Microstructure and mechanical properties of quasi-isotropic chopped fiber-reinforced PyC–SiC matrix composite prepared by novel nondamaging method

In this work, quasi-isotropic chopped carbon fiber-reinforced pyrolytic carbon and silicon carbide matrix (C_f/C–SiC) composites and chopped silicon carbide fiber-reinforced silicon carbide matrix (SiC_f/SiC) composites were prepared via novel nondamaging method, namely airlaid process combined with chemical vapor infiltration. Both composites exhibit random fiber distribution and homogeneous pore size. Young's modulus of highly textured pyrolytic carbon (PyC) matrix is 23.01 ± 1.43 GPa, and that of SiC matrix composed of columnar crystals is 305.8 ± 9.49 GPa in C_f/C–SiC composites. Tensile strength and interlaminar shear strength of C_f/C–SiC composites are 52.56 ± 4.81 and 98.16 ± 24.62 MPa, respectively, which are both higher than those of SiC_f/SiC composites because of appropriate interfacial shear strength and introduction of low-modulus and highly textured PyC matrix. Excellent mechanical properties of C_f/C–SiC composites, particularly regarding interlaminar shear strength, are due to their quasi-isotropic structure, interfacial debonding, interfacial sliding, and crack deflection. In addition to the occurrence of crack deflection at the fiber/matrix interface, crack deflection in C_f/C–SiC composites takes also place at the interface between PyC–SiC composite matrix and the interlamination of multilayered PyC matrix. Outstanding mechanical properties of as-prepared C_f/C–SiC composites render them potential candidates for application as thermal structure materials under complex stress conditions.     

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.     

界面类型对三维Nextel 720纤维增韧莫来石陶瓷基复合材料力学性能的影响

采用化学气相渗透工艺在Nextel 720纤维表面制备PyC和PyC／SiC两种涂层，然后以正硅酸乙酯和异丙醇铝作为先驱体，以先驱体浸渗热解法制备三维Nextd 720纤维增韧莫来石陶瓷基复合材料，比较分析了两种涂层复合材料的力学性能和断裂模式。结果表明：具预先涂覆PyC的复合材料中纤维与基体直接接触，发生烧结形成强结合界面，复合材料脆性断裂，三点抗弯强度仅56MPa。PyC／SiC涂层则演化为间隙／SiC复合界面层，SiC成为阻滞纤维与基体接触的阻挡层，间隙保证了纤维拔出，复合材料韧性断裂且三点抗弯强度高达267．2MPa。     

Microstructure and properties of CNTs reinforced CVI-pyrocarbon matrix

Pyrocarbon (PyC) matrices were prepared in two kinds of quartz fiber preforms by chemical vapor infiltration (CVI), and then the fibers were leached by HF. Effects of CNTs on the microstructures and mechanical properties of the quartz fiber reinforced carbon composites and PyC matrices, as well as the interface behaviors of the fiber reinforced composites, were discussed. Randomly oriented CNTs reinforced PyC micro-composites account for the pseudo ISO structure and contribute to the mechanical properties of the PyC matrix. Relative strength between reinforcement and matrix and interface bonding significantly affect the mechanical behaviors of the quartz fiber reinforced pyrocarbon composites: Quartz fiber with low strength and strong interface bonding result in limited strengthening effect on flexural strength of the fiber reinforced composite; low strength unidirectional quartz fiber and weak interface bonding in a much stronger matrix result in limited strengthening effect on tensile strength of the composite.     

Mechanical properties and strengthening mechanism of SiCf/SiC mini-composites modified by SiC nanowires

The effects of the SiC nanowires (SiCNWs) and PyC interface layers on the mechanical and anti-oxidation properties of SiC fiber (SiC_f)/SiC composites were investigated. To achieve this, the PyC layer was coated on the SiC_f using a chemical vapour infiltration (CVI) method. Then, SiCNWs were successfully coated on the surface of SiC_f/PyC using the electrophoretic deposition method. Finally, a thin PyC layer was coated on the surface of SiC_f/PyC/SiCNWs. Three mini-composites, SiC_f/PyC/SiC, SiC_f/PyC/SiCNWs/SiC, and SiC_f/PyC/SiCNWs/PyC/SiC, were fabricated using the typical precursor infiltration and pyrolysis method. The morphologies of the samples were examined using scanning electron microscopy and energy dispersive X-ray spectrometry. Tensile and single-fibre push-out tests were carried out to investigate the mechanical performance and interfacial shear strength of the composites before and after oxidization at 1200 °C. The results revealed that the SiC_f/PyC/SiCNWs/SiC composites showed the best mechanical and anti-oxidation performance among all the composites investigated. The strengthening and toughening is mainly achieved by SiCNWs optimization of the interfacial bonding strength of the composite and its own nano-toughening. On the basis of the results, the effects of SiCNWs on the oxidation process and retardation mechanism of the SiC_f/SiC mini-composites were investigated.     

