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

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

Fabrication of cylindrical SiCf/Si/SiC-based composite by electrophoretic deposition and liquid silicon infiltration

Cylindrical SiC-based composites composed of inner Si/SiC reticulated foam and outer Si-infiltrated SiC fiber-reinforced SiC (SiC_f/Si/SiC) skin were fabricated by the electrophoretic deposition of matrix particles into SiC fabrics followed by Si-infiltration for high temperature heat exchanger applications. An electrophoretic deposition combined with ultrasonication was used to fabricate a tubular SiC_f/SiC skin layer, which infiltrated SiC and carbon particles effectively into the voids of SiC fabrics by minimizing the surface sealing effect. After liquid silicon infiltration at 1550 °C, the composite revealed a density of 2.75 g/cm³ along with a well-joined interface between the inside Si/SiC foam and outer SiC_f/Si/SiC skin layer. The results also showed that the skin layer, which was composed of 81.4 wt% β-SiC, 17.2 wt% Si and 1.4 wt% SiO₂, exhibited a gastight dense microstructure and the flexural strength of 192.3 MPa.     

Fabrication of the tube-shaped SiCf/SiC by hot pressing

A manufacturing technique for fabricating a dense tubular SiC long fiber-reinforced SiC composite (SiC_f/SiC) by hot pressing was developed. After infiltrating a SiC-based matrix phase, containing a 12 wt% of Al₂O₃–Y₂O₃ sintering additive, into the fine voids of a Tyranno^TM-SA3 SiC fabric preform by electrophoretic deposition combined with the application of ultrasonic pulses, hot pressing was performed using 2 types of specially designed molds filled with graphite powder to transfer the vertical hot press force efficiently to the sidewalls of the tubular SiC_f/SiC. Compared to the low density (~60%) of SiC_f/SiC hot-pressed using a conventional mold, a density >95% could be acquired using a special mold filled with graphite powder as a pressure delivering medium. This method is suitable for fabricating a dense tubular SiC_f/SiC, which cannot be obtained using a conventional extrusion method.     

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 and microstructural characterisation of SiC- and SiBNC-fibre reinforced CMCs manufactured via PIP method before and after exposure to air

Non-oxide CMCs based on pyc-coated SiC-fibres (Tyranno SA3?) as well as novel amorphous ceramic fibres in the quaternary system Si–B–C–N (named SiBNC-fibres) were manufactured via polymer infiltration and pyrolysis process. Two different fibre architectures were applied: 0|90° unidirectional (UD) cross-ply and 0|90° plain weave fabric layer. UD cross-ply reinforced CMCs exhibit much more uniformly distributed filaments leading to better infiltration efficiency in resin transfer moulding process. Bending strength and fracture behaviour are strongly influenced by fibre architecture: UD cross-ply reinforced CMCs show higher bending strengths and less non-linear behaviour compared to plain weave fibre reinforcement. In tensile test there is no evidence of an influence of fibre architecture. Mechanical properties of unexposed SiC_pyc/SiCN and SiBNC_pyc/SiCN strongly correlate with fibre properties. After exposure to air (T = 1100 °C, 20 h), a significant decrease of mechanical properties could be observed, caused by complete oxidation of pyc-fibre coating interfered with silica formation.     

Enhanced mechanical and microwave-absorption properties of SiCf/AlPO4 composite with PIP–SiC interphase and the MWCNTs filler

A single-layer radar-absorbing structure in the X-band (8.2 GHz to 12.4 GHz) was designed and fabricated by blending multi-walled carbon nanotubes (MWCNTs) with the binder matrix of SiC fiber/aluminum phosphate matrix (SiC_f/AlPO₄) composite. The SiC interphase was successfully prepared on SiC fibers by a precursor infiltration and pyrolysis (PIP) method. The morphology of as-received interphase was observed by SEM, and its structure was characterized by XRD and Raman spectrum. The effects of PIP–SiC interphase on the mechanical and dielectric properties of the composite were investigated. The influence of MWCNTs content on the dielectric and microwave-absorption properties of coated SiC_f/AlPO₄ composite was discussed. When the content of MWCNTs was between 1.5 wt% and 3.5 wt% and the composite thickness is in the range of 2.5–3.5 mm, the SiC_f/AlPO₄ composite achieved excellent absorbing wave property in X-band.     

