Microstructure and mechanical properties of hot-pressed SiC nanofiber reinforced SiC composites

This study reports on the preparation and mechanical properties of a novel SiC_nf/SiC composite. The single crystal SiC nanofiber(SiC_nf) reinforced SiC ceramic matrix composites (CMC) were successfully fabricated by hot pressing the mixture of β-SiC powders, SiC_nf and Al–B–C powder. The effects of SiC_nf mass fraction as well as the hot-pressing temperature on the microstructure and mechanical properties of SiC_nf/SiC CMC were systematically investigated. The results demonstrated that the 15 wt% SiC_nf/SiC CMC obtained by hot pressing (HP) at 1850 °C with 30 MPa for 60 min possessed the maximum flexural strength and fracture toughness of 678.2 MPa and 8.33 MPa m^1/2, respectively. The nanofibers pull out, nanofibers bridging and cracks deflection were found by scanning electron microscopy, which are believed can strengthen and toughen the SiC_nf/SiC CMC via consuming plenty of the fracture energy. Besides, although the relative density of the prepared SiC_nf/SiC CMC further increased with the sintering temperature rose to 1900 °C, the further coarsend composites grains results in the deterioration of the mechanical properties for the obtained composites compared to 1850 °C.     

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.     

Nanoscale toughening of low carbon Al2O3-C refractories by means of SiCnw/Al2O3 composite reinforcement

To improve the thermal shock resistance of low carbon Al₂O₃-C refractories, SiC nanowires (SiC_nw) containing SiC_nw/Al₂O₃ composite reinforcement were introduced. The specific fracture energy of the Al₂O₃-C refractory matrix was obtained by statistical grid nano-indentation. The reinforcement mechanism of SiC_nw/Al₂O₃ on thermal shock resistance of refractories was investigated. The results revealed that the matrix-specific fracture energy of A6 (6 wt% SiC_nw/Al₂O₃ added) was 217 N/m, which was 58.4% higher than reference sample A0 (137 N/m) and 18.6% higher than MA6 (183 N/m, 6 wt% SiC/Al₂O₃ added). A6 showed the highest residual strength ratio of 49.8%, which was 114.7 % higher than A0 (23.2%) and 82.4 % higher than MA6 (27.3%). The components with different morphology in SiC_nw/Al₂O₃ cluster, especially SiC nanowires, promote the generation of microcracks, crack multi-deflection, and branching, which toughen the matrix and improve the thermal shock resistance of refractories. In comparison to the literature, A6 showed a higher rising in residual strength ratio than those with higher graphite content (4 wt% and 20 wt%), which will greatly reduce the consumption of carbon-containing refractories and contribute to the reduction of CO₂ emission.     

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.     

Enhanced fracture properties of ZrB2-based composites by in-situ grown SiC nanowires

To improve the fracture properties of ZrB₂-based composites, SiC nanowires (SiC_nw) were introduced into the powder mixtures via an in-situ growth method and the composites were fabricated by hot pressing. Microstructure observations found that the SiC_nw with a diameter of less than 100?nm presented twisted morphology and homogeneously distributed among ceramic particles. It was also found that the SiC_nw could inhibit the grain growth of ZrB₂-based composites. Compared to that of composites without SiC_nw, the fracture toughness and the work of fracture for the composites with SiC_nw were 7.17?MPa?m^1/2 and 205?J?m^?2, which increased by 61.1% and 91.6%, respectively. The main enhancing mechanisms could be associated with the obvious crack deflection, crack branching and pull out of SiC_nw. The SiC_nw could refrain the crack opening and reduce the stress intensity in front of crack tips, which absorbed more energy and improved the fracture properties.     

Effects of SiC whiskers on the mechanical properties and microstructure of SiC ceramics by reactive sintering

As-received and pre-coated SiC whiskers (SiC_w)/SiC ceramics were prepared by phenolic resin molding and reaction sintering at 1650 °C. The influence of SiC_w on the mechanical behaviors and morphology of the toughened reaction-bonded silicon carbide (RBSC) ceramics was evaluated. The fracture toughness of the composites reinforced with pre-coated SiC_w reached a peak value of 5.6 MPa m^1/2 at 15 wt% whiskers, which is higher than that of the RBSC with as-received SiC_w (fracture toughness of 3.4 MPa m^1/2). The surface of the whiskers was pre-coated with phenolic resin, which could form a SiC coating in situ after carbonization and reactive infiltration sintering. The coating not only protected the SiC whiskers from degradation but also provided moderate interfacial bonding, which is beneficial for whisker pull-out, whisker bridging and crack deflection.     

