of C_f cloth, polycarbosilane (PCS), ZrB₂, and Ta powders at 4 MPa and 1200 °C. PIP cycle influenced sintering process by increasing density of the composite from 2.34 to 2.82 g/cc. Residual carbon produced during the PIP cycles at 1200 °C was utilized to yield Ta_xC_y by the addition of Ta. SEM images illustrate that by increasing the number of PIP cycles, SiC derived from the PCS cover the C_f fibre, micropores, and cracks. PIP cycles and Ta_xC_y phase improved flexural strength of the composite from 20 to 114 MPa. Mass and linear ablation resistance studies at 1600–2000 °C exhibited that oxide formation at the outer surface caused a barrier; further, no oxidation underneath the composite was observed. SEM images display that at 2000 °C, SiO₂ and Ta_xO_y were molten and sealed the pores. Hence, ablation resistance was enhanced by blocking the penetration in high-temperature flame.     

The mechanical,thermophysical and electromagnetic properties of UD SiCf/SiC composites in different directions

Unidirectional (UD) silicon carbide (SiC) fiber-reinforced SiC matrix (UD SiC_f/SiC) composites with CVI BN interphase were fabricated by polymer infiltration-pyrolysis (PIP) process. The effects of the anisotropic distribution of SiC fibers on the mechanical properties, thermophysical properties and electromagnetic properties of UD SiC_f/SiC composites in different directions were studied. In the direction parallel to the axial direction of SiC fibers, SiC fibers bear the load and BN interphase ensures the interface debonding, so the flexural strength and the fracture toughness of the UD SiC_f/SiC composites are 813.0 ± 32.4 MPa and 26.1 ± 2.9 MPa·m^1/2, respectively. In the direction perpendicular to the axial direction of SiC fibers, SiC fibers cannot bear the load and the low interfacial bonding strengths between SiC fiber/BN interphase (F/I) and BN interphase/SiC matrix (I/M) both decrease the matrix cracking stress, so the corresponding values are 36.6 ± 6.9 MPa and 0.9 ± 0.5 MPa?m^1/2, respectively. The thermal expansion behaviors of UD SiC_f/SiC composites are similar to those of SiC fibers in the direction parallel to the axial direction of SiC fibers, and are similiar to those of SiC matrix in the direction perpendicular to the axial direction of SiC fibers. The total electromagnetic shielding effectiveness (EM SE_T) of UD SiC_f/SiC composites attains 32 dB and 29 dB when the axial direction of SiC fibers is perpendicular and parallel to the electric field direction, respectively. The difference of conductivity in different directions is the main reason causing the different SE_T. And the dominant electromagnetic interference (EMI) shielding mechanism is absorption for both studied directions.     

Effect of intermediate heat treatment on mechanical properties of SiCf/SiC composites with BN interphase prepared by ICVI

SiC_f/SiC composites with BN interface were prepared through isothermal-isobaric chemical vapour infiltration process. Room temperature mechanical properties such as tensile, flexural, inter-laminar shear strength and fracture toughness (K_IC) were studied for the composites. The tensile strength of the SiC_f/SiC composites with stabilised BN interface was almost 3.5 times higher than that of SiC_f/SiC composites with un-stabilised BN interphase. The fracture toughness is similarly enhanced to 23 MPa m^1/2 by stabilisation treatment. Fibre push-through test results showed that the interfacial bond strength between fibre and matrix for the composite with un-stabilised BN interface was too strong (>48 MPa) and it has been modified to a weaker bond (10 MPa) due to intermediate heat treatment. In the case of composite in which BN interface was subjected to thermal treatment soon after the interface coating, the interfacial bond strength between fibre and matrix was relatively stronger (29 MPa) and facilitated limited fibre pull-out.     

