Interfacial optimization of SiC nanocomposites reinforced by SiC nanowires with high volume fraction

High volume fraction SiC nanowires-reinforced SiC composites (SiCNWs/SiC) were prepared by hybrid process of chemical vapor infiltration and polymer impregnation/pyrolysis in this research. SiCNWs networks are first to be made promising a high volume fraction (20 vol%), and the pyrolytic carbon (PyC) interphase with 5 nm is designed on SiCNWs surface to optimize the bonding condition between SiCNWs and SiC matrix. Nanoindentation shows a modulus of 494 ± 14 GPa of SiCNWs/SiC composites without interphase comparing to the one with PyC interphase of 452 ± 13 GPa. However, the 3-point bending test shows a higher strength of the composite with PyC interphase (273 ± 32 MPa) comparing with the one without interphase (240 ± 38 MPa). The fracture surface is observed under SEM, which shows a longer SiCNWs pullout of the composite with PyC interphase. The energy dissipation during the 3-point bending test is calculated by the length of nanowire pull-out, it demonstrates that the SiCNWs with PyC interphase possess better performance for toughening composite. Further characterization proves that the PyC interphase can give SiCNWs/SiC composites higher fracture toughness (4.49 ± 0.44 MPa·m^1/2) than the composites without interphase (3.66 ± 0.28 MPa·m^1/2).     

Effect of interphase on mechanical properties and microstructures of 3D Cf/SiBCN composites at elevated temperatures

Interphase between the fibers and matrix plays a key role on the properties of fiber reinforced composites. In this work, the effect of interphase on mechanical properties and microstructures of 3D C_f/SiBCN composites at elevated temperatures was investigated. When PyC interphase is used, flexural strength and elastic modulus of the C_f/SiBCN composites decrease seriously at 1600°C (92 ± 15 MPa, 12 ± 2 GPa), compared with the properties at room temperature (371 ± 31 MPa, 31 ± 2 GPa). While, the flexural strength and elastic modulus of C_f/SiBCN composites with PyC/SiC multilayered interphase at 1600°C are as high as 330 ± 7 MPa and 30 ± 2 GPa, respectively, which are 97% and 73% of the values at room temperature (341 ± 20 MPa, 41 ± 2 GPa). To clarify the effect mechanism of the interphase on mechanical properties of the C_f/SiBCN composites at elevated temperature, interfacial bonding strength (IFBS) and microstructures of the composites were investigated in detail. It reveals that the PyC/SiC multilayered interphase can retard the SiBCN matrix degradation at elevated temperature, leading to the high strength retention of the composites at 1600°C.     

High-temperature flexural strength of I-CVI processed Cf/SiC composites with variable interphases

The effect of single-layer pyrocarbon (PyC) and multilayered (PyC/SiC)_n=4 interphases on the flexural strength of un-coated and SiC seal-coated stitched 2D carbon fiber reinforced silicon carbide (C_f/SiC) composites was investigated. The composites were prepared by I-CVI process. Flexural strength of the composites was measured at 1200 °C in air atmosphere. It was observed that irrespective of the type of interphase, the seal coated samples showed a higher value of flexural strength as compared to the uncoated samples. The flexural strength of 470 ± 12 MPa was observed for the seal coated C_f/SiC composite samples with multilayered interphase. The seal coated samples with single layer PyC interphase showed flexural strength of 370 ± 20 MPa. The fractured surfaces of tested samples were analyzed in detail to study the fracture phenomena. Based on microstructure-property relations, a mechanism has been proposed for the increase of flexural properties of C_f/SiC composites having multilayered interphase.     

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.     

Influence of graphitization treatment on microstructure and flexural strength of C/C-ZrC-SiC composites fabricated via reactive melt infiltration