Enhanced microwave-absorbing properties of FeCo magnetic film-functionalized silicon carbide fibers fabricated by a radio frequency magnetron method

Silicon carbide (SiC) fibers have potential application in microwave absorption materials in recent years. In this study, we provide a new method for improving the microwave-absorbing properties of SiC fibers. Magnetic FeCo films were fabricated on SiC fibers at low temperature and high vacuum by a radio frequency magnetron sputtering method. The properties of FeCo film/SiC fiber (FeCo/SiC_f) composites were investigated. When compared with SiC fiber, the FeCo/SiC_f composites exhibit excellent microwave-absorbing properties in the microwave range, with enhancements in the optimal reflectivity loss from −5.03 to −25.51 dB. This excellent performance may be because of the magnetic loss due to ferromagnetic resonance and interfacial polarization, thus inducing dielectric relaxation. In addition, the magnetic properties of FeCo/SiC_f composites are significantly improved: the value of saturation magnetization reaches up to 41.45 emu/g and the coercivity is 116.27 Oe. In addition, the strength of SiC fiber remains at 99.17% after the fabrication process. The method provided in this study for enhancing the microwave-absorbing properties of FeCo/SiC_f composites will pave a new way for the development of SiC microwave-absorbing materials.     

Effect of oxidation treatment on KD–II SiC fiber–reinforced SiC composites

Continuous silicon carbide fiber–reinforced silicon carbide matrix (SiC_f/SiC) composites have developed into a promising candidate for structural materials for high–temperature applications in aerospace engine systems. This is due to their advantageous properties, such as low density, high hardness and strength, and excellent high temperature and oxidation resistance. In this study, SiC_f/SiC composites were fabricated via polymer infiltration and pyrolysis (PIP) with the lower–oxygen–content KD–II SiC fiber as the reinforcement; a mixture of 2,4,6,8–tetravinyl–2,4,6,8–tetramethylcyclotetrasiloxane (V4) and liquid polycarbosilane (LPCS), known as LPVCS, was used as the precursor; while pyrolytic carbon (PyC) was used as the interface. The effects of oxidation treatment at different temperatures on morphology, structure, composition, and mechanical properties of the KD–II SiC fibers, SiC matrix from LPVCS precursor conversion, and SiC_f/SiC composites were comprehensively investigated. The results revealed that the oxidation treatment greatly impacted the mechanical properties of the SiC fiber, thereby significantly influencing the mechanical properties of the SiC_f/SiC composite. After oxidation at 1300 °C for 1 h, the strength retention rates of the fiber and composite were 41% and 49%, respectively. In terms of the phase structure, oxidation treatment had little effect on the SiC fiber, while greatly influencing the SiC matrix. A weak peak corresponding to silica (SiO₂) appeared after high–temperature treatment of the fiber; however, oxidation treatment of the matrix led to the appearance of a very strong diffraction peak that corresponds to SiO₂. The analysis of the morphology and composition indicated cracking of the fiber surface after oxidation treatment, which was increasingly obvious with the increase in the oxidation treatment temperature. The elemental composition of the fiber surface changed significantly, with drastically decreased carbon element content and sharply increased oxygen element content.     

