Tension-tension fatigue behavior of unidirectional SiC/Si3N4 composite with strong and weak interface bonding at room temperature

In this paper, the tension-tension fatigue behavior of unidirectional SiC/Si₃N₄ ceramic-matrix composite with strong and weak interface bonding at room temperature has been investigated using a micromechanical approach. The hysteresis loops models considering different interface slip cases have been developed to establish the relationships between fatigue hysteresis loops, hysteresis dissipated energy, hysteresis modulus, and the interface shear stress. The damage evolution process under tension-tension fatigue loading has been analyzed using hysteresis loops. By comparing experimental fatigue hysteresis dissipated energy with theoretical computational values, the interface shear stresses of SiC/Si₃N₄ composite with weak and strong interface bonding were obtained for different cycle numbers. The fatigue life S‒N curves and broken fibers fraction versus cycle number curves corresponding to different fatigue peak stresses have been predicted. For SiC/Si₃N₄ with strong interface bonding, the fatigue limit stress approaches to 75% tensile strength, which is much higher than that of composite with weak interface bonding, i.e., 58% tensile strength, due to the higher interface shear stress degradation rate for weak bonding interface.     

Modeling matrix multicracking development of fiber-reinforced ceramic-matrix composites considering fiber debonding

In this paper, the effect of fiber debonding on matrix multicracking development of different fiber-reinforced CMCs is investigated using the micromechanical approach. The Budiansky–Hutchinson–Evans shear-lag model is adopted to analyze the fiber and matrix stress distributions of the damaged composite. The fracture mechanics approach is used to determine the fiber/matrix interface debonding length. Combining the critical matrix strain energy criterion and fracture mechanics fiber/matrix interface debonding criterion, the stress-dependent matrix multicracking development is analyzed for different fiber volume fraction, fiber/matrix interface properties and matrix cracking characteristic stress. The experimental matrix multicracking development of unidirectional C/Si₃N₄, SiC/Si₃N₄, SiC/CAS, SiC/CAS-II, SiC/SiC, SiC/Borosilicate and mini-SiC/SiC composites are predicted.     

Structure and performance of Si3N4/SiC/CNT composite fibres

Herein, a homogeneously distributed and well-orientated ceramic-CNT composite fibre (Si₃N₄/SiC/CNTs) has been prepared using carbon nanotube fibres (CNTFs) premixed with silicon powder, followed by the reaction-bonded sintering process. The SiC layers around the CNT bundles interspersed in the composite are formed during the silicon reaction stage through the contact of silicon and CNTs, and the densification of the ceramic through the further reaction-bonded silicon carbide and nitride. Due to strong interface bonding, the composite fibres exhibit the potential for CNT-based damage sensing with a tensile strength upto 225 Mpa. Furthermore, the high-volume distribution of CNT sresults in a significant enhancement of the electrical and thermal conductivities as well as photoluminescence properties. Our work provides a useful approach for thefabrication of multifunctional fibres for imaging, engineering, and other complex applications.     

Damage resistance of SiC and Si3N4 coatings with control of microstructure and thickness

We investigated the contact damage and indentation stress–strain behavior of silicon carbide (SiC) coatings and binary coatings consisting of SiC and silicon nitride (Si₃N₄), synthesized on graphite substrates with porosities of 10 and 13% by a solid–vapor reaction, in order to determine the coatings’ damage resistance. The coating thickness was affected by the porosity of the substrate. The coatings on the substrate with 13% porosity showed a graded interface structure below the top dense layer. The SiC coatings were thicker than the SiC/Si₃N₄ composite coatings. The SiC coatings made the substrates hard, and SiC-coated substrates exhibited higher stress–strain curves than the substrates alone, but the SiC/Si₃N₄ composite coatings appeared unaffected. The coating thickness played an important role in limiting the effect of damage. The hardness values of the SiC coatings were higher than those of the substrates and the SiC/Si₃N₄ coatings. These corresponded well with the indentation stress–strain curves. The values of each coating showed saturated points depending on the applied load. This indicated that the substrate itself influenced the damage resistance of the coatings because of the layered structure of a harder coating with a softer substrate. The coatings enhanced contact damage and transmitted the damage to the substrates at a high load of P = 2000 N. Both coatings showed an extensive subsurface damage, independent of the porosity of the substrate. In cyclic indentation tests, the contact diameters linearly increased with the number of cycles and depended on the porosity of the substrate, showing smaller contact diameters by coating the substrate.     