The influence of different SiC amounts on the microstructure,densification, and mechanical properties of hot-pressed Al2O3-SiC composites

The hot pressing process of monolithic Al₂O₃ and Al₂O₃-SiC composites with 0-25 wt% of submicrometer silicon carbide was done in this paper. The presence of SiC particles prohibited the grain growth of the Al₂O₃ matrix during sintering at the temperatures of 1450°C and 1550°C for 1 h and under the pressure of 30 MPa in vacuum. The effect of SiC reinforcement on the mechanical properties of composite specimens like fracture toughness, flexural strength, and hardness was discussed. The results showed that the maximum values of fracture toughness (5.9 ± 0.5 MPa.m^1/2) and hardness (20.8 ± 0.4 GPa) were obtained for the Al₂O₃-5 wt% SiC composite specimens. The significant improvement in fracture toughness of composite specimens in comparison with the monolithic alumina (3.1 ± 0.4 MPa.m^1/2) could be attributed to crack deflection as one of the toughening mechanisms with regard to the presence of SiC particles. In addition, the flexural strength was improved by increasing SiC value up to 25 wt% and reached 395 ± 1.4 MPa. The scanning electron microscopy (SEM) observations verified that the increasing of flexural strength was related to the fine-grained microstructure.     

Fabrication and mechanical properties of carbon fibers/lithium aluminosilicate ceramic matrix composites reinforced by in-situ growth SiC nanowires

To improve the mechanical properties of carbon fibers/lithium aluminosilicate (C_f/LAS) composites, C_f/LAS with in-situ grown SiC nanowires (SiC_nw-C_f/LAS) were prepared by chemical vapor phase reaction, precursor impregnation, and hot press sintering, consecutively. The effect of multi-scaled reinforcements (micro-scaled C_f and nano-scaled SiC_nw) on the mechanical properties was investigated. The phase composition, microstructure and fracture surface of the composites were characterized by XRD, Raman Spectrum, SEM, and TEM. The morphology of SiC_nw has a close relation with the content of Si. Microstructure analysis suggests that the growth of SiC nanowires depends on the VLS mechanism. The multi-scale reinforcement formed by C_f and SiC_nw can significantly improve the mechanical properties of C_f/LAS. The bending strength of SiC_nw-C_f/LAS reaches to 597 MPa, achieving an increase of 19% to C_f/LAS. Moreover, the samples show a maximum fracture toughness of 11.01 MPa m^1/2, achieving an increase of 46.4% to C_f/LAS. Through analysis of the fracture surface, the improved mechanical properties could be attributed to the multi-scaled reinforcements by the pull-out and debonding of C_f and SiC_nw from the composites.     

Combustion synthesis of SiC-based ceramics reinforced by discrete carbon fibers with in situ grown SiC nanowires

This study proposes a combustion-based ceramic matrix composite processing technique intended on single-step in situ deposition of single-crystal SiC nanowires (SiC_nw) on the surface of carbon fibers (C_f) and formation of SiC_nw–reinforced SiC matrix. This was accomplished by Ta-catalyzed combustion of poly-(C₂F₄)-containing reactive mixtures with pre-mixed chopped C_f. Depending on the combustion conditions, carbon fiber surface is subjected either to formation of diffusion layers, ceramic particle incrustation or growth of continuous arrays of carbon-coated single-crystal SiC_nw with a nearly defect-free lattice, 10–50 nm diameter and 15–20 μm length. Thermodynamics, phase and structure formation mechanisms are explored, and the optimal conditions are outlined for reproducible C_f/in situ SiC_nw dual reinforcement of SiC-based ceramics. Hot pressing at 1500 °C produced C_f/in situ SiC_nw-reinforced ceramic SiC–TaSi₂ specimens with a relative density of 97%, 19 GPa Vickers hardness, 3-point flexural strength σ = 420 ± 70 MPa and fracture toughness K_1C = 12.5 MPa m^1/2.     