Effects of post-sintering annealing on the microstructure and toughness of hot-pressed SiCf/SiC composites with Al2O3-Y2O3 additions

This study examined the effects of post-sintering heat treatment on enhancing the toughness of SiC_f/SiC composites. Commercially available Tyranno^® SiC fabrics with contiguous dual ‘PyC (inner)-SiC (outer)’ coatings deposited on the SiC fibers were infiltrated with a SiC + 10 wt% Al₂O₃-Y₂O₃ slurry by electrophoretic deposition. SiC green tapes were stacked between the slurry-infiltrated fabrics to control the matrix volume fraction. Densification of approximately 94% ρ_theo was achieved by hot pressing at 1750 °C, 20 MPa for 2 h in an Ar atmosphere. Sintered composites were then subjected to isothermal annealing treatment at 1100, 1250, 1350, and 1750 °C for 5 h in Ar. The correlation between the flexural behavior and microstructure was explained in terms of the in situ-toughened matrix, phase evolution in the sintering additive, role of dual interphases and observed fracture mechanisms. Extensive fractography analysis revealed interfacial debonding at the hybrid interfaces and matrix cracking as the key fracture modes, which were responsible for the toughening behavior in the annealed SiC_f/SiC composites.     

Reactive brazing Cf/SiC to itself and to Mo using the NiPdPtAu-Cr filler alloy

The NiPdPtAu-Cr filler alloy was proposed for joining C_f/SiC composites. The wettability on C_f/SiC composite was studied by the sessile drop method at 1200 °C for 30 min. Under the brazing condition of 1200 °C for 10 min, the C_f/SiC-C_f/SiC joint strength was only 51.7 MPa at room temperature. However, when used a Mo layer, the C_f/SiC-Mo-C_f/SiC joint strength was remarkably increased to 133.2 MPa at room temperature and 149.5 MPa at 900 °C, respectively. At the interface between C_f/SiC and Mo, Mo participated in interfacial reactions, with the formation of Cr₃C₂/Mo₂C reaction layers at the C_f/SiC surface. The improvement in the joint strength should be mainly attributed to the formation of MoNiSi. The C_f/SiC-Mo joint strength was 86.9 MPa at room temperature and 73.7 MPa at 900 °C, respectively. After 10 cycles of thermal shock test at 900 °C the C_f/SiC-Mo joint strength of 71.6 MPa was still maintained.     

Crystallization of SiC and its effects on microstructure,hardness and toughness in TaC/SiC multilayer films

A series of TaC/SiC multilayer films with different SiC thicknesses (t_SiC) have been prepared by magnetron sputtering and their microstructure, hardness and toughness investigated by X-ray diffraction (XRD), transmission electron microscopy (TEM), atomic force microscopy (AFM), scanning electron microscopy (SEM) and nanoindentation. Results show that SiC crystallized and grew coherently with TaC layers at low t_SiC (≤ 0.8 nm), resulting from the template effect of TaC layers. Maximum hardness and toughness of 46.06 GPa and 4.21 MPa m^1/2 were achieved at t_SiC = 0.8 nm with good coherent interface. With further increasing of t_SiC, SiC layers partially transformed to an amorphous structure and gradually lost their coherent interface, leading to a rapid drop in hardness and toughness. The crystallization of SiC layers and the coherent growth are required to achieve superhardness and high toughness in the TaC/SiC multilayers.     

Highly conductive and high-strength carbon nanotube film reinforced silicon carbide composites

Film formed by carbon nanotubes is usually called carbon nanotube film (CNT_f). In the present study, CNT_f fabricated by floating catalyst method was used to prepare CNT_f/SiC ceramic matrix composites by chemical vapor infiltration (CVI). Mechanical and electrical properties of the resulting CNT_f/SiC composites with different CVI cycles were investigated and discussed, and the results revealed that the CNT_f has a good adaptability to CVI method. Tensile test demonstrated an excellent mechanical performance of the composites with highest tensile strength of 646 MPa after 2 CVI cycles, and the strength has a decline after 3 CVI cycles for an excessively dense matrix. While, the elastic modulus of the composite increased with the CVI cycles and reached 301 GPa after 3 CVI cycles. Tensile fracture morphologies of the composites were analyzed by scanning electron microscope to study the performance change laws with the CVI cycles. With SiC ceramic matrix infiltrated into the CNT_f, enhanced electrical conductivity of the CNT_f/SiC composite compared to pure CNT_f was also obtained, from 368 S/cm to 588 S/cm. Conductivity of the SiC matrix with free carbon forming in the CVI process was considered as the reason.     

