A novel cost-effective and near-net-shape fabrication process for SiO2f/SiO2 composites

In this study, we present a novel preparation process named vacuum-assisted slurry infiltration (VASI) for obtaining the SiO_2 f/SiO₂ composites. This method displays remarkably improvement in manufacturing cycles since it allows adopt the ceramic slurries with high solid content as well as low viscosity. Through the porous matrix design of combining coarse particles with fine particles, a homogeneous porous matrix is achieved. The SiO_2 f/SiO₂ composites prepared by the VASI method exhibit the rivaling flexural and tensile strength at 48.8 and 16.4 MPa, respectively. Meanwhile, such porous matrix can enable cracks deflecting and dissipating crack energy by fiber pullout and fiber debonding mechanisms. In comparison, composites fabricated via silica sol infiltration show lower mechanical properties and brittle fracture behavior due to the formation of some defects in the matrix. This work make the prospect for meeting the requirements of low-cost, short preparation cycles, and near-net-shape manufacturing technology for SiO_2 f/SiO₂ composites becomes realizable.     

Effects of particle size in silica sol on the mechanical and thermal properties of SiO2f/SiO2 composites

In this paper, quartz fiber-reinforced silica matrix SiO_2f/SiO₂ composites were prepared by the precursor impregnation-heat treatment method using quartz fiber needle felt as the reinforcement and silica sol as the precursor. The effects of particle size in silica sol (10, 50, and 100 nm) on the density, apparent porosity, mechanical properties, and thermal properties of SiO_2f/SiO₂ composites were investigated. The phase composition and microstructure of the composites were characterized by X-ray diffraction and scanning electron microscopy, respectively. The thermal expansion coefficient and thermal conductivity of composites were measured by a push rod method and the laser method. The results show that the density, apparent porosity, and mechanical strength of the specimens firstly increase and then decrease with the increase in the particle size in silica sol. The sample using silica sol with particle size 50 nm has the optimum overall performances (i.e., the flexural strength of 13.7 MPa and the compressive strength of 59.8 MPa), and shows a ductile fracture behavior. At 300°C–700°C, the average thermal expansion coefficient of the optimal sample is .783 × 10⁻⁶/°C. And the thermal conductivity of the samples increases with the increase in temperature, and it reached the highest value of .810 W/(m·K) at 700°C. The SiO_2f/SiO₂ composites show obvious advantages in the application of load-bearing and thermal insulation integration, and they are expected to meet the demanding requirements of hot-pressing sintering and non-ferrous metallurgy industries.     

Simultaneous enhancement of mechanical and microwave absorption properties with a novel in-situ synthesis α-Al2O3 fillers for SiCf/SiC composites

The Al and H₃BO₃ mixed powder was introduced into the PCS/Xylene precursor solution as in-situ synthesis α-Al₂O₃ filler by precursor infiltration and pyrolysis (PIP) method. The in-situ synthesis filler can effectively decrease the open porosity of SiC_f/SiC composites and give rise to multiple scattering of microwave and dipolar polarization. Therefore, the mechanical and microwave absorption properties of SiC_f/SiC composites can be simultaneously enhanced. The effects of in-situ synthesis filler on the morphologies, flexure strength and reflection loss values of SiC_f/SiC composites were investigated. With 2 wt% in-situ synthesis filler, the flexure strength of SiC_f/SiC composite was 305 MPa and the maximum reflection loss (RL_m) can reach ? 54.68 dB with the effective absorption band (EAB) of 3.51 GHz in the X band. With 5 wt% in-situ synthesis filler, the flexure strength of SiC_f/SiC composite was 207 MPa and the RL_m was ? 30.91 dB. Due to the inefficient infiltration process, the RL_m of SiC_f/SiC composites with 10 wt% in-situ synthesis filler was only ? 27.36 dB. Nevertheless, the flexure strength of that composite was 259 MPa, owing to the dense matrix. Additionally, the flexure strength of SiC_f/SiC composite without filler was 148 MPa and the RL_m was ? 26.40 dB.     

