Enhanced high-temperature dielectric and microwave absorption properties of SiC fiber-reinforced oxide matrix composites

Because of outstanding performances of the SiC fiber-reinforced ceramic matrix composites in aircraft/aerospace systems, two silicon carbide fiber-reinforced oxide matrices (SiC_f/oxides) composites have been prepared by a precursor infiltration and sintering method. Results indicate that the flexural strength of the SiC_f/Al₂O₃–SiO₂ composite reaches 159 MPa, whereas that of the SiC_f/Al₂O₃ composite is only 50 MPa. The high-temperature microwave absorption properties of the composite are significantly enhanced due to choosing Al₂O₃ and SiO₂ as the hybrid matrices. Particularly, the minimum reflection loss (RL) value of the SiC_f/Al₂O₃–SiO₂ composite reaches −37 dB in the temperature of 200 °C at 8.6 GHz, and the effective absorption bandwidth (RL ≤ −5 dB) is 4.2 GHz (8.2–12.4 GHz) below 400 °C. The superior microwave absorption properties at high temperatures indicate that the SiC_f/Al₂O₃–SiO₂ composite has promising applications in civil and military areas. © 2018 Wiley Periodicals, Inc. J. Appl. Polym. Sci. 2019 , 136, 47097.     

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.     

Dielectric and microwave absorption properties of CB doped SiO2f/PI double-layer composites

Carbon black (CB) with contents of 5.5?wt% and 15?wt% filled quartz glass fiber reinforced polyimide (SiO_2f/PI) composite were designed and prepared. A double-layer absorbing material was designed using the two composites materials as a matching layer and an absorption layer, respectively. The microwave absorption property of single-layer and double-layer composites is calculated according to transmission line theory. The results show that the microwave absorbing property of double-layer composite is better than that of single-layer at the same thickness. When the 5.5?wt%CB doped SiO_2f/PI composite is used as the matching layer with a thickness of 0.7?mm and 15?wt%CB doped SiO_2f/PI composite is used as the absorption layer with a thickness of 0.9?mm, the RL (reflection loss) of the composite reaches a minimum value of ?46.18?dB at 16.07?GHz. Meanwhile, the bandwidth of RL?≤??5?dB is 5.87?GHz and the bandwidth of RL?≤??10?dB is 3.95?GHz.     

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.     

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.     

In-situ formation of Al2O3/Al core-shell from waste material: Production of porous composite improved by graphene

Aluminum dross produced from aluminum industry was used to fabricate Al₂O₃/Al porous composites. The dross was milled for 20?h to obtain nano powder. The milled material was examined by TEM and XRD. Graphene (up to 4?wt%) was mixed with the dross and utilized to reinforce sintered composites. The milled powders were compacted then fired at various temperatures up to 700?°C. Physical properties in terms of bulk density and apparent porosity for sintered composites were tested using Archimedes method. SEM attached by energy dispersive spectrometer (EDS) was used to inspect microstructure and elemental analysis of sintered composites. Microhardness and compressive strength were also measured. Ultrasonic nondestructive technique was utilized to examine the elastic moduli. Electrical conductivity of sintered composite was also studied. During milling up to 20?h, Al₂O₃/Al core-shell was in-situ formed with size of 65.9 and 23.8?nm, respectively. The apparent porosity of sintered composites was improved with rising graphene percent while it decreased with increasing sintering temperature. Increasing of graphene mass percent and firing temperature led to remarkable increase in all mechanical properties and electrical conductivity. The maximum compressive strength, hardness, elastic modulus and electrical conductivity were 200?MPa, 1200?MPa, 215?GPa and 1.42?×?10^?5 S/m, respectively, obtained for composite sintered at 700?°C having 4?wt% graphene.     

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.     

Effect of heat treatment on the microstructure and strength of yttrium silicate matrix-modified SiCf/SiC composites

Yttrium silicate was introduced into the matrix of SiC_f/SiC composites via the slurry impregnation and reactive chemical vapor infiltration (RCVI) methods to improve the water and oxygen corrosion resistance of the modified composite materials. The effects of heat treatment on the modified matrix and strength of the composites were systematically investigated. The results showed that the modified matrix was composed of a mixture of yttrium monosilicate, yttrium disilicate, and silicon carbide. The modified yttrium silicate matrix (named Y-Si-O matrix) and the silicon carbide matrix were laminated and well combined. After heat treatment, the amount of Y-Si-O in the mixed matrix increased. The modified composites with yttrium silicate had a similar flexural strength as SiC_f/SiC composites (∼400 MPa). After treated at 1000 °C – 1300 °C, the strength of the modified composites increased by 17 %–26 %. The highest strength was measured for composites treated at 1200 °C.     