Effect of SiC interphase on the mechanical,high-temperature dielectric and high-temperature microwave absorption properties of the SiCf/SiC/Mu composites

In this study, SiC interphase was prepared via a precursor infiltration-pyrolysis process, and effects of dipping concentrations on the mechanical, high-temperature dielectric and microwave absorption properties of the SiC_f/SiC/Mu composites had been investigated. Results indicated that different dipping concentrations influenced ultimate interfacial morphology. The SiC interphase prepared with 5 wt% PCS/xylene solution was smooth and homogeneous, and no bridging between the fiber monofilament could be observed. At the same time, SiC interphase prepared with 5 wt% PCS/xylene solution had significantly improved mechanical properties of the composite. In particular, the flexural strength of the composite prepared with 5 wt% PCS/xylene solution reached 281 MPa. Both ε′ and ε′′ of the SiC_f/SiC/Mu composites were enhanced after preparing SiC interphase at room temperature. The SiC_f/SiC/Mu composite prepared with 5 wt% PCS/xylene solution showed the maximum dielectric loss value of 0.38 at 10 GHz. Under the dual action of polarization mechanism and conductance loss, both ε′ and ε′′ of the SiC_f/SiC/Mu composites enhanced as the temperature increased. At 700 °C, the corresponding bandwidth (RL ≤ ?5 dB) of SiC_f/SiC/Mu composites prepared with 5 wt% PCS/xylene solution can reach 3.3 GHz at 2.6 mm. The SiC_f/SiC/Mu composite with SiC interphase prepared with 5 wt% PCS/xylene solution is expected to be an excellent structural-functional material.     

Direct ink writing of chopped carbon fibers reinforced polymer-derived SiC composites with low shrinkage and high strength

The chopped carbon fiber reinforced SiC (C_f/SiC) composite has been regarded as one of the excellent high-temperature structural materials for applications in aerospace and military fields. This paper presented a novel printing strategy using direct ink writing (DIW) of chopped fibers reinforced polymer-derived ceramics (PDCs) with polymer infiltration and pyrolysis (PIP) process for the fabrication of C_f/SiC composites with high strength and low shrinkage. Five types of PDCs printing inks with different C_f contents were prepared, their rheological properties and alignment of carbon fiber in the printing filament were studied. The 3D scaffold structures and bending test samples of C_f/SiC composites were fabricated with different C_f contents. The results found that the C_f/SiC composite with 30 wt% C_f content has high bending strength (～ 7.09 MPa) and negligible linear shrinkage (～ 0.48%). After the PIP process, the defects on the C_f/SiC composite structures were sufficiently filled, and the bending strength of C_f/SiC composite can reach up to about 100 MPa, which was about 30 times greater than that of the pure SiC matrix without C_f. This work demonstrated that the printed C_f/SiC composites by using this method is beneficial to the development of the precision and complex high-temperature structural members.     

Effect of interphase on mechanical properties and microstructures of 3D Cf/SiBCN composites at elevated temperatures

Interphase between the fibers and matrix plays a key role on the properties of fiber reinforced composites. In this work, the effect of interphase on mechanical properties and microstructures of 3D C_f/SiBCN composites at elevated temperatures was investigated. When PyC interphase is used, flexural strength and elastic modulus of the C_f/SiBCN composites decrease seriously at 1600°C (92 ± 15 MPa, 12 ± 2 GPa), compared with the properties at room temperature (371 ± 31 MPa, 31 ± 2 GPa). While, the flexural strength and elastic modulus of C_f/SiBCN composites with PyC/SiC multilayered interphase at 1600°C are as high as 330 ± 7 MPa and 30 ± 2 GPa, respectively, which are 97% and 73% of the values at room temperature (341 ± 20 MPa, 41 ± 2 GPa). To clarify the effect mechanism of the interphase on mechanical properties of the C_f/SiBCN composites at elevated temperature, interfacial bonding strength (IFBS) and microstructures of the composites were investigated in detail. It reveals that the PyC/SiC multilayered interphase can retard the SiBCN matrix degradation at elevated temperature, leading to the high strength retention of the composites at 1600°C.     

Fine study of hierarchical interphase constructed by boron nitride and carbon nanotubes in SiCf/SiC composites

A fine study of the interfacial part in the silicon carbide fiber (SiC_f) reinforced silicon carbide (SiC) composites was conducted by transmission electron microscopy. The boron nitride (BN) and carbon nanotubes (CNTs) were progressively coated on the SiC_f by chemical vapor deposition method to form a hierarchical structure. Three composites with different interfaces, SiC_f–CNTs/SiC, SiC_f@BN/SiC, and SiC_f@BN–CNTs/SiC, were fabricated by polymer infiltration and pyrolysis method. The interfaces and microstructures of the three composites were carefully characterized to investigate the improvement mechanism of strength and toughness. The results showed that BN could protect the surface of SiC_f from corrosion and oxidation so that improved the possibility of debonding and pullout. CNTs could avoid the propagation of cracks in the composites so that improved the damage resistance of the matrix. The synergistic reinforcement brought by BN and CNTs interfaces made the SiC_f@BN–CNTs/SiC composites with a tensile fracture strength as high as 359 MPa, with an improvement of 23% compared to that of SiC_f@BN/SiC.     