Degradation of Al2O3f/SiO2 composites exposed to Na2SO4 environment and MMH/N2O4 bipropellants test

Al₂O_3f/SiO₂ composites were fabricated efficiently using sol-gel process. The degradation behavior exposed to Na₂SO₄ environment at 1100℃ and MMH/N₂O₄ bipropellants test were investigated and compared. The results showed that the strength of Al₂O_3f/SiO₂ composites gradually decreased as the ratio of Na₂SO₄:water increased; the strength of the composites was only 23.56 MPa at 20% (Na₂SO₄:water), which suggested that the composites maintained lower strength. Cracks began to appear in SiO₂ matrix, and the structure of Al₂O₃f/SiO₂ composites could be corroded which would corrode the SiO₂ matrix, leaving naked fibers. Developing a protective layer with higher stability for Al₂O_3f/SiO₂ composites would be considered for long time use. The composites showed higher ablation resistance to MMH/N₂O₄ bipropellant test; the flexural strength was (77.15 ± 4.56) MPa and the retention ratio was 98.7%. The degradation of Al₂O_3f/SiO₂ composites was promoted owing to the thermal-mechanical and chemical factors. SiO₂ matrix became weak and fragile at elevated temperature; some SiO₂ matrix became loosened and porous after being washed away through the shearing of MMH/N₂O₄ bipropellants, which prevented cracks from penetrating Al₂O₃ fibers. With ongoing test, the fibers were worsened by thermal-mechanical corrosion.     

Effect of SiC interphase on the mechanical,high-temperature dielectric and high-temperature microwave absorption properties of the SiCf/SiC/Mu composites

In this study, SiC interphase was prepared via a precursor infiltration-pyrolysis process, and effects of dipping concentrations on the mechanical, high-temperature dielectric and microwave absorption properties of the SiC_f/SiC/Mu composites had been investigated. Results indicated that different dipping concentrations influenced ultimate interfacial morphology. The SiC interphase prepared with 5 wt% PCS/xylene solution was smooth and homogeneous, and no bridging between the fiber monofilament could be observed. At the same time, SiC interphase prepared with 5 wt% PCS/xylene solution had significantly improved mechanical properties of the composite. In particular, the flexural strength of the composite prepared with 5 wt% PCS/xylene solution reached 281 MPa. Both ε′ and ε′′ of the SiC_f/SiC/Mu composites were enhanced after preparing SiC interphase at room temperature. The SiC_f/SiC/Mu composite prepared with 5 wt% PCS/xylene solution showed the maximum dielectric loss value of 0.38 at 10 GHz. Under the dual action of polarization mechanism and conductance loss, both ε′ and ε′′ of the SiC_f/SiC/Mu composites enhanced as the temperature increased. At 700 °C, the corresponding bandwidth (RL ≤ ?5 dB) of SiC_f/SiC/Mu composites prepared with 5 wt% PCS/xylene solution can reach 3.3 GHz at 2.6 mm. The SiC_f/SiC/Mu composite with SiC interphase prepared with 5 wt% PCS/xylene solution is expected to be an excellent structural-functional material.     

Processing and flexural properties of 3D,seven-directional braided (SiO2)f/SiO2 composites prepared by silica sol-infiltration-sintering method

Three dimensional (3D), seven-directional braided (SiO₂)_f/SiO₂ composites were prepared by silica sol-infiltration-sintering (SIS) method. The flexural properties were evaluated by three-point bending test. The flexural strength and flexural elastic modulus were found to be about 107 MPa and 17.5 GPa, respectively. The results of stress vs. deflection curve and SEM examination revealed that the fracture mechanism of the (SiO₂)_f/SiO₂ composite was a mixed mode of brittle and ductile. The bond strength of fiber/matrix was weak at low temperature, causing the extensive fiber pull-out. On the other hand, the brittle fracture of some fibers maybe caused by the propagation of micro defect or crack, which existed in the as-prepared composites for the ten-cycle process.     