Processing and properties of polycrystalline cubic boron nitride reinforced by SiC whiskers

Dense polycrystalline cBN (PcBN)–SiCw composites were fabricated by a two-step method: First, SiO₂ was coated on the surface of cubic boron nitride (cBN) particles by the sol-gel method. Then, silicon carbide whisker (SiC_w)- coated cBN powder was prepared by carbon thermal reaction between SiO₂ and carbon powders at 1500°C for 2 hour. Then, cBN–SiC_w complex powders were sintered by high-pressure and high-temperature sintering technology using Al, B, and C as sintering additives. The phase compositions and microstructures of cBN–SiC_w composites were investigated by X-ray diffraction and scanning electron microscopy, respectively. It was found that the SiC_w and Al₃BC₃ had been fabricated by in situ reaction, which cannot only promote densification but also improve mechanical properties. The relative density of PcBN composites increased from 96.3% to 99.4% with increasing SiC_w contents from 5 to 20 wt%. Meanwhile, the Vickers hardness, fracture toughness and flexural strength of as-obtained composites exhibited a similar trend as that of relative density. The composite contained 20 wt% of SiC_w exhibited the highest Vickers hardness and fracture toughness of 42.7 ± 1.9 GPa and 6.52 ± 0.21 MPa•m^1/2, respectively. At the same time, the flexural strength reached 406 ± 21 MPa.     

Improved mechanical properties of reaction-bonded SiC through in-situ formation of Ti3SiC2

Reaction-bonded SiC is a ceramic with excellent thermal properties, good corrosion resistance and the characteristic of near-net-shape manufacturing. However, the poor fracture toughness of free Si limits the applications of reaction-bonded SiC. In this study, TiC was added to reaction-bonded SiC and reacted with free Si to form Ti₃SiC₂. The effects of TiC and carbon black on the mechanical properties of reaction-bonded SiC were investigated. The results demonstrated that the in-situ formation of Ti₃SiC₂ and decrease in the content and size of free Si improved the mechanical properties of reaction-bonded SiC ceramics. The mechanical properties of TiC-added reaction-bonded SiC with 17.5 wt% carbon black were superior to those of TiC-added reaction-bonded SiC with 15 wt% carbon black. Moreover, increasing the TiC content of reaction-bonded SiC with 17.5 wt% carbon black from 0 to 7.5 wt% caused an increase in its bending strength from 183.92 to 424.43 MPa and an increase in fracture toughness from 3.7 to 5.24 MPa m^1/2.     

Developing high performance in titanium carbide nanocomposites containing hybrid SiC nanowire and CNT

Lightweight titanium carbide (TiC) has garnered considerable engineering applications in various advanced manufacturing industries. However, the intrinsic brittleness of TiC significantly limited its further applications. High-toughness and damage-tolerance TiC is always highly desirable for industry. Herein, we developed high-performance TiC nanocomposites reinforced by hybrid carbon nanotube (CNT) and SiC nanowire (SiC_nw) through two-step spark plasma sintering, highlighting the synergic role of CNT and SiC_nw on the microstructure and properties of the TiC matrix. Specifically, CNT was helpful in maintaining the high aspect ratio of SiC_nw during the sintering process, while SiC_nw contributed to the homogeneous distribution of CNT throughout the TiC matrix. The flexural strength and fracture toughness were simultaneously enhanced by 48.1% and 56.9% in case of CNT/SiC_nw ratio of 1:2 comparing with pure TiC, respectively. This study provided the new insight on developing high-performance TiC materials.     

