Mechanical and dielectric properties of SiCf/BN/SiBCN composites via different synthesis technologies

SiC fibers reinforced SiBCN ceramic matrix composites (SiC_f/BN/SiBCN composites) were synthesized by direct chemical vapor infiltration (CVI), polymer infiltration pyrolysis (PIP) or chemical vapor infiltration combined with polymer infiltration pyrolysis (CVI + PIP). It is shown that the insertion of a continuous and dense SiBCN matrix via the CVI process improves the flexural strength and modulus. Interface debonding and fiber pullout happened with 50–100 nm BN interface in CVI and CVI + PIP SiC_f/BN/SiBCN composites. The relative complex permittivity was measured in X-band. Higher ε′′ values in CVI-containing composites can be observed, which can be attributed to the accumulation of C and SiC phases and a multilayer matrix. Strong electromagnetic wave attenuation ability was obtained with high dielectric loss.     

Effect of SiC nanowires on the mechanical properties and thermal conductivity of 3D-SiCf/SiC composites prepared via precursor infiltration pyrolysis

In this study, SiC nanowires (SiC_NWS) were grown in situ on the surface of PyC interface through chemical vapor infiltration (CVI) to improve the mechanical characteristics and thermal conductivity of three-dimensional SiC_f/SiC composites fabricated via precursor infiltration pyrolysis (PIP). The effect of SiC_NWS on the properties of the obtained composites was investigated by comparing them with conventional SiC_f/PyC/SiC composites. After the deposition of SiC_NWS, the flexural strength of the SiC_f/SiC composites was found to increase by 46 %, and the thermal conductivity showed an obvious increase at 25?1000 °C. The energy release of the composites in the damage evolution process was analysed by acoustic emission. The results indicated that the damage evolution process was delayed owing to the decrease in porosity, the crack deflection and bridging of the SiC_NWS. Furthermore, the excellent thermal conductivity was attributed to the thermally conductive pathways formed by the SiC_NWS in the dense structure.     

Ring compression properties of SiCf/SiC composites prepared by chemical vapor infiltration

SiC fiber reinforced SiC matrix (SiC_f/SiC) composites prepared by chemical vapor infiltration are one of promising materials for nuclear fuel cladding tube due to pronounced low radioactivity and excellent corrosion resistance. As a structure component, mechanical properties of the composites tubes are extremely important. In this study, three kinds of SiC_f preform with 2D fiber wound structure, 2D plain weave structure and 2.5D shallow bend-joint structure were deposited with PyC interlayer of about 150–200?nm, and then densified with SiC matrix by chemical vapor infiltration at 1050?°C or 1100?°C. The influence of preform structure and deposition temperature of SiC matrix on microstructure and ring compression properties of SiC_f/SiC composites tubes were evaluated, and the results showed that these factors have a significant influence on ring compression strength. The compressive strength of SiC_f/SiC composites with 2D plain weave structure and 2.5D shallow bend-joint structure are 377.75?MPa and 482.96?MPa respectively, which are significantly higher than that of the composites with 2D fiber wound structure (92.84?MPa). SiC_f/SiC composites deposited at 1100?°C looks like a more porous structure with SiC whiskers appeared when compared with the composites deposited at 1050?°C. Correspondingly, the ring compression strength of the composites deposited at 1100?°C (566.44?MPa) is higher than that of the composites deposited at 1050?°C (482.96?MPa), with a better fracture behavior. Finally, the fracture mechanism of SiC_f/SiC composites with O-ring shape was discussed in detail.     

Fabrication of SiC whisker-reinforced SiC ceramic matrix composites based on 3D printing and chemical vapor infiltration technology

Spray drying, binder jetting and chemical vapor infiltration (CVI) were used in combination for the first time to fabricate SiC whisker-reinforced SiC ceramic matrix composites (SiC_W/SiC). Granulated needle-shaped SiC_W was spray dried into SiC_W spherical particles to increase flowability and thereby increase printability. Then, binder jetting was employed to print a novel SiC_W preform with two-stage pores using the SiC_W spherical particles. The subsequent CVI technology produced pure, dense, and continuous SiC matrix with high modulus and strength. Consequently, SiC_W/SiC with appropriate mechanical properties was obtained. Finally, the challenges of the novel method and the ways to improve the mechanical properties of SiC_W/SiC are discussed.     

