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.     

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.     

Fabrication and properties of Cf/ZrC‐SiC‐based composites by an improved reactive melt infiltration

C_f/ZrC‐SiC composites with a density of 2.52 g/cm³ and a porosity of 1.68% were fabricated via reactive melt infiltration (RMI) of Si into nano‐porous C_f/ZrC‐C preforms. The nano‐porous C_f/ZrC‐C preforms were prepared through a colloid process, with a ZrC “protective coating” formed surrounding the carbon fibers. Consequently, highly dense C_f/ZrC‐SiC composites without evident fiber/interphase degradation were obtained. Moreover, abundant needle‐shaped ZrSi₂ grains were formed in the composites. Benefiting from this unique microstructure, flexural strength, and elastic modulus of the composites are as high as 380 MPa and 61 GPa, respectively, which are much higher than C_f/ZrC‐SiC composites prepared by conventional RMI.     

Additive manufacturing of continuous carbon fiber–reinforced silicon carbide ceramic composites

A material extrusion (MEX) technology has been developed for the additive manufacturing of continuous carbon fiber–reinforced silicon carbide ceramic (C_f/SiC) composites. By comparing and analyzing the rheological properties of the slurries with different compositions, a slurry with a high solid loading of 48.1 vol% and high viscosity was proposed. Furthermore, several complex structures of C_f/SiC ceramic composites were printed by this MEX additive manufacturing technique. Phenolic resin impregnation–carbonization process reduces the apparent porosity of the green body and protects the C_f. Finally, the reactive melting infiltration (RMI) process was used to prepare samples with different C_f contents from 0 to 2 K (a bundle of carbon fibers consisting of 1000 fibers). Samples with C_f content of 1 K show the highest bending strength (161.6 ± 10.5 MPa) and fracture toughness (3.72 ± 0.11 MPa·m^1/2) while the thermal conductivity of the samples with the C_f content of 1 K reached 11.0 W/(m·K). This study provides a strategy to prepare C_f/SiC composites via MEX additive manufacturing and RMI.     

Reactive melt infiltrated Cf/SiC composites with robust matrix derived from novel engineered pyrolytic carbon structure

Needle-punched C_f/SiC composites were fabricated by a novel pore tuned reactive melt infiltration (RMI) process. The novel hierarchically porous carbon structure in the fiber preform with the porosity well open to liquid silicon was engineered by impregnation of phenolic resin with addition of a pore former. Neither residual bulk carbon nor residual bulk silicon is detected in the matrix of the C_f/SiC composites prepared by the pore tuned RMI, indicating that a robust matrix with homogenous SiC can be formed. The composite prepared by the pore tuned RMI exhibits a tensile strength of 159±5 MPa, which is 46% higher than that without addition of pore former.     

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.     

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.     

Enhanced mechanical and dielectric properties of SiCf/SiC composites with silicon oxycarbide interphase

SiC_f/SiC composites with silicon oxycarbide (SiOC) interphase were successfully prepared using silicone resin as interphase precursor for dip-coating process and polycarbosilane as matrix precursor for PIP process assisted with hot mold pressing. The effects of SiOC interphase on mechanical and dielectric properties were investigated. XRD and Raman spectrum results show that SiOC interphase is composed of silicon oxycarbide and free carbon with a relatively low crystalline degree. The surface morphology of SiC fibers with SiOC interphase is smooth and homogeneous observed by SEM. The flexural strength and failure displacement of SiC_f/SiC composites with SiOC interphase vary with the thickness of interphase and the maximum value of flexural strength is 289 MPa with a failure displacement of 0.39 mm when the thickness of SiOC interphase is 0.25 µm. The complex permittivity of the composites increases from 8.8-i5.7 to 9.8-i8.3 with the interphase thicker.     

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.     

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%.     

Effect of slurry and sol-gel introduce SiCnws on ablation and bending behaviors of modified SiCf/HfC-SiC composites

The slurry and sol-gel methods were used to introduce SiC nanowires (SiC_nws) into the SiC_f/HfC-SiC composites. The microstructures, ablation, and bending behaviors of the SiC_nws modified composites prepared by the two methods were compared. The bending strengths of the modified composites obtained by introducing SiC_nws by the slurry and sol-gel methods were 224 ± 19 and 154 ± 14 MPa, respectively. The results showed that SiC fibers with chemical corrosion and thermal damage during the sol-gel process decreased the bending strength of the SiC_nws-modified SiC_f/HfC-SiC composites. Meanwhile, the pyrolytic carbon interface accompanying corrosion damage in the sol-gel process led to the degradation of interface function, which hindered the interface debonding and fiber sliding of the composites during the bending test. After ablation, the bending strengths of the two composites were 188 ± 19 and 50 ± 7 MPa, respectively. The bending strength retention of the modified composites fabricated by the slurry method (83.9%) was higher than that (32.5%) of the composites fabricated by the sol-gel method after ablation. As the composites fabricated by the slurry method exhibited a good ablation resistance under the oxyacetylene flame (∼2350°C).     