The effect of oxide,carbide, nitride and boride additives on properties of pressureless sintered SiC: A review

Properties such as high hardness, low density, and high elastic modulus have made SiC ceramics proper choices for a variety of industrial applications. However, disadvantages such as low sinterability, and low fracture toughness have limited the fabrication of these ceramics. Past researches show that the use of Al₂O₃-Y₂O₃ additives play an important role in improving the sinterability and the properties of the composites. The use of oxide, carbide, nitride and boride additives results in improved sinterability, physical and mechanical properties. The investigations show that the microstructure, porosities, amount of additives, reaction of additives with the matrix, grain size and, finally, the sintering temperature are the most important factors affecting the properties of SiC ceramics. In this paper, the effect of using various additives, the sintering temperature and the annealing heat treatment on sinterability, microstructure and properties of the SiC matrix composites fabricated by pressureless sintering method have been investigated.     

Effects of SiC nanowires and whiskers on high-entropy carbide-based composites sintered at low and high temperatures

This study aimed to investigate the toughening effects of SiC nanowires (SiC_nw) and SiC whiskers (SiC_w) on high-entropy carbide based composites prepared at different temperatures (1600°C and 2000°C). At low temperature (1600°C), SiC_nw and SiC_w maintain their original morphology and properties, and exhibit the good toughening effects. The SiC_nw with larger aspect ratio and more curly wires exhibit a much stronger toughening effect on the (Ti_0.2Zr_0.2Nb_0.2Ta_0.2Mo_0.2)C_0.8 composites reinforced with 15 vol.% SiC_nw, which shows the highest value of fracture toughness about 6.7 MPa∙m^1/2. However, at high sintering temperature (2000°C), SiC_nw and SiC_w are prone to thermal-induced damages, which significantly reduces their mechanical properties, and thus, toughening effects on (Ti_0.2Zr_0.2Nb_0.2Ta_0.2Mo_0.2)C_0.8 composites. The addition of SiC_w, which have better thermal stability at 2000°C, results in the (Ti_0.2Zr_0.2Nb_0.2Ta_0.2Mo_0.2)C_0.8–15 vol.% SiC_w composite exhibiting relatively better fracture toughness, about 3.7 MPa∙m^1/2. Based on the results of the current study, the critical influence of SiC_nw and SiC_w on the toughening of (Ti_0.2Zr_0.2Nb_0.2Ta_0.2Mo_0.2)C_0.8 composites is highly dependent on their high-temperature thermal stability.     

Comparison of the proton irradiation-induced damage in SiCf/SiC with Sc-nitrate and Al2O3-Y2O3 sintering additives

We report microstructural evaluation in proton-irradiated SiC_f/SiC up to a fluence level of 10¹⁸?p⁺/m² (E?=?20?MeV) performed at the Korea Multi-purpose Accelerator Complex (KOMAC). To fabricate the SiC_f/SiC, a SiC-based matrix with two different sintering additives, Sc-nitrate and Al₂O₃-Y₂O₃, were infiltrated into the Tyranno^® SiC preform by electrophoretic deposition and subsequent hot pressing. Scanning (SEM) and high resolution (HREM) electron microscopy was used to probe crack formation, pore generation and surface amorphization upon irradiation. SiC matrix was comparatively more crack-resistant in the SiC_f/SiC with Sc-nitrate than that with Al₂O₃-Y₂O₃. Subsurface porosity evolved in the form of continuous bands for Al₂O₃-Y₂O₃ and discrete pockets for Sc-nitrate additives. Selective leaching of Si from the grain surface leads to the formation of a graded structure and surface amorphization. Irradiation-induced roughness on the fibers facilitates easy debonding at the SiC_f-PyC_coating interface but no significant changes in the flexural behavior were observed.     

Preparation of SiC/SiC composites with high toughness by reaction of the SiCP+C double-cladding layer with liquid silicon