Preparation and tensile behavior of SiCf/SiC mini composites containing different types and thicknesses of interphase

SiC fiber-reinforced SiC matrix (SiC_f/SiC) composites are promising materials for high-temperature structural applications. In this study, KD-II SiC fiber bundles with a C/Si ratio of approximately 1.25 and an oxygen amount of 2.53%, were used as reinforcement. PyC interphase, PyC-SiC co-deposition interphase I and II, with different thicknesses, and SiC matrix were deposited into the SiC fiber bundles by using chemical vapor infiltration (CVI) to form SiC_f/SiC mini composites. When the thickness of the interphase is approximately 1000 nm, the ultimate tensile stress and strain of SiC_f/SiC mini composites with PyC-SiC co-deposition interphase I can reach 1120.0 MPa and 0.72%, respectively, which are significantly higher than those of SiC_f/SiC mini composites with a PyC interphase (740.0 MPa, 0.87%) and PyC-SiC co-deposition interphase II (645.0 MPa, 0.54%). The effect of thicknesses and types of interphase on tensile fracture behavior of mini composites and then the fracture mechanism are discussed in detail.     

Mechanical properties and strengthening mechanism of SiCf/SiC mini-composites modified by SiC nanowires

The effects of the SiC nanowires (SiCNWs) and PyC interface layers on the mechanical and anti-oxidation properties of SiC fiber (SiC_f)/SiC composites were investigated. To achieve this, the PyC layer was coated on the SiC_f using a chemical vapour infiltration (CVI) method. Then, SiCNWs were successfully coated on the surface of SiC_f/PyC using the electrophoretic deposition method. Finally, a thin PyC layer was coated on the surface of SiC_f/PyC/SiCNWs. Three mini-composites, SiC_f/PyC/SiC, SiC_f/PyC/SiCNWs/SiC, and SiC_f/PyC/SiCNWs/PyC/SiC, were fabricated using the typical precursor infiltration and pyrolysis method. The morphologies of the samples were examined using scanning electron microscopy and energy dispersive X-ray spectrometry. Tensile and single-fibre push-out tests were carried out to investigate the mechanical performance and interfacial shear strength of the composites before and after oxidization at 1200 °C. The results revealed that the SiC_f/PyC/SiCNWs/SiC composites showed the best mechanical and anti-oxidation performance among all the composites investigated. The strengthening and toughening is mainly achieved by SiCNWs optimization of the interfacial bonding strength of the composite and its own nano-toughening. On the basis of the results, the effects of SiCNWs on the oxidation process and retardation mechanism of the SiC_f/SiC mini-composites were investigated.     

Ti3SiC2 interphase coating in SiCf/SiC composites: Effect of the coating fabrication atmosphere and temperature

The SiC fibers were coated with Ti₃SiC₂ interphase by dip-coating. The Ti₃SiC₂ coated fibers were heat-treated from 900 °C to 1100 °C in vacuum and argon atmospheres to comparatively analyze the effect of temperature and atmosphere on the microstructural evolution and mechanical strength of the fibers. The results show that the surface morphology of Ti₃SiC₂ coating is rough in vacuum and Ti₃SiC₂ is decomposed at 1100 °C. However, in argon atmosphere, the surface morphology is smooth and Ti₃SiC₂ is oxidized at 1000 °C and 1100 °C. At 1100 °C, Ti₃SiC₂ oxidized to form a thin layer of amorphous SiO₂ embedded with TiO₂ grains. Meanwhile, defects and pores appeared in the interphase scale. As a result, the fiber strength treated in the argon was lower than that treated in vacuum. The porous Ti₃SiC₂ interphase fabricated under vacuum was then employed to prepare the SiC_f/SiC mini composite by chemical vapor infiltration (CVI) combined with precursor infiltration pyrolysis (PIP), and can effectively improve the toughness of SiC_f/SiC mini composite. The propagating cracks can be deflected within the porous interphase layer, which promotes fiber pull-outs under the tensile strength.     

3D-SiC decorated with SiC whiskers: Chemical vapor infiltration on the porous 3D-SiC lattices derived from polycarbosilane-based suspensions

SiC_w/3D-SiC composites were fabricated by chemical vapor infiltration (CVI) of the 3D SiC lattices, which were prepared via direct ink writing of polycarbosilane-based suspensions. Microstructure, composition and tensile strength of the composites were investigated. Curing and pyrolysis temperature greatly affected the shrinkage, weight loss, density and composition of the 3D SiC. Although sound structure with spanning feature was achieved, cracks and pores in 3D SiC were formed during the pyrolysis owing to the large shrinkage. CVI process decreased the porosity and led to fully dense surface of the SiC_w/3D-SiC composites. After 60h of CVI, short β-SiC fibres or long SiC whiskers were deposited in the structural spacing of 3D lattices or spherical pores inside the filaments, respectively. The tensile strength of the composites by CVI increased from 3.3 MPa to 15.7 MPa (20 h) and 47.3 MPa (60 h), due to the high strength of dense CVI layers and in-situ formed SiC whiskers in pores. This work showed a way to strengthen the 3D SiC with in-situ formed whiskers via the polymer precursor routes.     