Mechanical properties of SiCf/SiC composites with alternating PyC/BN multilayer interfaces

Alternating pyrolytic carbon/boron nitride (PyC/BN)_n multilayer coatings were applied to the KD–II silicon carbide (SiC) fibres by chemical vapour deposition technique to fabricate continuous SiC fibre-reinforced SiC matrix (SiC_f/SiC) composites with improved flexural strength and fracture toughness. Three-dimensional SiC_f/SiC composites with different interfaces were fabricated by polymer infiltration and pyrolysis process. The microstructure of the coating was characterised by scanning electron microscopy, X–photoelectron spectroscopy and transmission electron microscopy. The interfacial shear strength was determined by the single-fibre push-out test. Single-edge notched beam (SENB) test and three-point bending test were used to evaluate the influence of multilayer interfaces on the mechanical properties of SiC_f/SiC composites. The results indicated that the (PyC/BN)_n multilayer interface led to optimum flexural strength and fracture toughness of 566.0?MPa and 21.5?MPa?m^1/2, respectively, thus the fracture toughness of the composites was significantly improved.     

Mechanical and dielectric properties of SiCf/BN/SiBCN composites via different synthesis technologies

SiC fibers reinforced SiBCN ceramic matrix composites (SiC_f/BN/SiBCN composites) were synthesized by direct chemical vapor infiltration (CVI), polymer infiltration pyrolysis (PIP) or chemical vapor infiltration combined with polymer infiltration pyrolysis (CVI + PIP). It is shown that the insertion of a continuous and dense SiBCN matrix via the CVI process improves the flexural strength and modulus. Interface debonding and fiber pullout happened with 50–100 nm BN interface in CVI and CVI + PIP SiC_f/BN/SiBCN composites. The relative complex permittivity was measured in X-band. Higher ε′′ values in CVI-containing composites can be observed, which can be attributed to the accumulation of C and SiC phases and a multilayer matrix. Strong electromagnetic wave attenuation ability was obtained with high dielectric loss.     

Joining of SiCf/SiC using polycarbosilane and polysilazane preceramic mixtures

Polycarbosilane (PCS)/polysilazane (PSZ) preceramic mixtures with weight ratios of 100/0, 75/25, 50/50, 25/75, and 0/100 were used as a filler for the joining of SiC_f/SiC to obtain high purity SiC at the joining region. SiC_f/SiC was fabricated by the electrophoretic infiltration of a SiC-based matrix phase into Tyranno SA3 SiC fabrics followed by hot-pressing at 1750?°C under 20?MPa for 2?h in an Ar atmosphere. Microstructural analysis confirmed a sound join without cracks after joining at 1750?°C for 2?h under a pressure of 10?MPa. SiC was the only phase remaining at the joint when PCS was used, while a small amount of Si₃N₄ along with the main SiC were observed in the join using PSZ. The flexural strengths of the butt-joint SiC_f/SiC were 120 and 137?MPa for the samples joined using a pure PCS and PSZ at 1750?°C, respectively, whereas those joined using the mixture fillers showed relatively lower strength.     

Effects of heat treatment on mechanical properties of 3D Si3N4f/BN/Si3N4 composites by PIP