A new Li-based ceramic of Li4MgSn2O7: Synthesis,phase evolution and microwave dielectric properties

A pure-phase Li₄MgSn₂O₇ (L₄MS) was successfully synthesized through optimizing the calcination condition. Microwave dielectric properties of the L₄MS ceramic with the phase evolution were investigated together with its low-temperature sintering. The sample maintains a single L₄MS phase as sintered below 1200?°C, such that τ_f remains a constant value of ～12.4?ppm/°C. Accompanied by the appearance of impurity phases (Li₂SnO₃)_ss and especially (MgO)_ss at higher sintering temperatures, excellent microwave dielectric properties of ε_r?=?13.1–13.5, Q?×?f?=?106,800–126,810?GHz and τ_f ?=?0–?4.2?ppm/°C are obtained in samples sintered at 1215–1260?°C for 4?h. Reduction of sintering temperature using LiF sintering aid also helps achieve pure-phase dense L₄MS ceramic. The L₄MS?+?x wt.% LiF ceramic exhibits ε_r～13.7, Qxf～97,000?GHz (x?≤?3) and τ_f ～8–13?ppm/°C sintered at 850?°C for potential LTCC applications, and ε_r ～13.9, Qxf～146,000?GHz and τ_f ～1.5–6?ppm/°C (x?≥?4) as sintered 1000?°C, exhibiting large potentials for microwave dielectric candidates.     

Investigation on low-temperature sinterable behavior and tunable dielectric properties of BLMT glass-Li2ZnTi3O8 composite ceramics

The novel low-temperature sinterable ceramic composites were fabricated by mixing B₂O₃-La₂O₃-MgO-TiO₂ (BLMT) glass with Li₂ZnTi₃O₈ ceramic. All composites could be well sintered at 900?°C for 2?h through liquid-phase sintering and viscous sintering process. With BLMT glass increasing, the main phase of composites changed from Li₂ZnTi₃O₈ to LaBO₃ phase crystallized from glass. Nevertheless, the rutile phase was observed in composites with ≥10?wt% glass, which could adjust the temperature coefficient of resonant frequency (τ_f) to near-zero owing to the opposite τ_f value to other phases. Simultaneously relative permittivity (ε_r) and quality factor (Q$\times$f) could be controlled by varying the content of Li₂ZnTi₃O₈ ceramic and BLMT glass. The composite with 20?wt% glass exhibited excellent dielectric properties: ε_r?=?22.7, Q?×?f?=?19,900?GHz, and τ_f ?=?0.28?ppm/°C. In addition, the good chemical compatibility between the composite with 5?wt% glass and Ag electrode made it as a potential candidate for LTCC technology.     

Effect of sintering temperature on electrical properties of SiC/ZrB2 ceramics

SiC/20?wt% ZrB₂ composite ceramics were fabricated via pressureless solid phase sintering in argon atmosphere at different temperature. The effect of sintering temperature on microstructure, electrical properties and mechanical properties of SiC/ZrB₂ ceramics was investigated. Electrical resistivity exhibits twice significant decreases with increasing sintering temperature. The first decrease from 1900?°C to 2000?°C is attributed to the obvious decrease of continuous pore channels in as-sintered materials. The second decrease from 2100?°C to 2200?°C results from the improvement of carbon crystallization and the disappearance of amorphous layers enveloping ZrB₂ grains. Additionally, the increase of sintered density with increasing temperature caused greatly advance of flexural strength, elastic modulus and Vickers hardness. But excessive temperature is detrimental to flexural strength because of SiC grain growth.     