Effect of ZrC amount and distribution on the thermomechanical properties of Cf/SiC-ZrC composites

C_f/SiC-ZrC composites with different amounts and distributions of ZrC were fabricated by polymer impregnation and pyrolysis. The effects of the ZrC amount and distribution on the microstructural, mechanical, and ablation properties of C_f/SiC-ZrC composites were investigated. C_f/SiC-ZrC composites obtained by the alternating infiltration of ZrC organic precursors and polycarbosilane groups exhibit good tensile strength (240 ± 17.7 MPa) because the ZrC and SiC matrix can mix evenly. However, C_f/SiC-ZrC composites using only ZrC organic precursor infiltration show a low tensile strength (191 ± 16.6 MPa) because more defects can be introduced into the composites. Ablation characterization by a 30 kW plasma wind tunnel for 60 seconds showed that the C_f/SiC-ZrC composites with the highest amount of ZrC matrix (67.8 wt.%) possessed the lowest linear erosion rate of 4 μm/s because liquid SiO₂ could fill the porous ZrO₂ to form a homogenous protective layer. Nevertheless, the C_f/SiC-ZrC composites with a relatively high ZrC amount (55.3 wt.%) exhibited a poorer ablation performance compared to that of C_f/SiC-ZrC composites with a low ZrC amount (38.7 wt.%).     

Effects of ZrSiO4 content on properties of SiO2-based ceramics prepared by digital light processing

SiO₂-based ceramic cores are widely used in the preparation of gas turbine engine hollow blades due to their excellent chemical stability and easy removal after casting. In this paper, ZrSiO₄ reinforced SiO₂-based ceramics were fabricated using digital light processing (DLP) technology. The results showed that the addition of ZrSiO₄ reduced the cure depth due to its high UV light absorptivity and refractive index. When the content of ZrSiO₄ increased to 15 wt%, the cristobalite content reached the maximum, and radial shrinkage reached the minimum of 1.4%. ZrSiO₄ grains could hinder the propagation of cracks, enhancing the room-temperature flexural strength. At 1550 °C, fracturing across SiO₂ grains in SiO₂-based ceramics led to the great improvement of high-temperature flexural strength. When the content of ZrSiO₄ reached 15 wt%, the flexural strength at room temperature and high temperature was 11.5 MPa and 36.7 MPa, respectively. Therefore, the SiO₂-based ceramics prepared using DLP technology have good room temperature and high temperature properties, and are expected to be used for hollow blade casting.     

Effects of ZrO2 nanoparticles on the microstructure and mechanical properties of ZrO2/AlSi10Mg composites manufactured by laser powder bed fusion

In this work, the nano-ZrO₂ particles were mixed into AlSi10Mg alloy to prepare ZrO₂/AlSi10Mg composites with different x wt.% ZrO₂ (x = 0, 0.15, 0.3, 0.45, 0.6, 0.75). The microstructure, mechanical properties and the anisotropy of the ZrO₂/AlSi10Mg composites fabricated by laser powder bed fusion (LPBF) were studied. The results show that nano-ZrO₂ particles can be uniformly dispersed on the AlSi10Mg powder by the method of pre-dispersion and mechanical mixing. When the mass ratio of ZrO₂ in ZrO₂/AlSi10Mg composites is 0.3 wt%, the values of the tensile strength, yield strength and elongation are 493.64 MPa, 321.30 MPa and 11.74%, respectively. Compared with AlSi10Mg alloy, the tensile strength of ZrO₂/AlSi10Mg composites with 0.3 wt% is increased by 30–55 MPa and the elongation is increased by 3–5%. In addition, the mechanical properties of AlSi10Mg alloy and ZrO₂/AlSi10Mg composites of 0.3 wt% exhibit antistrophic behavior in different direction, which is due to the differences of microstructure, texture and stress distribution between transverse direction (TD) and build direction (BD). Compared with other AlSi10Mg matrix composites, ZrO₂/AlSi10Mg composites of this work show excellent strength and plasticity matching.     

High-temperature properties of 2.5D SiO2f/SiO2 composites by sol–gel

2.5D SiO_2f/SiO₂ composites were fabricated by sol–gel process. The mechanical and fracture behavior of SiO_2f/SiO₂ composites under higher temperature were discussed. The oxidation behavior at 1200 °C and 1500 °C was investigated. The results showed that SiO_2f/SiO₂ composites had high flexural strength, and the fracture mechanism was a combination of brittle and ductile fracture. After higher temperature oxidation, the fracture mechanism changed to typical brittle/sudden fracture. For long time usage at higher temperature, it was necessary to stabilize SiO₂ fibers and SiO₂ matrix of SiO_2f/SiO₂ composites.     

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.     