Fabrication and properties of SiCnw-reinforced SiC composites by reactive melt infiltration with BN and PyC interface

To tailor the fiber–matrix interface of SiC nanowires-reinforced SiC (SiC_nw/SiC) ceramic matrix composites (CMCs) for improved mechanical properties, SiC nanowires were coated with BN and pyrolytic carbon (PyC) compound coatings prepared by the dip-coating process in boric acid and urea solution and the pyrolysis of phenolic resin. SiC_nw/SiC CMC with PyC/BN interfaces were fabricated by reactive melt infiltration (RMI) at 1680°C for 1 h. The influences of phenolic resin content on the microstructure and mechanical properties of the CMC were investigated. The results showed that the flexural strength and fracture toughness reach the maximum values of 294 MPa and 4.74 MPa m^1/2 as the phenolic resin content was 16 and 12 wt%, respectively. The displacement–load curve of the sample exhibited a gradient drop with increasing phenolic resin content up to 12 wt%. The results demonstrated that the PyC/BN compound coatings could play the role of protecting the SiC_nw from degradation as well as improving the more moderate interfacial bonding strengths during the RMI.     

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.     

Architectural engineering inspired method of preparing Cf/ZrC–SiC with graceful mechanical responses

Inspired by grouting technique in architectural engineering, an innovative method of slurry injection and vacuum impregnation was put forward to introduce nanosized ZrC–SiC ceramics into PyC modified 3-D needle-punched carbon fiber preform homogeneously and continuously, followed by spark plasma sintering to prepare C_f/ZrC–SiC with graceful mechanical responses. The composite possessed improved fracture toughness and work of fracture at 5.37 ± 0.25 MPa∙m^1/2 and 951 ± 12 J/m², 50% and nearly one order of magnitude higher than those of ZrC–SiC composite, respectively, with rivaling flexural strength at 177 ± 8 MPa synchronously. A graceful fracture mode was embodied in an obviously extended yield plateau with increased failure displacement by 300%. This enhancement was attributed to the uniform and continuous combination of ZrC–SiC with carbon fiber preform as well as protection and interface tailoring from PyC coating. The study offered an easy and effective method of preparing 3-D fiber reinforced ceramic matrix composites.     

Interfacial optimization of SiC nanocomposites reinforced by SiC nanowires with high volume fraction

High volume fraction SiC nanowires-reinforced SiC composites (SiCNWs/SiC) were prepared by hybrid process of chemical vapor infiltration and polymer impregnation/pyrolysis in this research. SiCNWs networks are first to be made promising a high volume fraction (20 vol%), and the pyrolytic carbon (PyC) interphase with 5 nm is designed on SiCNWs surface to optimize the bonding condition between SiCNWs and SiC matrix. Nanoindentation shows a modulus of 494 ± 14 GPa of SiCNWs/SiC composites without interphase comparing to the one with PyC interphase of 452 ± 13 GPa. However, the 3-point bending test shows a higher strength of the composite with PyC interphase (273 ± 32 MPa) comparing with the one without interphase (240 ± 38 MPa). The fracture surface is observed under SEM, which shows a longer SiCNWs pullout of the composite with PyC interphase. The energy dissipation during the 3-point bending test is calculated by the length of nanowire pull-out, it demonstrates that the SiCNWs with PyC interphase possess better performance for toughening composite. Further characterization proves that the PyC interphase can give SiCNWs/SiC composites higher fracture toughness (4.49 ± 0.44 MPa·m^1/2) than the composites without interphase (3.66 ± 0.28 MPa·m^1/2).     