Influence of different matrices on the mechanical and microwave absorption properties of SiC fiber-reinforced oxide matrix composites

Fiber-reinforced ceramic matrix composites have excellent mechanical and microwave absorption properties, but still present considerable challenges. We prepared a SiC_f/mullite-SiO₂ composite (composite A) and a SiC_f/Al₂O₃-SiO₂ composite (composite B) by a precursor infiltration and sintering (PIS) process. Compared with the composite B, the composite A was easily densified. The flexural strength of the composite A reached 216 MPa, whereas that of the composite B was 159 MPa. The imaginary part of permittivity for composites A and B, which was determined by the contents of matrix and porosity, varied in the range of 2.5–3.5 and 3.6–5, respectively. The microwave absorption properties of the composite A were significantly enhanced in the range of 8.2–12.4 GHz. The results indicate that an optimal reflection loss of ?44 dB was reached at 12 GHz with a thickness of 2.9 mm for the composite A. These SiC fiber-reinforced oxide matrix materials have promising applications in microwave absorption, especially at high temperatures.     

The effects of preparation temperature on the SiCf/SiC 3D4d woven composite

Continuous silicon carbide fiber reinforced silicon carbide matrix (SiC_f/SiC) composites have promising applications in aero-engine due to their unique advantages, such as low density, high modulus and strength, outstanding high temperature resistance and oxidation resistance. As SiC fibers are main reinforcements in SiC_f/SiC composites, the crystallization rate and initial damage degree of SiC fibers are seriously influenced by preparation temperatures of SiC_f/SiC composites, namely mechanical properties of SiC fibers and SiC_f/SiC composites are influenced by preparation temperatures. In this paper, KD-II SiC fibers were woven into 3D4d preforms and SiC matrix was fabricated by PIP process at 1100 °C, 1200 °C, 1400 °C and 1600 °C. Digital image correlation (DIC) method was adopted to measure the uniaxial tensile properties of these SiC_f/SiC composites. In addition, finite element method (FEM) based on representative volume element (RVE) was adopted to predict the mechanical properties of SiC_f/SiC composites. The good agreements between numerical results and experimental results of uniaxial tensile tests verified the validity of the RVE. In last, the transverse tensile, transverse shear, uniaxial shear properties were predicted by this method. The predicted results illustrated that axial tensile, transverse tensile and axial shear properties were greatly influenced by the preparation temperatures of SiC_f/SiC composites while transverse shear properties were not significantly various. And the mechanical properties of SiC_f/SiC composites peaked at 1200 °C among these four temperatures while their values reached their lowest points at 1600 °C because of thermal damage and brittle failure of SiC_f/SiC composites.     

Preparation and characterization of ZrB2 and TaC containing Cf/SiC composites via Polymer-Infiltration-Pyrolysis process

To improve the thermo-chemical resistance of PIP–C_f/SiC composites, the SiC matrix is modified by adding ZrB₂ and Ta powder to the pre-ceramic slurry to form C_f/SiC–ZrB₂–TaC composites. Within this study the modified composites are investigated regarding their microstructure, chemical composition and physical properties (density = 2,39–2,72 g/cm³; porosity = 20,3–24,8 vol.-%; fiber volume content = 52–57 vol.-%). Mechanical properties are investigated in order to ensure that there is no negative influence by ZrB₂ and TaC matrix modification. The matrix modification is followed by an improvement in bending strength (up to 27% increase), Young’s modulus (up to 28% increase) and for interlaminar shear strength (up to 22% increase). Finally the thermo-chemical behavior of the C_f/SiC–ZrB₂–TaC composites is evaluated in a combustion chamber-like environment using the Airbus Group long-term material test facility (Environmental Relevant Burner Rig-Kerosene, ERBURIG^K). The results show that the thermo-chemical resistance of C_f/SiC–ZrB₂–TaC composites is improved and the oxygen permeability through the composite is decreased (from 5 to 1 layer).     