Significance of modification of slurry infiltration process for the precursor impregnation and pyrolysis process of SiCf/SiC composites

Several intermediate steps were applied before the precursor infiltration and pyrolysis process to improve the infiltration of SiC slurry for promoting the infiltration of SiC slurry into fiber voids. These steps include sonication, popping, electrophoretic deposition, vacuum infiltration and cold isostatic pressing (CIP). The intermediate processes, especially popping and CIP, had a beneficial effect on green density enhancement and improving the homogeneous infiltration of the slurry into fiber fabrics. The density of the SiC_fiber/SiC_filler green body was 2.20 g/cm³, which corresponded to 68 % of relative density. The SiC_f/SiC composite has a high density of 2.65 g/cm³ after seven PIP cycles.     

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.     

Morphology and anti-ablation properties of PIP Cf/C–SiC composites with different CVI carbon content under 4.2 MW/m2 heat flux oxy-acetylene test

In this work, the needled carbon fiber preforms were used to make seven groups of carbon/carbon composite billets with different matrix carbon contents by controlling the processing time of chemical vapor infiltration (CVI). C_f/C–SiC composites were prepared by infiltration of SiC into these C/C composites billets using polycarbosilane (PCS) through precursor infiltration and pyrolysis (PIP). After oxy-acetylene torch testing (heat flux of 4.2 MW/m²) for 200s, 300s and 400s, respectively, it revealed that the anti-ablation properties of the C_f/C–SiC composite samples were enhanced by a higher content of SiC matrix. Additionally, specimens bearing longer duration tests showed a trend of lower average ablation rates. The lowest linear ablation rate is 0.008 mm/s and the mass ablation rate is 0.0019 g/s for those high SiC content samples tested for 400s. The SEM images of the tested samples showed the mechanism and the non-linear process of ablation resistance progression.     

Computational characterisation of microwave heating of fibre preforms for CVI of SiCf/SiC composites

Silicon carbide fibre reinforced silicon carbide matrix composites (SiC_f/SiC) are known as materials with high-performance mechanical properties for the aerospace industry. Microwave-enhanced (ME) chemical vapour infiltration (CVI) heating of ceramic matrix composites is potentially an energy efficient production technique capable of yielding near fully dense SiC_f/SiC composites in a much shorter time span. This paper reports on the output of computational analysis of electromagnetic (EM) and thermal characteristics of the ME CVI process occurring with thin circular SiC fibre preform in a Labotron microwave system from SAIREM. Computer simulation is performed with the use of the finite-difference time-domain technique implemented in QuickWave computational environment. Multiple puzzling phenomena observed in the earlier experimental work are illuminated in the present study and the causes for the formation of microwave-induced temperature fields are clarified. With the use of the developed EM model, resonant and non-resonant frequencies of the Labotron system for different temperatures of the processed samples are analysed to explain the differences and variability in heating rates. This showed that when microwave processing of small SiC samples, energy coupling is extremely sensitive to frequency: a change of the reflection coefficient from 0.05 (absorbing) to 0.75 (reflective) could be made by a drift as small as 0.003–0.005 GHz, respectively, indicating the importance of scaling the microwave cavity to the sample size and the ability to precisely control the frequency of the microwave source. Moreover, energy coupling is temperature-dependent: low reflections produces very high heating rates (greater than 550 ℃ min^-1); the opposite is true for high reflections where heating rates are significantly slower. Temperature fields in the SiC fibre preforms are computed with the coupled EM-thermal model at different frequencies. It is shown that while being highly non-uniform in the beginning of the process, temperature patterns evolve to being fairly homogeneous by its end. Overall, the results suggest a means for better control of the equipment to pave the way to more efficient, controlled, and repeatable implementations of the ME CVI technology to produce high quality SiC_f/SiC composites.     