Effect of interface types on the heat-resistance of Cansas-II SiCf /SiC composites

The heat-resistance of the Cansas-II SiC/CVI-SiC mini-composites with a PyC and BN interface was studied in detail. The interfacial shear strength of the SiC/PyC/SiC mini-composites decreased from 15 MPa to 3 MPa after the heat treatment at 1500 °C for 50 h, while that of the SiC/BN/SiC mini-composites decreased from 248 MPa to 1 MPa, which could be mainly attributed to the improvement of the crystallization degree of the interface and the decomposition of the matrix. Aside from the above reasons, the larger declined fraction of the interfacial shear strength of the SiC/BN/SiC mini-composites might also be related to the gaps in the BN interface induced by the volatilization of B₂O₃·SiO₂ phase, leading to a significant larger declined fraction of the tensile strength of the SiC/BN/SiC mini-composites due to the obvious expansion of the critical flaws on the fiber surface. Therefore, compared with the CVI BN interface, the CVI PyC interface has better heat-resistance at high temperatures up to 1500 °C due to the fewer impurities in PyC.     

Superior mechanical properties of lithium aluminosilicate composites by pyrolytic carbon intercalated carbon fibers/carbon nanotubes multi-scale reinforcements

Performance degradation always occurs in carbon fibers/carbon nanotubes (CFs/CNTs) multi-scale reinforced composites prepared by chemical vapor deposition (CVD) method. In this study, pyrolytic carbon (PyC) interlayers are introduced to overcome this problem, and the mechanism is studied in detail. The multi-scale reinforcements are combined with lithium aluminosilicate (LAS) glass-ceramic into ceramic matrix composites by slurry impregnation and hot pressing sintering. The results show that the PyC interlayers can protect the CFs from corrosion of the catalyst at high temperature, improve stress transfers and promote the synergy between various components. The CNTs and LAS matrix form a transition area, which causes deflection and shunting when cracks propagate. These factors have greatly increased the crack extension energy, so the mechanical properties have been greatly improved. The flexural strength, fracture toughness and work of fracture reach 602 ± 55 MPa, 10.7 ± 2 MPa m^1/2, 4.6 ± 0.7 kJ m⁻², respectively, which are 42.3%, 42.6% and 76.9% higher than CF/LAS. This work expands the study of the CFs/CNTs multi-scale reinforcements and the LAS composites, and provides a useful reference for the related research.     

Fabrication and characteristic of non-oxide fiber tow reinforced silicon nitride matrix composites by low temperature CVI process

Non-oxide fiber tow reinforced silicon nitride matrix composite was fabricated by low temperature CVI process with PyC as interphase. The tensile strength of the C and SiC fiber tow composites were 547 MPa and 740 MPa, respectively. The difference in tensile strength was analyzed based on the length, amount of pull-out fiber and also interface bonding. The infiltration uniformity of CVI silicon nitride (SiN) matrix within SiC fiber tow was comparable with that of CVI SiC matrix. These results suggested that the low temperature CVI process is suitable for the fabrication of fiber reinforced SiN matrix composites with proper interface bonding and high strength.     

The improvement of mechanical properties of SiC/SiC composites by in situ introducing vertically aligned carbon nanotubes on the PyC interface

In order to improve the mechanical properties, vertically aligned carbon nanotubes (VACNTs) were in situ introduced on the pyrocarbon (PyC) interfaces of the multilayer preform via chemical vapor deposition (CVD) process under tailored parameters. Chemical vapor infiltration (CVI) process was then employed to densify the multilayer preform to acquire SiC/SiC composites. The results show that the growth of VACNTs on PyC interface is highly dependent to the deposition temperature, time and constituent of gas during CVD process. The preferred orientation and high graphitization of VACNTs were obtained when temperature is 800?℃ and C₂H₄/H₂ ratio is 1:3. The bending strength and fracture toughness of SiC/SiC composites with PyC and PyC-VACNTs interfaces were compared. Compared to the SiC/SiC composite with PyC interface, the bending strength and fracture toughness increase 1.298 and 1.359 times, respectively after the introduction of PyC-VACNTs interface to the SiC/SiC composites. It is also demonstrated that the modification of PyC interface with VACNTs enhances the mechanical properties of SiC/SiC composites due to the occurrence of more fiber pull-outs, interfacial debonding, crack branching and deflection     