Fabrication of laminated SiCw/SiC ceramic composites by CVI

Laminated SiC_w/SiC ceramic composites were prepared by chemical vapor infiltration (CVI) and tape casting, and the advantages of this method were investigated. The results showed that this method can increase strength of the composites by reducing the damage of SiC whiskers and increasing their volume fraction, and increase toughness of the composites by controlling the interfacial bonding between whiskers and matrix and inter-laminar bonding between layers. The volume fraction of whiskers reached 40 vol.%, and the flexural strength, tensile strength and fracture toughness were 315 MPa, 158 MPa and 8.02 MPa m^1/2, respectively. Interfacial and interlaminar crack deflection and bridging were observed.     

Microstructure and mechanical properties of SiC-SiC joints joined by spark plasma sintering

The development of reliable joining technology is of great importance for the full use of SiC. Ti₃SiC₂, which is used as a filler material for SiC joining, can meet the demands of neutron environment applications and can alleviate residual stress during the joining process. In this work, SiC was joined using different powders (Ti₃SiC₂ and 3Ti/1.2Si/2C/0.2Al) as filler materials and spark plasma sintering (SPS). The influence of the joining temperature on the flexural strength of the SiC joints at room temperature and at high temperatures was investigated. Based on X-ray diffraction and scanning electron microscopy analyses, SiC joints with 3Ti/1.2Si/2C/0.2Al powder as the filler material possess high flexural strengths of 133 MPa and 119 MPa at room temperature and at 1200 °C, respectively. The superior flexural strength of the SiC joint at 1200 °C is attributed to the phase transformation of TiO₂ from anatase to rutile.     

Improvement of high-temperature stability of PIP SiCf/SiC material through in situ grown BNNTs

In this paper, the effect of in situ grown boron nitride nanotubes (BNNTs) and preparation temperature on mechanical behavior of PIP (Precursor Infiltration and Pyrolysis) SiC_f/SiC minicomposites under monotonic and compliance tensile is investigated. In situ BNNTs are grown on the surface of SiC fibers using ball milling–annealing process. Composite elastic modulus, tensile strength, fracture strain, tangent modulus, and loading/unloading inverse tangent modulus (ITM) are obtained and adopted to characterize the mechanical properties of the composites. Microstructures of in situ grown BNNTs and tensile fracture surfaces are observed under scanning electronic microscopic (SEM). For SiC_f/SiC minicomposites with BNNTs, the elastic modulus, tensile strength, and fracture strain are all lower than those of SiC_f/SiC minicomposites without BNNTs, mainly due to high preparation temperature and the oxidation of the PyC interphase during the annealing process. Tensile stress–strain curves of SiC_f/SiC minicomposites with and without BNNTs are predicted using the developed micromechanical constitutive model. The predicted results agreed with experimental data. This work will provide guidance for predicting the service life of SiC_f/SiC composite materials and may enable these materials to become a backbone for thermal structure systems in aerospace applications.     

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.     

Oxidation and thermal shock resistant properties of Al-modified environmental barrier coating on SiCf/SiC composites

SiC_f/SiC ceramic matrix composites (CMCs) are being widely used in the hot-sections of gas-turbines, especially for aerospace applications. These CMCs are subjected to surface recession if exposed to heat-corrosion. In this research, an alternative environmental barrier coating (EBC) is introduced to protect the SiC_f/SiC CMC from high temperature degradation that is, Al film was deposited on the surface of SiC_f/SiC CMC followed by heat-treatment in a vacuum. After that, a dense Al₂O₃ overlay was in-situ synthesized on the surface of CMC, and in this process the microstructure evolution of SiC_f/SiC CMC was analyzed. The oxidation and thermal shock resistance were characterized, showing that the Al-modified SiC_f/SiC CMC has a better oxidation resistance, because the dense Al₂O₃ overlay can hinder oxygen diffusion from environment. What is more, the water-quenching testes show that the Al-modified SiC_f/SiC CMC has a good spallation resistance.