Effect of fabric structure on the permeability and regeneration ability of porous SiCf/SiC composite prepared by CVI

In this paper, porous SiC_f/SiC composites are prepared by chemical vapor infiltration of SiC matrix on stitched fibrous preforms with different fabrics laminate structure. The microstructure of the fibrous preforms before and after infiltration of SiC matrix and the permeability and the regeneration efficiency of the porous SiC_f/SiC composites with different laminate structure have been determined. Experimental results show that the porous SiC_f/SiC composites with twill fabrics laminate structure exhibits a higher permeability with a higher volume porosity and mean pore diameter. In comparing the regeneration ability of two types laminate structure filter medium, as expected, the twill fabrics laminate structure exhibits a better regeneration efficiency than the plain fabrics laminate structure due to its higher air permeability.     

The mechanical,thermophysical and electromagnetic properties of UD SiCf/SiC composites in different directions

Unidirectional (UD) silicon carbide (SiC) fiber-reinforced SiC matrix (UD SiC_f/SiC) composites with CVI BN interphase were fabricated by polymer infiltration-pyrolysis (PIP) process. The effects of the anisotropic distribution of SiC fibers on the mechanical properties, thermophysical properties and electromagnetic properties of UD SiC_f/SiC composites in different directions were studied. In the direction parallel to the axial direction of SiC fibers, SiC fibers bear the load and BN interphase ensures the interface debonding, so the flexural strength and the fracture toughness of the UD SiC_f/SiC composites are 813.0 ± 32.4 MPa and 26.1 ± 2.9 MPa·m^1/2, respectively. In the direction perpendicular to the axial direction of SiC fibers, SiC fibers cannot bear the load and the low interfacial bonding strengths between SiC fiber/BN interphase (F/I) and BN interphase/SiC matrix (I/M) both decrease the matrix cracking stress, so the corresponding values are 36.6 ± 6.9 MPa and 0.9 ± 0.5 MPa?m^1/2, respectively. The thermal expansion behaviors of UD SiC_f/SiC composites are similar to those of SiC fibers in the direction parallel to the axial direction of SiC fibers, and are similiar to those of SiC matrix in the direction perpendicular to the axial direction of SiC fibers. The total electromagnetic shielding effectiveness (EM SE_T) of UD SiC_f/SiC composites attains 32 dB and 29 dB when the axial direction of SiC fibers is perpendicular and parallel to the electric field direction, respectively. The difference of conductivity in different directions is the main reason causing the different SE_T. And the dominant electromagnetic interference (EMI) shielding mechanism is absorption for both studied directions.     

Microwave heated chemical vapour infiltration of SiC powder impregnated SiC fibre preforms

Abstract

Abstract

A microwave heated methyl trichlorosilane based chemical vapour infiltration technique has been used to form SiC_f/SiC composites from SiC fibre preforms preimpregnated with SiC powder using two different fabrication techniques. While infiltration rates obtained from samples loaded with powder were generally higher than for preforms without powder, preferential infiltration occurred in regions where the SiC powder was most concentrated as a result of the initial non-uniform distribution of the powder across the preforms. The consequence was density gradients in the final composites. Nevertheless, average densities as high as 75% could be achieved in a 10 h process.     

Effect of SiCnws on flexural strength of SiCf/HfC-SiC composites after impact and ablation

SiC nanowires (SiC_nws) modified SiC_f/HfC-SiC composites were prepared by precursor infiltration and pyrolysis (PIP) and chemical vapor infiltration (CVI) methods. The microstructure, flexural strengths, impact and impact-ablation tests of the composites with and without SiC_nws were investigated. The results showed that after introducing SiC_nws, not only the retention rate of HfC ceramic produced by PIP was increased obviously, but also the fracture displacement of the modified composites was reduced due to the enhancement effect of SiC_nws at interface between SiC fiber and matrix. After impact and impact-ablation, the strength retention of SiC_nws modified composites was 91.6 % and 69.1 % respectively, higher than that of the composites without SiC_nws (85.2 % and 54.8 %). As the impact resistance of the modified composites was improved by the pull-out and bridging of SiC_nws, the ablation resistance of the impacted composites was enhanced as well.     

Microstructure and properties of 2D-Cf/SiC composite fabricated by combination of CVI and PIP process with SiC particle as inert fillers

2D-C_f/SiC composite was manufactured by chemical vapor inflation (CVI) combined with polymer impregnation and pyrolysis (PIP) with SiC particle as inert fillers. The effects of CVI processes on SiC morphologies and the properties of composite were investigated. The composites were characterized by XRD, flexural strength test and SEM. The results revealed that uniform SiC coatings and nanowires were prepared when MTS/H₂ ratio of 1:8 was employed, while gradient thick coatings were fabricated as MTS/H₂ ratio of 1:1 was employed. The flexural strength of composites varied from 156 MPa at MTS/H₂ ratio of 1:1 to 233 MPa at MTS/H₂ ratio of 1:8. All of composites exhibited toughness due to significant debonding and pullout of fibers. The laminated structure of coatings on the fibers and nanowires were manufactured by combination of above different CVI process, and the obtained composites showed flexural strength of as high as 248 MPa and impressive toughness.     