Effects of heat treatment on mechanical and dielectric properties of 3D Si3N4f/BN/Si3N4 composites by CVI

In this study, three-dimensional silicon nitride fiber-reinforced silicon nitride matrix (3D Si₃N_4f/BN/Si₃N₄) composites with a boron nitride (BN) interphase were fabricated through chemical vapor infiltration. Through comparing the changes of microstructure, thermal residual stress, interface bonding state, and interface microstructure evolution of composites before and after heat treatment, the evolution of mechanical and dielectric properties of Si₃N_4f/BN/Si₃N₄ composites was analyzed. Flexural strength and fracture toughness of composites acquired the maximum values of 96 ± 5 MPa and 3.8 ± 0.1 MPa·m^1/2, respectively, after heat treatment at 800 °C; however, these values were maintained at 83 ± 6 MPa and 3.1 ± 0.2 MPa·m^1/2 after heat treatment at 1200 °C, respectively. The relatively low mechanical properties are mainly attributed to the strong interface bonding caused by interfacial diffusion of oxygen and subsequent interfacial reaction and generation of turbostratic BN interphase with relatively high fracture energy. Moreover, the Si₃N_4f/BN/Si₃N₄ composites also displayed moderate dielectric constant and dielectric loss fluctuating irregularly around 5.0 and 0.04 before and after heat treatment, respectively. They were mainly determined based on the intrinsic properties of materials system and complex microstructure of composites.     

Selection principle of the synthetic route for fabrication of HfB2 and HfB2-SiC ceramics

Densification, microstructure, and mechanical properties of spark plasma sintered HfB₂ and HfB₂-SiC ceramics using HfB₂ powders from borothermal reduction and boro/carbothermal reduction were investigated and compared. It was found that HfB₂ceramics obtained by boro/carbothermal reduction exhibited a significantly higher sinterability compared to that by borothermal reduction. Inversely, HfB₂-SiC ceramics obtained by borothermal reduction exhibited a refined microstructure and better mechanical properties (Vickers hardness: 23.60 ± 2.43 GPa; fracture toughness: 5.89 ± 0.30 MPa.m^1/2) than that by boro/carbothermal reduction. These results indicated that optimal fabrication of HfB₂-based ceramics could be achieved by the selection of synthetic route of HfB₂ powders.     

Microstructure and mechanical properties of carbon/carbon composites with PyC/SiC/TiC multilayer interphases

Carbon/carbon composites with PyC/SiC/TiC multilayer interphases (CCs-PST) have been successfully prepared by a joint process of chemical vapor deposition and carbothermal reduction. Effect of the Ti(OC₄H₉)₄/C₆H₄(OH)₂ molar ratio on the morphology of TiC particles was investigated and the ratio was optimized as 8:1. When the Ti(OC₄H₉)₄/C₆H₄(OH)₂ molar ratio was 8:1, many homogeneously distributed TiC nanoparticles with the sizes of 100–500 nm on the fibers were observed. The structural evolution of CCs-PST was discussed and the mechanical properties of as-prepared materials were investigated by flexural and interlaminar shear tests. The resulted composites demonstrated a PyC and SiC mixed inner interphase with the thickness of 0.5–1 $\mathrm{\mu }\mathrm{m}$ and a TiC outer interphase with a thickness about 0.5 µm. Flexural strength of 201.45 ± 5.27 MPa and modulus of 21.21 ± 1.58 GPa showed a 41.7% and 7.83% improvement respectively as compared with that of the neat CCs. The interlaminar shear strength of CCs-PST was 66.71 ± 4.87 MPa, which was 51.20% higher than that of the CCs. The improved mechanical properties were attributed to the enhanced interface bond between fibers and matrix induced by the PST.     

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.     

Phase-field simulation of microscale crack propagation/deflection in SiCf/SiC composites with weak interphase

To understand the microscale toughening mechanism, the crack propagation, and stress–strain response of unidirectional SiC_f/SiC composites with h-BN interphase under transverse and longitudinal tension are investigated by a promising micromechanical phase field (PF) method along with representative volume element. Of much interest, the calculation results are well consistent with the available experimental results. With a strong dependence on the interphase strength, the toughening mechanisms during crack propagation are well presented, for example, fiber pull-out, crack deflection, and interphase debonding. Furthermore, the longitudinal tensile strength of SiC_f/SiC composites increases with decreasing the interphase strength, where only a weak enough interphase can result in a significant crack deflection by its cracking. In particular, the ratio of the interphase strength along fibers to the matrix strength should be less than 1.254 to ensure crack deflection in the interphase and fiber pull-out. Moreover, the transverse tensile strength of SiC_f/SiC composites reaches a maximum with increasing the interphase thickness into the range of 0.25–0.5 µm.     