Wet chemical deposition of BN,SiC and Si3N4 interphases on SiC fibers

Fiber coatings based on BN, BN/SiC and BN/Si₃N₄ were deposited on Hi Nicalon type S SiC fibers. The coating parameters were optimized using a design of experiments study. With optimized parameter sets, the coatings exhibited a high degree of coverage on the fibers and almost no fiber bridging could be observed. The coated fiber bundles are flexible and can be processed further by techniques such as filament winding. In comparison to a non-processed reference sample, the maximum tensile load of the fiber bundles with BN, BN/SiC and BN/Si₃N₄ coatings was reduced by only 5 %, 13 % and 10 %, respectively. The coated fiber bundles retained their tensile strength after thermal annealing up to 1650 °C in a nitrogen atmosphere for 0.5 h. SiC_f/SiC samples with BN/SiC fiber coatings exhibited higher values of bending strength and strain-to-failure as a reference sample without fiber coating indicating the functionality of the fiber coatings.     

Microstructure and tensile behavior of (BN/SiC)n coated SiC fibers and SiC/SiC minicomposites

Interphase plays an important role in the mechanical behavior of SiC/SiC ceramic-matrix composites (CMCs). In this paper, the microstructure and tensile behavior of multilayered (BN/SiC)_n coated SiC fiber and SiC/SiC minicomposites were investigated. The surface roughness of the original SiC fiber and SiC fiber deposited with multilayered (BN/SiC), (BN/SiC)₂, and (BN/SiC)₄ (BN/SiC)₈ interphase was analyzed through the scanning electronic microscope (SEM) and atomic force microscope (AFM) and X-ray diffraction (XRD) analysis. Monotonic tensile experiments were conducted for original SiC fiber, SiC fiber with different multilayered (BN/SiC)_n interfaces, and SiC/SiC minicomposites. Considering multiple damage mechanisms, e.g., matrix cracking, interface debonding, and fibers failure, a damage-based micromechanical constitutive model was developed to predict the tensile stress-strain response curves. Multiple damage parameters (e.g., matrix cracking stress, saturation matrix crack stress, tensile strength and failure strain, and composite’s tangent modulus) were used to characterize the tensile damage behavior in SiC/SiC minicomposites. Effects of multilayered interphase on the interface shear stress, fiber characteristic strength, tensile damage and fracture behavior, and strength distribution in SiC/SiC minicomposites were analyzed. The deposited multilayered (BN/SiC)_n interphase protected the SiC fiber and increased the interface shear stress, fiber characteristic strength, leading to the higher matrix cracking stress, saturation matrix cracking stress, tensile strength and fracture strain.     

Sandwich structure SiCf/Si3N4–SiOC–Si3N4 composites for high-temperature oxidation resistance and microwave absorption

SiC fiber reinforced ceramic matrix composites (SiC_f-CMCs) have been widely used as structural-functional materials at high temperatures. However, their mechanical and electromagnetic wave (EMW) absorbing properties will deteriorate due to high-temperature oxidation. Therefore, unique sandwich structure, consisting of inner Si₃N₄ impedance layer, middle porous SiOC loss layer and dense oxidation-resistant Si₃N₄ layer, was proposed to enhance multiple material properties in oxidation environment. Herein, SiC_f/Si₃N₄–SiOC–Si₃N₄ composites was fabricated by alternating chemical vapor infiltration (CVI) and polymer infiltration pyrolysis (PIP) methods. For these composites, SiC fiber is used as both reinforcing phase and electromagnetic (EM) absorber. CVI Si₃N₄ matrix was distributed in inner and outer layer of the SiC_f/Si₃N₄–SiOC–Si₃N₄ composites. While inner Si₃N₄ layer between BN interphase and SiOC matrix forms nano-heterogeneous interphase to consume EM energy and enhance mechanical properties of composites, outer dense and oxidation-resistant CVI Si₃N₄ coating serves to maintain properties. PIP SiOC matrix exhibits porous structure that can effectively deflect cracks and achieve multiple scattering of EMW. SiC_f/Si₃N₄–SiOC–Si₃N₄ composites with sandwich structure demonstrated excellent EMW absorbing properties and mechanical performance in high-temperature oxidation environments.     