Low temperature sintering and microwave dielectric properties of Zn1.8SiO3.8 ceramics with BaCu(B2O5) additive for LTCC applications

The Zn_1.8SiO_3.8 (ZS) ceramics with BaCu(B₂O₅) (BCB) additive were synthesized by the conventional solid-state reaction route and the effect of BCB additive on the microwave dielectric properties of the ceramics was investigated. The results demonstrate that BCB could effectively decrease the sintering temperature from 1300?°C to 930?°C and does not induce obviously degradation of the microwave dielectric properties. The 6.wt% BCB added ZS ceramics exhibited a low sintering temperature (~ 930?°C) and excellent dielectric properties of ε_r =?6.79, Q×f =?33,648?GHz, and τ_f =??30?ppm/°C. To compensate the negative τ_f value of this system, TiO₂ powders were introduced. Particularly when 10.wt% TiO₂ was added, good microwave dielectric properties of ε_r=?8.175, Q×f=?21,252?GHz, and τ_f =?1.2?ppm/°C were obtained for the 6.wt% BCB added ZS ceramic sintered at 930?°C for 3?h. Moreover, BCB added ZS-TiO₂ ceramics have a chemical compatibility with silver, which indicate that the BCB added ZS ceramics are promising candidate for LTCC applications.     

Fabrication and mechanical behavior of ZrB2 strengthened SiCf/SiC composites prepared by hybrid processing route

A SiC fiber-reinforced composite containing a SiC-ZrB₂ mixed matrix (SiC_f/(SiC-ZrB₂)) with high density and enhanced mechanical properties was fabricated. ZrB₂ at 5 or 40?vol% was added to a (SiC + C) slurry to be infiltrated into the voids of 2D woven Tyranno?-SA grade-3 fabrics by electrophoretic deposition. Subsequent hot pressing at 1300?°C and 10?MPa for 1?h, followed by liquid silicon infiltration (LSI) at 1600?°C for 5?h in an Ar atmosphere resulted in the formation of the reaction-bonded SiC matrix, which revealed a composite density close to 97%. SiC_f/(SiC-ZrB₂) having open porosities of 0.2–0.6% showed peak strengths of 398 and 320?MPa for 5 and 40?vol% ZrB₂ addition, respectively. The large mismatch in the coefficient of thermal expansion and Young's modulus between the SiC and ZrB₂ phases was attributed to a reverse trend in the strength of composites. Brittle behavior of the composites in flexure can be explained by the strong bonding between the matrix and fibers formed by the reaction of interphase with molten Si during LSI. Strength retention after oxidation at 1000 and 1400?°C for 2?h was also compared in terms of ZrB₂ amount contained in the composites.     

Effect of SiC nanowires on the high-temperature microwave absorption properties of SiCf/SiC composites

SiC-nanowire-reinforced SiC_f/SiC composites were successfully fabricated through an in situ growth of SiC nanowires on SiC fibres via chemical vapour infiltration. The dielectric and microwave absorption properties of the composites were investigated within the frequency range of 8.2–12.4 GHz at 25–600 °C. The electric conductivity and complex permittivity of the composites displayed evident temperature-dependent behaviour and were enhanced with increasing temperature. The composites exhibited superior microwave absorption abilities with a minimum reflection loss value of ?47.5 dB at 11.4 GHz and an effective bandwidth of 2.8 GHz at 600 °C. Apart from the contribution of the interconnected SiC nanowire network and multiple reflections, the excellent microwave absorption performance was attributed to dielectric loss that originated from SiC nanowires with abundant stacking faults and heterostructure interfaces. Results suggested that the composites are promising candidates for high-temperature microwave absorbing materials.     

Sintering behaviour of fluorapatite–silicate composites produced from natural fluorapatite and quartz

In this work, the sintering behaviour of fluorapatite (FAp)–silicate composites prepared by mixing variable amounts of natural quartz (2.5 wt% to 20 wt%) and FAp was studied. The composites were pressureless sintered in air at temperatures from 1000 °C to 1350 °C. The effects of temperatures on the densification, phase formation, chemical bonding and Vickers hardness of the composites were evaluated. All the samples exhibited mixed phase, comprising FAp and francolite as the major constituents along with some minor phases of cristobalite, wollastonite, dicalcium silicate and/or whitlockite dependent on the quartz content and sintering temperature. The composite containing 2.5 wt% quartz exhibited the best sintering properties. The highest bulk density of 3 g/cm³ and a Vickers hardness of >4.2 GPa were obtained for the 2.5 wt% quartz–FAp composite when sintered at 1100 °C. The addition of quartz was found to alter the microstructure of the composites, where it exhibited a rod-like morphology when sintered at 1000 °C and a regular rounded grain structure when sintered at 1350 °C. A wetted grain surface was observed for composites containing high quartz content and was believed to be associated with a transient liquid phase sintering.     