Direct ink writing of chopped carbon fibers reinforced polymer-derived SiC composites with low shrinkage and high strength

The chopped carbon fiber reinforced SiC (C_f/SiC) composite has been regarded as one of the excellent high-temperature structural materials for applications in aerospace and military fields. This paper presented a novel printing strategy using direct ink writing (DIW) of chopped fibers reinforced polymer-derived ceramics (PDCs) with polymer infiltration and pyrolysis (PIP) process for the fabrication of C_f/SiC composites with high strength and low shrinkage. Five types of PDCs printing inks with different C_f contents were prepared, their rheological properties and alignment of carbon fiber in the printing filament were studied. The 3D scaffold structures and bending test samples of C_f/SiC composites were fabricated with different C_f contents. The results found that the C_f/SiC composite with 30 wt% C_f content has high bending strength (～ 7.09 MPa) and negligible linear shrinkage (～ 0.48%). After the PIP process, the defects on the C_f/SiC composite structures were sufficiently filled, and the bending strength of C_f/SiC composite can reach up to about 100 MPa, which was about 30 times greater than that of the pure SiC matrix without C_f. This work demonstrated that the printed C_f/SiC composites by using this method is beneficial to the development of the precision and complex high-temperature structural members.     

Mechanical behavior of 2.5D (shallow straight-joint) and 3D four-directional braided SiO2f/SiO2 composites

The effect of two different fiber architectures on the mechanical properties and mechanical behavior of the SiO_2f/SiO₂ composites processed by silicasol-infiltration-sintering has been investigated. The composites were sintered at relatively low temperature (450 °C). The fiber/matrix interface strength was weak. The characteristics of 2.5D (shallow straight-joint) structure and 3D four-directional braided structure were determined. The tensile strength, flexural strength, shear strength and failure mechanisms of both 2.5D (shallow straight-joint) and 3D four-directional braided SiO_2f/SiO₂ composites were characterized. It was found that the fiber placement in the preform will strongly affect the mechanical property and failure behavior of the composite. The results of the tests and microstructural observations indicated that 3D four-directional braided SiO_2f/SiO₂ composite had better mechanical properties than 2.5D (shallow straight-joint) SiO_2f/SiO₂ composite. 3D four-directional braided SiO_2f/SiO₂ composite exhibited more graceful failure under loading than 2.5D (shallow straight-joint) SiO_2f/SiO₂ composite.     

Microstructure and mechanical properties of boron carbide/graphene nanoplatelets composites fabricated by hot pressing

In this study, boron carbide (B₄C)-graphene nanoplatelets (GNPs) composites, with enhanced strength and toughness, were fabricated by hot pressing at 1950 °C under a pressure of 30 MPa for 1 h. Microstructure analysis revealed that the GNPs are homogenously dispersed within the B₄C matrix. Raman spectroscopy and electron microscopy showed the orientation of the GNPs in the composites. The effects of the amount of GNPs on the microstructure and mechanical properties of the composites were also investigated. The optimal mechanical properties were achieved using 1 wt% GNPs. The relative density, Vickers hardness, flexure strength, and fracture toughness of the B₄C-GNPs composite ceramic were found to be 99.12%, 32.8 GPa, 508 MPa, and 4.66 MPa m^1/2, respectively. The main toughening mechanisms included crack deflection in three dimensions, GNPs pull-out, and crack bridging. The curled and semi-wrapped GNPs encapsulated individual B₄C grains to resist GNPs pull-out and to deflect propagating cracks.     

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.     

The effect of alumina-based sintering aid on the microstructure,selected mechanical properties,and coefficient of friction of Cf/SiC composite prepared via spark plasma sintering (SPS) method