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.     

A high-temperature structural and wave-absorbing SiC fiber reinforced Si3N4 matrix composites

The SiC_f/Si₃N₄ composite with low–high–low permittivity sandwich structure was designed for high-temperature electromagnetic (EM) wave absorption and mechanical stability. The SiC_f/Si₃N₄ possessed the remarkable mechanical properties at room temperature (the flexural strength is 357 ± 16 MPa and the fracture toughness is 10.8 ± 1.7 MPa m^1/2) for the strong fiber strength, moderate interface bonding strength and uniform matrix. Furthermore, the retention rate is as high as 80% at 800 °C. The A/B/C nanostructure and the sandwich meta-structure endowed the SiC_f/Si₃N₄ with an excellent EM absorbing property at room temperature. The SiC_f/Si₃N₄ still absorbed 75% of the incident EM waves energy in X and Ku bands when the temperature increases up to 600 °C, which is only 6% lower than that at room temperature, for the partial compensation of the decreased interfacial polarization loss for the increased conductivity loss and dipole polarization loss.     

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.     

Microstructure and mechanical properties of Si3N4f/BN composites with BN interphase prepared by chemical vapor deposition of borazine

The boron nitride (BN) interphase of silicon nitride (Si₃N₄) fiber-reinforced BN matrix (Si₃N_4f/BN) composites was prepared by chemical vapor deposition (CVD) of liquid borazine, and the microstructure, growth kinetics and crystallinity of the BN coating were examined. The effects of coating thickness on the mechanical strength and fiber/matrix interfacial bonding strength of the composites were then investigated. The CVD BN coating plays a key role in weakening the interfacial bonding condition that improves the mechanical properties of the composites. The layering structure of the BN coating promotes crack propagation within the coating, which leads to a variety of toughening mechanisms including crack deflection, fiber bridging and fiber pull out. Single-fiber push-out experiments were performed to quantify the fiber/matrix bonding strength with different coating thicknesses. The physical bonding strength due to thermal mismatch was discussed.     

Fabrication of Si3N4–SiC/SiO2 composites using 3D printing and infiltration processing

Si₃N₄–SiC/SiO₂ composites were prepared by employing three-dimensional (3D) printing using selective laser sintering (SLS) and infiltration processing. The process was based on the infiltration of silica sol into porous SLS parts, and silicon carbide and silicon nitride particles were bonded by melted nano-sized silica particles. To optimize the manufacturing process, the phase compositions, microstructures, porosities, and flexural strengths of the Si₃N₄–SiC/SiO₂ composites prepared at different heat-treatment temperatures and infiltration times were compared. Furthermore, the effects of the SiC mass fraction and the addition of Al₂O₃ and mullite fibers on the properties of the Si₃N₄–SiC/SiO₂ composites were investigated. After repeated infiltration and heat treatment, the flexural strength of the 3D-printed Si₃N₄–SiC/SiO₂ composite increased significantly to 76.48 MPa. Thus, a Si₃N₄–SiC/SiO₂ composite part with a complex structure was successfully manufactured by SLS and infiltration processes.     

Microstructure and mechanical properties of Si3N4f/Si3N4 composites with different coatings

The Si₃N₄ coating and Si₃N₄ coating with Si₃N₄ whiskers as reinforcement (Si₃N_4w-Si₃N₄) were prepared by chemical vapor deposition (CVD) on two-dimensional silicon nitride fiber reinforced silicon nitride ceramic matrix composites (2D Si₃N_4f/Si₃N₄ composites). The effects of process parameters of as-prepared coating including the preparation temperature and volume fraction of Si₃N_4w on the microstructure and mechanical properties of the composites were investigated. Compared with Si₃N₄ coating, Si₃N_4w-Si₃N₄ coating shows more significant effect on the strength and toughness of the composites, and both strengthening and toughening mechanism were analyzed.     