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.     

Effect of manganese addition on sintering behavior and mechanical properties of alumina toughened zirconia

The effect of MnO₂ additives on the sintering behavior and mechanical properties of alumina-toughened zirconia (ATZ, with 10 vol% alumina) composites was investigated by incorporating different amounts of MnO₂ (0, 0.5, 1.0, and 1.5 wt%) and sintering at various temperatures ranging from 1300 to 1450 °C. The addition of MnO₂ up to 1.0 wt% improved the sintered density, hardness, flexural strength, and fracture toughness of the composite. However, the addition of 1.5 wt% MnO₂ degraded the relative density, hardness, and flexural strength of the composite due to the transformation of the ZrO₂ phase from tetragonal to monoclinic and grain coarsening. Optimal results were obtained with 1.0 wt% MnO₂ and sintering at 1450 °C, which improved the mechanical properties (hardness: 13.5 GPa, flexural strength: 1.2 GPa, fracture toughness: 8.5 MPa m^1/2) and lowered the sintering temperature compared to the conventional sintering temperature of ATZ composites (1550 °C). Thus, the ATZ composite doped with MnO₂ is a promising material for structural engineering ceramics owing to its improved mechanical properties and lower sintering temperature.     

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.     

Preparation of porous SiC-Al2O3 ceramics via gelcasting utilising a shrinkable pore-forming agent and oxidised coarse-grained SiC

By utilising soaked millet as a shrinkable pore-forming agent, porous silicon carbide-alumina (SiC-Al₂O₃) ceramics were prepared via gelcasting. The fabrication of SiC-Al₂O₃ ceramics based on oxidised and unoxidised coarse-grained SiC was also studied. The water swelling, drying shrinkage, and low-temperature carbonisation of the millet were investigated. We found that the shrinkage of the soaked millet was greater than that of gel body during drying, which left large gaps that prevented shrinkage stresses from destroying the gel body. Low-temperature carbonisation of the millet should be performed slowly at 220–240?°C because its expansion rate increases to 45% at 250?°C, resulting in the cracking of samples. At a constant sintering temperature, the flexural strength of the SiC-Al₂O₃ ceramics prepared with SiC powders oxidised at 1000?°C was the highest, indicating that oxidised powders can successfully decrease the required sintering temperature and improve the flexural strength of composite ceramics. Based on our optimised process, porous SiC-Al₂O₃ ceramics were sintered at 1500?°C for 2?h. When their skeletons were fully developed, their pore sizes were in the range of 1.5–2?mm. Their porosity and flexural strength were 60.2–65.1% and 8.3–10.5?MPa, respectively.     

Effect of Ti3SiC2 on the ablation behavior and mechanism of Cf-C-SiC-Ti3SiC2 composites under oxyacetylene torch at 3000 °C

In this research, ablation resistance of C_f-C-SiC and C_f-C-SiC-Ti₃SiC₂ composites, fabricated by liquid silicon infiltration (LSI) method were investigated. The infiltration process was conducted at 1500?°C for 30?min and then the samples were annealed at 1350?°C. X-ray diffraction (XRD) technique and scanning electron microscopy (SEM) were utilized in order to investigate the phase composition and microstructure of the ablated samples, respectively. When compared with C_f-C-SiC composite, results showed that mass and linear ablation rates of C_f-C-SiC-Ti₃SiC₂ composite have been improved by 50% and 37.5%, respectively. The mass and linear ablations rates of C_f-C-SiC composite were reached to 23.8?mg/s and 0.096?mm/s, respectively, while these values for C_f-C-SiC-Ti₃SiC₂ were reached to 11.8?mg/s and 0.06?mm/s, respectively. Microscopic investigations showed that formation of protective oxide layer and its stability on the surface of MAX-containing composite are the main reasons for improvement of ablation properties. While the oxide film formed on C_f-C-SiC composite has been blown away by flame.