SiC/SiC composites prepared by liquid silicon infiltration (LSI) have the advantages of high densification, matrix cracking stress and ultimate tensile strength, but the toughness is usually insufficient. Relieving the residual microstress in fiber and interphase, dissipating crack propagation energy, and improving the crystallization degree of interphase can effectively increase the toughness of the composites. In this work, a special SiC particles and C (SiC_P +C) double-cladding layer is designed and prepared via the infiltration of SiC_P slurry and chemical vapor infiltration (CVI) of C in the porous SiC/SiC composites prepared by CVI. After LSI, the SiC generated by the reaction of C with molten Si combines with the SiC_P to form a layered structure matrix, which can effectually relieve residual microstress in fiber and interphase and dissipate crack propagation energy. The crystallization degree of BN interphase is increased under the effects of C-Si reaction exotherm. The as-received SiC/SiC composites possess a density of 2.64 g/cm³ and a porosity of 6.1%. The flexural strength of the SiC/SiC composites with layered structure matrix and highly crystalline BN interphase is 577 MPa, and the fracture toughness reaches up to 37 MPa·m^1/2. The microstructure and properties of four groups of SiC/SiC composites prepared by different processes are also investigated and compared to demonstrate the effectiveness of the SiC_P +C double-cladding layer design, which offers a strategy for developing the SiC/SiC composites with high performance.     

Effects of SiC amount and morphology on the properties of TiB2-based composites sintered by hot-pressing

This investigation intended to assess the influence of SiC morphology on the sinterability and physical-mechanical features of TiB₂-SiC composites. For this aim, different volume percentages of SiC particles and SiC whiskers were introduced to TiB₂ samples hot-pressed at 1950 °C for 2 h under an external pressure of 25 MPa. The characterization of as-sintered specimens was carried out using X-ray diffraction, optical microscopy, and scanning electron microscopy. The relative density studies revealed that SiC_w had a more significant impact on the sinterability of TiB₂-based composites. The XRD investigation confirmed the production of an in-situ TiC phase during the hot-pressing; however, some peaks related to the graphitized carbon also appeared in the patterns of SiC_w-doped ceramics. The addition of 25 vol% SiC_p halved the average grain size of TiB₂ while introducing the same content of SiC_w decreased this value by just around 20%. Finally, the highest Vickers hardness and fracture toughness were obtained for the sample reinforced with 25 vol% SiC_w, standing at 29.3 GPa and 6.1 MPa m^1/2, respectively.     

Preparation,mechanical, dielectric and microwave absorption properties of hierarchical porous SiCnw-Si3N4 composite ceramics

Herein, hierarchical porous SiC_nw-Si₃N₄ composite ceramics with good electromagnetic absorption properties were prepared. A porous Si₃N₄ matrix with different pore structures was first prepared by gelcasting-pressureless sintering (G-PLS) and gelcasting combined with particle stabilized foam-pressureless sintering (G-PSF-PLS). SiC_nw was then introduced by catalytic chemical vapor deposition (CCVD). An increase in solid loading (25–40 vol%) decreased apparent porosity (47.7–41.3%) and improved flexural strength (142.19–240.36 MPa) and fracture toughness (2.25–3.68 MPa·m^1/2). The addition of foam stabilizer propyl gallate (PG, 0.5–1.0 wt%) significantly increased apparent porosity (73.2–86.4%) and realized large-sized spherical pores, reducing flexural strength (58.23–38.56 MPa) and fracture toughness (0.75–0.41 MPa·m^1/2). High apparent porosity and large-sized pores facilitated the introduction of SiC_nw. The 25 vol% sample exhibited a reflection loss of ? 14.67 dB with an effective absorption bandwidth of 3.47 GHz, suggesting a development potential in the electromagnetic wave absorption field.     

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.     

Joining of SiC ceramics by combining NITE-SiC interlayer and its thickness control

Combined with the thickness control of interlayers (∼10 µm and ∼60 µm), SiC nano-powders with Al₂O₃-Y₂O₃-MgO-CaO additive (NITE-SiC) were used as the joining materials to achieve the low-temperature joining of SiC ceramics. Some residual pores were observed in the interlayer with a thickness of ∼60 µm after joining at 1650 ℃, and the shear strength of SiC joints measured was 39.3 ± 5.5 MPa. Observations showed the fracture of joints occurred at the interlayer. When the thickness of the interlayer decreased to ∼10 µm, no cracks or porosity were observed at the interface region after joining at 1650 ℃. The shear strength of SiC joints increased to 69.5 ± 8.9 MPa, and the fracture originated from the matrix. The results demonstrated using NITE-SiC with Al₂O₃-Y₂O₃-MgO-CaO additive as the joining layer and reducing the thickness of the interlayer could lower the joining temperature and significantly improve the mechanical strength of joints.