C/C-ZrC-SiC composites were prepared by chemical vapor infiltration (CVI) and molten salt assisted reactive melt infiltration (RMI). The microstructure of low density and high density C/C composites without graphitization (LC/HC) and graphitization at 2000 °C (LCG/HCG) were compared. Moreover, the effects of graphitization of LC and HC on the microstructure and flexural strength of C/C-ZrC-SiC composites were investigated in detail. The composites prepared by infiltration of LC and LCG had lower flexural strength, 220.01 ± 21.18 MPa and 197.94 ± 19.05 MPa, respectively. However, the composites prepared by HC and HCG presented higher flexural strength, 308.76 ± 12.35 MPa and 289.62 ± 8.70 MPa, respectively. This was due to the phenomenon of fiber erosion in both LC and LCG during the RMI process. After graphitization, the flexural strength of C/C-ZrC-SiC composites prepared by RMI decreased, but the fracture behavior of the composites tends to be more mild. The decreased strength of the composites were caused by the increased matrix cracks, fiber damage in high temperature and the weak interfacial bonding. The improve of failure behavior of the composites was due to interface debonding between the fiber and matrix, and composites can consume the fracture energy through fiber pull-out.     

Effect of PyC interphase thickness on mechanical behaviors of SiBC matrix modified C/SiC composites fabricated by reactive melt infiltration

A dense carbon fiber reinforced silicon carbide matrix composites modified by SiBC matrix (C/SiC-SiBC) was prepared by a joint process of chemical vapor infiltration, slurry infiltration and liquid silicon infiltration. The effects of pyrolytic carbon (PyC) interphase thickness on mechanical properties and oxidation behaviors of C/SiC-SiBC composites were evaluated. The results showed that C/SiC-SiBC composites with an optimal PyC interphase thickness of 450 nm exhibited flexural strength of 412 MPa and fracture toughness of 24 MPa m^1/2, which obtained 235% and 300% improvement compared with the one with 50 nm-thick PyC interphase. The enhanced mechanical properties of C/SiC-SiBC composites with the increase of interphase thickness was due to the weakened interfacial bonding strength and the decrease of matrix micro-crack amount associated with the reduction of thermal residual stress. With the decrease in matrix porosity and micro-crack density, C/SiC-SiBC composites with 450 nm-thick interphase exhibited excellent oxidation resistance. The residual flexural strength after oxidized at 800, 1000 and 1200 °C in air for 10 h was 490, 500 and 480 MPa, which increased by 206%, 130% and 108% compared with those of C/SiC composites.     

Effect of PyC interphase thickness on mechanical and ablation properties of 3D Cf/ZrC–SiC composite

Three-dimensional (3D) C_f/ZrC–SiC composites were successfully prepared by the polymer infiltration and pyrolysis (PIP) process using polycarbosilane (PCS) and a novel ZrC precursor. The effects of PyC interphase of different thicknesses on the mechanical and ablation properties were evaluated. The results indicate that the C_f/ZrC–SiC composites without and with a thin PyC interlayer of 0.15 µm possess much poor flexural strength and fracture toughness. The flexural strength grows with the increase of PyC layer thickness from 0.3 to 1.2 µm. However, the strength starts to decrease with the further increase of the PyC coating thickness to 2.2 µm. The highest flexural strength of 272.3±29.0 MPa and fracture toughness of 10.4±0.7 MPa m^1/2 were achieved for the composites with a 1.2 µm thick PyC coating. Moreover, the use of thicker PyC layer deteriorates the ablation properties of the C_f/ZrC–SiC composites slightly and the ZrO₂ scale acts as an anti-ablation component during the testing.     

Mild-thermal fabrication and phase conformation of chopped glass fiber-reinforced low-density unsaturated polyester resin with NH<Subscript>4</Subscript>HCO<Subscript>3</Subscript>

Chopped glass fiber-reinforced low-density unsaturated polyester resin product (CFR-LDUPRP) was fabricated utilizing chopped glass fiber and ammonium bicarbonate through an innovative mild-thermal process featuring an ideal phase conformation. Based on the mild-thermal mechanism and preliminary experiments, an orthogonal experiment was conducted to obtain the optimal conditions of CFR-LDUPRP fabrication. The optimal fabrication temperature of 76.0 °C, 20.00 phr of 3 mm chopped glass fiber, 2.50 phr of NH₄HCO₃ and 1.50 phr of tert-butylperoxy benzoate (TBPB) comprised the optimal conditions for CFR-LDUPRP fabrication. Under this condition, the density (ρ), compressive strength (P), and specific compressive strength (P_s) of CFR-LDUPRP specimen were 0.63?±?0.02 g cm^??3, 24.29?±?0.73 MPa, and 38.56?±?1.02 MPa g^??1 cm³, in the given order. The analyses of nonisothermal DSC and semi-quantitative FTIR revealed that NH₄HCO₃ neutralized the residual acid in the resin, leading to an early polymerization of resin and a prolonged curing process of UPR. The endothermic decomposition of NH₄HCO₃ and the vaporization of water enabled a mild-thermal mechanism, which was beneficial for the growth of bubbles and for the distribution of chopped glass fiber in the resin. Proper phase conformation of the resin, bubbles, chopped glass fiber together with cracks and microvoids in the resin matrix, characterized by SEM and ¹H NMR, facilitated the polymerization of UPR and improved properties of CFR-LDUPRP. Bubbles diameter ranged from 0.27 to 0.61 mm without linking or destroyed bubbles.     