Microstructure control of highly oriented short carbon fibres in SiC matrix composites fabricated by direct ink writing

A novel method is proposed for fabricating highly oriented carbon fibre reinforced SiC ceramic composites (C_f/SiC) by direct ink writing (DIW). For the first time, the control of carbon fibers’ orientation in DIW was studied by numerical simulation. An interfacial layer was prepared by chemical vapor infiltration (CVI). The microstructure and phase composition of C_f/SiC were studied by scanning electron microscopy and X-ray diffraction, respectively. The results showed that fibers of different interfacial thicknesses could be obtained effectively by varying the CVI time. The breakage of short fibres remarkably improved the fracture toughness of the parts. The specimens showed excellent mechanical properties with bending strength of 274 ± 13 MPa and fracture toughness of 5.82 ± 0.25 MPa m^1/2. This method could be extended to the preparation of other resin and ceramic composites.     

Processing of Cf/SiC composites by hot pressing using polymer binders followed by polymer impregnation and pyrolysis

Continuous carbon fiber (C_f) reinforced silicon carbide (SiC) matrix composite (C_f/SiC) was processed through hot pressing (HP) using polycarbosilane (PCS) in matrix and polysilazane in interphase regions as polymer binders. HP experiments were conducted at 4 MPa, 1200 °C and 1 h; followed by PCS polymer impregnation and pyrolysis (PIP) at 1200 °C under vacuum. The BN/SiC-Si₃N₄ interphase formed on the C_f cloth during BN dispersed polysilazane polymer coating and pyrolysis. The influence of PCS quantity during HP experiments on C_f/SiC composites was studied. Results suggest that sintering of SiC matrix in C_f/SiC composite improves by increasing PCS content during HP; however, high PCS content increases the liquidity of SiC-PCS mixture to flow out of the composite structure. The C_f/SiC composites with relative density ranging from 79 to 83% and flexural strength from 67 to 138 MPa was achieved.     

Tailoring Carbon Fiber/Carbon Nanotubes Interface to Optimize Mechanical Properties of Cf‐CNTs/SiC Composites

C_f/SiC composites were fabricated using fiber coatings including CNTs and matrix infiltration using the polymer impregnation and pyrolysis process. Interface between fiber and CNTs (CF/CNTs) was tailored to optimize mechanical properties of hybrid composites. The tailored interphases, such as Pyrocarbon (PyC) and PyC/SiC, protect fibers from degradation during the growth of CNTs successfully. Hybrid composites with well‐tailored CF/CNTs interface displayed significantly increased mechanical strength (352 ± 21 MPa) compared with that (34 ± 3 MPa) of composites reinforced with CNTs, which grown on carbon fibers directly. The interfacial bonding strength of hybrid composites was improved and optimized by tailoring the CF/CNTs interface. Interfacial failure modes were studied, and a firm interface bonding at the joint where CNTs grown was observed.     

Influence of graphitization treatment on microstructure and flexural strength of C/C-ZrC-SiC composites fabricated via reactive melt infiltration

C/C-ZrC-SiC composites were prepared by chemical vapor infiltration (CVI) and molten salt assisted reactive melt infiltration (RMI). The microstructure of low density and high density C/C composites without graphitization (LC/HC) and graphitization at 2000 °C (LCG/HCG) were compared. Moreover, the effects of graphitization of LC and HC on the microstructure and flexural strength of C/C-ZrC-SiC composites were investigated in detail. The composites prepared by infiltration of LC and LCG had lower flexural strength, 220.01 ± 21.18 MPa and 197.94 ± 19.05 MPa, respectively. However, the composites prepared by HC and HCG presented higher flexural strength, 308.76 ± 12.35 MPa and 289.62 ± 8.70 MPa, respectively. This was due to the phenomenon of fiber erosion in both LC and LCG during the RMI process. After graphitization, the flexural strength of C/C-ZrC-SiC composites prepared by RMI decreased, but the fracture behavior of the composites tends to be more mild. The decreased strength of the composites were caused by the increased matrix cracks, fiber damage in high temperature and the weak interfacial bonding. The improve of failure behavior of the composites was due to interface debonding between the fiber and matrix, and composites can consume the fracture energy through fiber pull-out.