C_f-SiC air brake discs are being developed due to their high-temperature oxidation resistance compared to conventional C_f/C discs. The C_f-SiC air brake discs should have a coefficient of friction (COF) close to 0.4, a low wear rate, a density higher than 95% of the theoretical density, and flexural strength of more than 200 MPa. To reach the properties of C_f-SiC composite to the required characteristics of the air brake disc, different amounts of alumina-based sintering aid were used. For this purpose, first silicon carbide nanoparticles, sintering aids Al₂O₃–MgO, MgAl₂O₄, Al₂O₃–Y₂O₃, Al₂O₃–SiO₂–MgO, and carbon fiber (20 wt%) with a 5-mm length were prepared. Next, the final composite bulk was created via the SPS method at 1900 °C under a pressure of 50 MPa. The density of the sample sintered with the Al₂O₃–SiO₂–MgO sintering aid was higher than that of other sintering aids. The density value was obtained at 98% and 100% at 8 wt% and 4 wt% respectively. It was also found that the use of 4 wt% of Al₂O₃–SiO₂–MgO offered better mechanical properties compared to 8 wt%, due to the absence of Al₈Si₄O₂₀ phase at 4 wt%. The examination of mechanical properties showed that the hardness (3564 Vickers) and flexural strength (479 MPa) of the sample with the Al₂O₃–SiO₂–MgO sintering aid were higher than those of other sintering aids. The samples with the Al₂O₃–SiO₂–MgO sintering aid with 4 wt% revealed a COF of 0.41, showing the closest feature to the desired indices of aircraft brake discs.     

Effects of sintering temperature on mechanical properties of 3D mullite fiber (ALF FB3) reinforced mullite composites

A new method to weaken the interfacial bonding and increase the strength of 3D mullite fiber reinforced mullite matrix (Mu_f/Mu) composites is proposed and tested in this paper. Firstly, Mu_f/Mu composites were fabricated through sol–gel process with varied sintering temperature. Then, the effects of sintering temperature on mechanical properties of the composites were tested. As sintering temperature was raised from 1000 °C to 1300 °C, the three-point flexural strength of the composites firstly decreased from 66.17 MPa to 41.83 MPa, and then increased to 63.17 MPa. In order to explain the relationship between composite strength and sintering temperature, morphology and structure of the mullite fibers and mullite matrix after the same heat-treatment as in the fabrication conditions of the composites were also investigated. Finally, it is concluded that this strength variation results from the combined effects of matrix densification, interfacial bonding and fiber degradation under different sintering temperatures.     

Effect of short carbon fiber content on the mechanical properties of TiB2-based composites prepared by spark plasma sintering

In this study, TiB₂-30 vol% SiC composites containing 0, 5, 10, and 15 vol% short carbon fibers (C_f) were produced by spark plasma sintering (SPS). The effect of carbon fiber content on microstructure, density, and mechanical properties (micro-hardness and flexural strength) of the fabricated composites was studied. Scanning electron microscopy (SEM) results indicated that the fibers were uniformly dispersed in the TiB₂–SiC matrix using wet ball milling before SPS process. Fully dense TiB₂–SiC–C_f composites were achieved by SPS process at 1900°C for 10 min under 30 MPa. With the addition of fibers, the relative density of the composites did not change considerably. Mechanical tests revealed that microhardness was reduced about 19% by the incorporation of carbon fibers, whereas the flexural strength improved significantly. However, the flexural strength diminished by adding carbon fibers above to critical value (5 vol%) due to residual thermal stresses, nonhomogeneous structure and graphitization of carbon fibers. It was found that the composite with 5 vol% C_f had the highest flexural strength (482 MPa), which was enhanced by 20% compared with the TiB₂–SiC composite.     

Ambient and elevated temperature mechanical properties of hot-pressed fused silica matrix composite

The ambient and elevated temperature mechanical properties of two kinds of hot-pressed fused silica matrix composites, SiO₂+5 vol.% Si₃N₄ and SiO₂+5 vol.% Si₃N₄+ 10 vol.% C_f, were investigated. Si₃N₄ additions greatly enhanced the ambient strength and fracture toughness, while, further incorporation of chopped carbon fibers only but sharply increased the fracture toughness value from 1.22 to 2.4 MPa m^1/2. The strength of the two composites synchronously exhibited anomalous gains at certain elevated temperature range especially from 1000 to 1200 °C, and reached their maximum values at 1000 °C, 168.9 and 130.6 MPa, which were 77.0 and 77.4% higher than their ambient strength, respectively. The two composites exhibited catastrophic fracture even at 1000 °C, but manifested prominent plastic deformation at 1200 °C and usually no fracture occurred during the strength test. Vickers’ indentation crack propagation behavior, combined with fractographs studies, suggested that toughening from carbon fiber was attributed primarily to the fiber bridging, pull-out and crack deflection.     

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.