In situ growth of SiC wires on CVI densification of SiC foam

Silicon carbide (SiC) foam prepared by polymer infiltration and pyrolysis (PIP) process was further densified with β-SiC by chemical vapor infiltration (CVI) technique. Scanning electron microscopy and high-resolution transmission electron microscopy images confirmed the presence of highly entangled and branched in situ grown SiC wires of uniform diameter (∼500 nm) over the struts of open-cell SiC foam. A uniform rate increase in diameter from nanometer to micron range (∼11 μm) was observed with an increase in the CVI reaction period. X-ray diffraction results showed the formation of highly crystalline β-SiC structure along the <111> direction with stacking faults. The formation of SiC wires was explained by the vapor–liquid–solid mechanism and evenness of the surface and uniform growth rate of SiC confirmed the homogeneous concentration of gaseous species during CVI reaction. The compressive strength increased with relative density, with maximum values of 5.5 ± 1.26 MPa for ultimate SiC foam (ρ = 400 kg/m³) prepared by hybrid PIP/CVI technique. The thermo-oxidative stability of the resultant foam was evaluated up to 1650°C under air and shows excellent thermal stability compared to SiC foam prepared by PIP route. The densified SiC foam can find potential applications in the field of hot gas filters, catalyst supports, microwave absorption properties, and heat insulation for high-temperature applications.     

Influence of pyrolysis and melt infiltration temperatures on the mechanical properties of SiCf/SiC composites

In order to improve the degree of matrix densification of SiC_f/SiC composites based on liquid silicon infiltration (LSI) process, the microstructure and mechanical properties of composites according to various pyrolysis temperatures and melt infiltration temperatures were investigated.Comparing the microstructures of SiC_f/C carbon preform by a one-step pyrolysis process at 600 °C and two-step pyrolysis process at 600 and 1600 °C, the width of the crack and microcrack formation between the fibers and matrix in the fiber bundle increased during the two-step pyrolysis process. For each pyrolysis process, the density, porosity, and flexural strength of the SiC_f/SiC composites manufactured by the LSI process at 1450–1550 °C were measured to evaluate the degree of matrix densification and mechanical properties. As a result, the SiC_f/SiC composite that was fabricated by the two-step pyrolysis process and LSI process showed an 18% increase in density, 16%p decrease in porosity, and 150% increase in flexural strength on average compared to the composite fabricated by the one-step pyrolysis process.In addition, among the SiC_f/SiC specimens fabricated by the LSI process after the same two-step pyrolysis process, the specimen that underwent the LSI process at 1500 °C showed 30% higher flexural strength on average than those at 1450 or 1550 °C. Furthermore, under the same pyrolysis temperature, the mechanical strength of SiC_f/SiC specimens in which the LSI process was performed at 1500 °C was higher than that of the 1550 °C although both porosity and density were almost similar. This is because the mechanical properties of the Tyranno-S grade SiC fibers degraded rapidly with increasing LSI process temperature.     

Fabrication of a 3D4d braided SiCf/SiC composite via PIP process assisted with an EPD method

In order to improve the thermal conductivity and full-fill the gaps between the fiber bundles for three-dimensional four-directional (3D4d) braided SiC_f/SiC composites, 500?nm submicron-sized β-SiC particles were introduced into the 3D4d preform by an electrophoretic deposition (EPD) method. ζ-potential of the KD-Ⅱ SiC fibers and the aqueous suspension of the β-SiC particles were analyzed, as well as the efficiency of the deposition. After densified via PIP process, microstructure, three-point bending strength and thermal conductivity of the composite were investigated. The results showed that, SiC particles filled the gaps between the SiC fiber bundles efficiently, and thermal conductivity of the composites fabricated through PIP process assisted by EPD was 2.3 times that of the composites fabricated via PIP only. The bending strength of the EPD-composites was 647.08?±?69.53?MPa, which decreased to 2/3 of that of the composites manufactured only by PIP, owing to the reduction of fiber volume fraction and the damages to the interface coatings and fibers under the action of the electric field.