The fabrication of three-dimensional silicon nitride (Si₃N₄) fiber-reinforced silicon nitride matrix (3D Si₃N_4f/BN/Si₃N₄) composites with a boron nitride (BN) interphase through precursor infiltration and pyrolysis (PIP) process was reported. Heat treatment at 1000–1200 °C was used to analyze the thermal stability of the Si₃N_4f/BN/Si₃N₄ composites. It was found after heat treatment the flexural strength and fracture toughness change with a pattern that decrease first and then increase, which are 191 ± 13 MPa and 5.8 ± 0.5 MPa·m^1/2 respectively for as-fabricated composites, and reach the minimum values of 138 ± 6 MPa and 3.9 ± 0.4 MPa·m^1/2 respectively for composites annealed at 1100 °C. The influence mechanisms of the heat treatment on the Si₃N_4f/BN/Si₃N₄ composites include: (Ⅰ) matrix shrinkage by further ceramization that causes defects such as pores and cracks in composites, and (Ⅱ) prestress relaxation, thermal residual stress (TRS) redistribution and a better wetting at the fiber/matrix (F/M) surface that increase the interfacial bonding strength (IBS). Thus, heat treatment affects the mechanical properties of composites by changing the properties of the matrix and IBS, where the load transfer efficiency onto the fibers is fluctuating by the microstructural evolution of matrix and gradually increasing IBS.     

Effects of in-situ carbon layer and volume fraction of SiC fiber on the mechanical properties and fracture behaviors of SiCf/SiC composites fabricated by a modified PIP method

Unidirectional SiC_f/SiC composites (UD SiC_f/SiC composites) with excellent mechanical properties were successfully fabricated by a modified PIP method which involved the preparation of film-like matrix containing carbon layer with a low concentration PCS solution followed by the rapid densification of composites with a high concentration PCS solution. Carbon layers were in-situ formed and alternating with SiC layers in the as-received matrix. The unique microstructure endows the composites with appropriate interfacial bonding state, good load transfer ability of interphase and matrix and load bearing ability of fiber, and great crack deflection capacity, which ensures the synergy of high strength and toughness of composites. It is also found that the fiber volume fraction in the preform makes a non-negligible effect on the distribution of interphase and matrix, of which the reasonable adjustment can be utilized to optimize the mechanical properties of composites. Compared with the composites only using high concentration PCS solution, the UD SiC_f/SiC composites prepared by the modified PIP method exhibit superior mechanical properties. Ultrahigh flexural strength of 1318.5 ± 158.3 MPa and fracture toughness of 47.6 ± 5.6 MPa·m^1/2 were achieved at the fiber volume fraction of 30%.     

Microstructure and mechanical performance of SiCf/BN/SiC mini-composites oxidized at elevated temperature from ambient temperature to 1500 °C in air

SiC_f/BN/SiC mini-composites comprising single tow SiC fibre-reinforced SiC with chemical vapour deposited (CVD) BN interface layers were fabricated. The mechanical performance and binding strength of the composites and the fibre/interface for the oxidized SiC_f/BN/SiC mini-composite samples (oxidation at 1000, 1200, 1300, 1400 and 1500 °C in air for two hours) were investigated by tensile tests and fibre push-out tests, respectively. The value of oxidation mass change was also measured. Some unusual phenomena for the SiC_f/BN/SiC mini-composites oxidized at 1000 °C were discovered in this work. The tensile strength reached a maximum value, and the mass gain rate showed as a singular negative value, while the shear strength between the fibre and the matrix was moderate. Scanning electron microscopy, energy dispersive spectrometry, infrared spectroscopy and X-ray diffraction characterization methods were used to reveal the microstructural evolution and investigate the unusual phenomenon during oxidation procedures. This work will provide guidance for predicting the service life of SiC_f/BN/SiC composite materials and may enable these materials to become a backbone for thermal structure systems in aerospace applications.     

Mechanical,thermal, and dielectric properties of SiCf/SiC composites reinforced with electrospun SiC fibers by PIP

Electrospun unidirectional SiC fibers reinforced SiC_f/SiC composites (e-SiC_f/SiC) were prepared with ∼10% volume fraction by polymer infiltration and pyrolysis (PIP) process. Pyrolysis temperature was varied to investigate the changes in microstructures, mechanical, thermal, and dielectric properties of e-SiC_f/SiC composites. The composites prepared at 1100 °C exhibit the highest flexural strength of 286.0 ± 33.9 MPa, then reduced at 1300 °C, mainly due to the degradation of electrospun SiC fibers, increased porosity, and reaction-controlled interfacial bonding. The thermal conductivity of e-SiC_f/SiC prepared at 1300 °C reached 2.663 W/(m∙K). The dielectric properties of e-SiC_f/SiC composites were also investigated and the complex permittivities increase with raising pyrolysis temperature. The e-SiC_f/SiC composites prepared at 1300 °C exhibited EMI shielding effectiveness exceeding 24 dB over the whole X band. The electrospun SiC fibers reinforced SiC_f/SiC composites can serve as a potential material for structural components and EMI shielding applications in the future.     