SiCf/SiO2复合材料的制备及界面层对其力学性能的影响

以碳化硅(SiC)纤维为增强体,采用真空浸渍法制备了2.5维连续SiC纤维增韧的SiO2基(SiCf/SiO2)复合材料,研究了SiC纤维编织体上不同的界面层对SiCf/SiO2复合材料力学性能的影响.化学气相渗透(CVI)法制备的热解碳(PyC)和PyC/SiC双层界面层分别使材料的抗弯强度由无界面层的52.2 MPa提高至67.4 MPa和180.3 MPa,但均使材料的韧性降低.用扫描电镜观察了材料的断口形貌,结果表明,PyC和PyC/SiC层不仅提高了材料的抗弯强度,而且增加了基体同纤维间的结合力,使基体有效地将载荷传递给纤维.PyC/SiC层能有效地保护SiC纤维,防止烧结过程中释放出的结晶水对纤维的损伤,有助于提高材料的力学性能.     

Mechanical properties and oxidation resistance of SiCf/CVI-SiC composites with PIP-SiC interphase

SiC coatings were successfully synthesized on SiC fibers by precursor infiltration and pyrolysis (PIP) method using polycarbosilane (PCS) as precursor. The morphology of as-fabricated coatings was observed by SEM, and its structure was characterized by XRD and Raman spectrum. The SiC fiber reinforced chemical vapor infiltration SiC (SiC_f/CVI-SiC) composites with PIP-SiC coatings as interphase were fabricated. And, the effects of PIP-SiC interphase on mechanical properties of composites were investigated. The experimental results point out that the coating is smooth and there is little bridging between fibers. The coating is amorphous with SiC and carbon micro crystals. The flexural strength of composites with and without PIP-SiC interphase is 220 and 100 MPa, respectively. And the composites with PIP-SiC interphase obviously exhibit a toughened fracture behavior. The oxidation resistance of composites with PIP-SiC interphase is much better than that of composites with pyrolytic carbon (PyC) interphase.     

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.     

Boosting bonding strength of hydroxyapatite coating for carbon/carbon composites via applying tree-planting interface structure

Hydroxyapatite (HA) coated carbon/carbon composites (CC) is a potential material for orthopedic application because of the combination of good biocompatibility and mechanical properties. In this work, we synthesize a tree-planting interface which is composed of holes formed by micro-oxidized CC substrates and carbon nanotubes (CNTs) to achieve a high bonding strength of HA coating. The holes include annular gaps between carbon fiber and pyrolytic carbon, as well as irregular holes formed by oxidized pyrolytic carbon. The CNTs can grow inside the holes and extend into the HA coating. As a result, the bonding strength of HA coating with tree-planting interface achieves 11.14 ± 0.78 MPa. It increases by 181.3% comparing with the HA coating on CC without interface (3.96 ± 0.30 MPa). The in-vitro bioactivity evaluated by the response of mesenchymal stem cells (MSCs) shows promotions of cell proliferation and cell activity with increasing culture time. After applied with tree-planting interface, the HA coating with strong bonding and good bioactivity may be applied in orthopedic field in the future.     

Effect of PyC interphase thickness on mechanical behaviors of SiBC matrix modified C/SiC composites fabricated by reactive melt infiltration

A dense carbon fiber reinforced silicon carbide matrix composites modified by SiBC matrix (C/SiC-SiBC) was prepared by a joint process of chemical vapor infiltration, slurry infiltration and liquid silicon infiltration. The effects of pyrolytic carbon (PyC) interphase thickness on mechanical properties and oxidation behaviors of C/SiC-SiBC composites were evaluated. The results showed that C/SiC-SiBC composites with an optimal PyC interphase thickness of 450 nm exhibited flexural strength of 412 MPa and fracture toughness of 24 MPa m^1/2, which obtained 235% and 300% improvement compared with the one with 50 nm-thick PyC interphase. The enhanced mechanical properties of C/SiC-SiBC composites with the increase of interphase thickness was due to the weakened interfacial bonding strength and the decrease of matrix micro-crack amount associated with the reduction of thermal residual stress. With the decrease in matrix porosity and micro-crack density, C/SiC-SiBC composites with 450 nm-thick interphase exhibited excellent oxidation resistance. The residual flexural strength after oxidized at 800, 1000 and 1200 °C in air for 10 h was 490, 500 and 480 MPa, which increased by 206%, 130% and 108% compared with those of C/SiC composites.     

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.     

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.