Porous Si3N4/SiC Ceramics Prepared via Nitridation of Si Powder with SiC Addition

Porous Si₃N₄/SiC ceramics with high porosity were prepared via nitridation of Si powder, using SiC as the second phase and Y₂O₃ as sintering additive. With increasing SiC addition, porous Si₃N₄/SiC ceramics showed high porosity, low flexural strength, and decreased grain size. However, the sample with 20wt% SiC addition showed highest flexural strength and lowest porosity. Porous Si₃N₄/SiC ceramics with a porosity of 36–45% and a flexural strength of 107‐46MPa were obtained. The linear shrinkage of all porous Si₃N₄/SiC ceramics is below 0.42%. This study reveals that the nitridation route is a promising way to prepare porous Si₃N₄/SiC ceramics with favorable flexural strength, high porosity, and low linear shrinkage.     

Toughness and R-curve behaviour of laminated Si3N4/SiCw ceramics

Laminated Si₃N₄/SiC_w ceramics were successfully prepared by tape casting and hot-pressing. Its mechanical properties were measured and the impact resistance was discussed. The toughness of the laminated Si₃N₄/SiC_w ceramics was 13.5 MPa m^1/2, which was almost 1.6 times that of Si₃N₄/SiC_w composite ceramics, namely 8.5 MPa m^1/2. Moreover, the indentation strength of laminated Si₃N₄/SiC_w ceramics was not sensitive to increasing indentation loads and exhibited a rising R-curve behaviour, indicating that the laminated Si₃N₄/SiC_w ceramics had excellent impact resistance. The improved toughness and impact resistance of laminated Si₃N₄/SiC_w ceramics was attributed to the residual stress caused by a thermal expansion coefficient mismatch between the different layers, resulting in crack deflection and bridging of SiC whiskers in the interface layer, thus consuming a large amount of fracture work.     

Processing,characterization and properties of novel gradient Si3N4/SiC fibers derived from polycarbosilanes

In this work, we report a novel kind of Si₃N₄/SiC composite fibers, which exhibit a controlled gradient Si₃N₄(shell)/SiC(core) structure. These composite fibers are fabricated through a controlled nitridation and pyrolysis process on electron irradiation-cured polycarbosilane fibers. Structural and chemical analysis based on Elemental Analyzer, FT-IR, Raman spectroscopy, electron probe micro-analyzer, X-ray photoelectron spectroscopy, and X-ray diffraction confirm the gradient structure of obtained fibers, which consist a shell with high Si₃N₄ content and a SiC core. The as-fabricated fibers exhibit dense and smooth surfaces, and no microscopic holes or defects were observed. The effects of nitridation temperature on mechanical properties and electrical resistivity were also investigated. Combined with high mechanical properties and lightweight, the present gradient Si₃N₄/SiC fibers open a new strategy to fabricate multifunctional and electromagnetic wave absorbing materials.     

Stress distribution around Fe5Si3 and its effect on interface status and mechanical properties of Si3N4 ceramics

Si₃N₄ ceramics with different amount of Fe₅Si₃ were prepared by adding FeSi₂. Residual thermal stress distribution and elastic energy around Fe₅Si₃ particles in various depths were calculated. The interface status between second phase particles and matrix was analyzed in terms of stress and energy. High tangential compressive stresses and low radial tensile stresses were generated along the surface of the ceramics. Elastic strain energy caused by unit interface was high around big particles in deep area of the ceramics. Microcracks are observed around the big Fe₅Si₃ particles. Furthermore, accord to our calculation, microcracks are easily generated around particles in superficial layer of matrix when second phase particles have lower thermal expansion coefficient than the matrix, while microcracks tend to be generated in deep layer of matrix preferentially when the thermal expansion coefficient of second phase particles is higher than matrix. Residual stresses and microcracks around Fe₅Si₃ particles greatly influenced mechanical properties. Fracture toughness of Si₃N₄ ceramics with similar Si₃N₄ particle size distribution increased with the amount of Fe₅Si₃, and fine Fe₅Si₃ particles could enhance the strength of Si₃N₄ ceramics. Si₃N₄ ceramics exceeding 1.2 GPa strength were prepared.     