Tensile creep behavior of SiCf/SiC ceramic matrix minicomposites

Single fiber-tow minicomposites represent the major load-bearing element of woven and laminate ceramic matrix composites (CMCs). To understand the effects of fiber type, fiber content, and matrix cracking on tensile creep in SiC_f/SiC CMCs, single-tow SiC_f/SiC minicomposites with different fiber types and contents were investigated. The minicomposites studied contained either Hi-Nicalon™ or Hi-Nicalon™ Type S SiC fibers with a boron nitride (BN) interphase and a chemical-vapor-infiltrated-silicon-carbide (CVI-SiC) matrix. Tensile creep was performed at 1200 °C in air. A bottom-up creep modeling approach was applied where creep parameters of the fibers and matrix were obtained separately at 1200 °C. Next, a theoretical model based on the rule of mixtures was derived to model the fiber and matrix creep-time-dependent stress redistribution. Fiber and matrix creep parameters, load transfer model results, and numerical modeling were used to construct a creep strain model to predict creep damage evolution of minicomposites with different fiber types and contents.     

Microstructure and damage evolution of SiCf/PyC/SiC and SiCf/BN/SiC mini-composites: A synchrotron X-ray computed microtomography study

SiC_f/PyC/SiC and SiC_f/BN/SiC mini-composites comprising single tow SiC fibre-reinforced SiC with chemical vapor deposited PyC or BN interface layers are fabricated. The microstructure evolutions of the mini-composite samples as the oxidation temperature increases (oxidation at 1000, 1200, 1400, and 1600?°C in air for 2?h) are observed by scanning electron microscopy, energy dispersive spectrometry, and X-ray diffraction characterization methods. The damage evolution for each component of the as-fabricated SiC_f/SiC composites (SiC fibre, PyC/BN interface, SiC matrix, and mesophase) is mapped as a three-dimensional (3D) image and quantified with X-ray computed tomography. The mechanical performance of the composites is investigated via tensile tests.The results reveal that tensile failure occurs after the delamination and fibre pull-out in the SiC_f/PyC/SiC composites due to the volatilization of the PyC interface at high temperatures in the air environment. Meanwhile, the gaps between the fibres and matrix lead to rapid oxidation and crack propagation from the SiC matrix to SiC fibre, resulting in the failure of the SiC_f/PyC/SiC composites as the oxidation temperature increases to 1600?°C. On the other hand, the oxidation products of B₂O₃ molten compounds (reacted from the BN interface) fill up the fracture, cracks, and voids in the SiC matrix, providing excellent strength retention at elevated oxidation temperatures. Moreover, under the protection of B₂O₃, the SiC_f/BN/SiC mini-composites show a nearly intact microstructure of the SiC fibre, a low void growth rate from the matrix to fibre, and inhibition of new void formation and the SiO₂ grain growth from room to high temperatures. This work provides guidance for predicting the service life of SiC_f/PyC/SiC and SiC_f/BN/SiC composite materials, and is fundamental for establishing multiscale damage models on a local scale.     

Effect of PyC interphase thickness on mechanical and ablation properties of 3D Cf/ZrC–SiC composite

Three-dimensional (3D) C_f/ZrC–SiC composites were successfully prepared by the polymer infiltration and pyrolysis (PIP) process using polycarbosilane (PCS) and a novel ZrC precursor. The effects of PyC interphase of different thicknesses on the mechanical and ablation properties were evaluated. The results indicate that the C_f/ZrC–SiC composites without and with a thin PyC interlayer of 0.15 µm possess much poor flexural strength and fracture toughness. The flexural strength grows with the increase of PyC layer thickness from 0.3 to 1.2 µm. However, the strength starts to decrease with the further increase of the PyC coating thickness to 2.2 µm. The highest flexural strength of 272.3±29.0 MPa and fracture toughness of 10.4±0.7 MPa m^1/2 were achieved for the composites with a 1.2 µm thick PyC coating. Moreover, the use of thicker PyC layer deteriorates the ablation properties of the C_f/ZrC–SiC composites slightly and the ZrO₂ scale acts as an anti-ablation component during the testing.