High-temperature electromagnetic wave absorption properties of Cf/SiCNFs/Si3N4 composites

Carbon fibers reinforced Si₃N₄ composites with SiC nanofiber interphase (C_f/SiCNFs/Si₃N₄) were prepared by combining catalysis chemical vapor deposition and gel-casting process. Microstructures, mechanical properties, and electromagnetic wave absorption properties within X-band at 25°C-800°C of C_f/SiCNFs/Si₃N₄ composites were investigated. Results show that SiC nanofibers are combined well with Si₃N₄ matrix and carbon fibers, the fracture toughness is thus increased more than double from 3.51 MPa·m^1/2 of the Si₃N₄ ceramic to 7.23 MPa·m^1/2 of the as-prepared composites. As the temperature increases from 25°C to 800°C, C_f/SiCNFs/Si₃N₄ composites show a temperature-dependent complex permittivity, attenuation constant, and impedance. The relatively high attenuation capability of C_f/SiCNFs/Si₃N₄ composites at elevated temperature results in a great minimum reflection loss of −20.3 dB at 800°C with a thin thickness of 2.0 mm. The superior electromagnetic wave absorption performance mainly originates from conductive loss, multi-reflection, and strong polarization formed by the combined effects of carbon fibers and SiC nanofibers.     

Structural correlations at Si/Si3N4 interface and atomic stresses in Si/Si3N4 nanopixel-10 million-atom molecular dynamics simulation on parallel computers

We have combined first-principle calculations of charge transfer at the Si/Si₃N₄ interface with the interaction potential models for bulk Si and Si₃N₄ to produce a model for the Si/Si₃N₄ interface. Using these interatomic potentials, million atom molecular dynamics simulations have been performed to characterize the structure of Si(111)/Si₃N₄(0001) and the Si(111)/a-Si₃N₄ interfaces. Ten million-atom simulations are performed using multiresolution molecular-dynamics method on parallel computers. Atomic stress distributions are determined in a 54 nm nanopixel on a 0·1 μm silicon substrate. Effects of surfaces, edges, and lattice mismatch at the Si(111)/Si₃N₄(0001) interface on the stress distributions are also investigated. Stresses are found to be highly inhomogeneous in the nanopixel—the top surface of silicon nitride has a compressive stress of +3 GPa and the stress is tensile, −1 GPa, in silicon below the inter-face. These simulation methods can also be applied to other semiconductor/ceramic interfaces as well as to metal/ceramic and ceramic/ceramic interfaces.     

In situ synthesis of Si2N2O/Si3N4 composite ceramics using polysilyloxycarbodiimide precursors

In situ synthesis of Si₂N₂O/Si₃N₄ composite ceramics was conducted via thermolysis of novel polysilyloxycarbodiimide ([SiOSi(NCN)₃]_n) precursors between 1000 and 1500 °C in nitrogen atmosphere. The relative structures of Si₂N₂O/Si₃N₄ composite ceramics were explained by the structural evolution observed by electron energy-loss spectroscopy but also by Fourier transform infrared and ²⁹Si-NMR spectrometry. An amorphous single-phase Si₂N₂O ceramic with porous structure with pore size of 10–20 μm in diameter was obtained via a pyrolyzed process at 1000 °C. After heat-treatment at 1400 °C, a composite ceramic was obtained composed of 53.2 wt.% Si₂N₂O and 46.8 wt.% Si₃N₄ phases. The amount of Si₂N₂O phase in the composite ceramic decreased further after heat-treatment at 1500 °C and a crystalline product containing 12.8 wt.% Si₂N₂O and 87.2 wt.% Si₃N₄ phases was obtained. In addition, it is interesting that residual carbon in the ceramic composite nearly disappeared and no SiC phase was observed in the final Si₂N₂O/Si₃N₄ composite.