Fabrication and characteristic of non-oxide fiber tow reinforced silicon nitride matrix composites by low temperature CVI process

Non-oxide fiber tow reinforced silicon nitride matrix composite was fabricated by low temperature CVI process with PyC as interphase. The tensile strength of the C and SiC fiber tow composites were 547 MPa and 740 MPa, respectively. The difference in tensile strength was analyzed based on the length, amount of pull-out fiber and also interface bonding. The infiltration uniformity of CVI silicon nitride (SiN) matrix within SiC fiber tow was comparable with that of CVI SiC matrix. These results suggested that the low temperature CVI process is suitable for the fabrication of fiber reinforced SiN matrix composites with proper interface bonding and high strength.     

Fabrication of C/C-SiC composites using high-char-yield resin

Carbon fiber reinforced ceramic matrix composites (C/C-SiC composites) were fabricated using a type of high-char-yield phenolic resin with the char yield of 81.17 wt.%. Firstly, the fabric prepreg was prepared by spreading the phenolic resin solution onto the two dimensional carbon fiber plain weave fabric and dried consequently. Afterward, the resin was cured and then the carbon fiber reinforced polymer (CFRP) was pyrolyzed to get amorphous carbon. Finally, C/C-SiC composites were obtained through liquid silicon infiltration (LSI) process. SEM micrographs showed that the Si/SiC area was homogeneously dispersed in the matrix, and during the siliconization process, a layer of SiC was formed along the surface of carbon fibers or carbon matrix. The fiber volume of CFRP was about 40 vol.%, which was much lower than other studies. XRD result indicated that only β-SiC type was formed. The result of X-ray computed tomography clearly showed the structure changes before and after the melt infiltration process. Mechanical property test showed that the composites had fracture strength of 186 ± 23 MPa, and a flexural modulus of 106 ± 8 GPa.     

Fabrication and property evaluation of titanium silicide active filler incorporated ceramic matrix composite

Ceramic Matrix Composites (CMCs) are advanced materials used for high tech applications. Polymer Infiltration and Pyrolysis (PIP) route is a versatile route for the fabrication of CMCs, but the inherent volume shrinkage and porosity in the polymer-derived ceramic (PDC) matrix makes the PIP route unattractive. Carbon fibre reinforced silicon boron oxy-carbide (C_f/SiBOC) CMCs were fabricated via the PIP process using titanium silicide (TiSi₂) active filler. This study details the effect of TiSi₂ and different interphase materials, pyrocarbon (PyC) & boron nitride (BN), on the flexural strength and oxidation resistance properties of C_f/SiBOC CMCs. From the present study, it was concluded that the presence of an active filler and a suitable interphase material is essential for the fabrication of better CMCs in terms of oxidation resistance and flexural strength.     

Biobased composites prepared by compression molding with a novel thermoset resin from soybean oil and a natural‐fiber reinforcement

Biobased composites were manufactured with a compression‐molding technique. Novel thermoset resins from soybean oil were used as a matrix, and flax fibers were used as reinforcements. The air‐laid fibers were stacked randomly, the woven fabrics were stacked crosswise (0/90°), and impregnation was performed manually. The fiber/resin ratio was 60 : 40. The prepared biobased composites were characterized by impact and flexural testing. Scanning electron microscopy of knife‐cut cross sections of the specimens was also done to investigate the fiber–matrix interface. Thermogravimetric analysis of the composites was carried out to provide indications of thermal stability. Three resins from soybean oil [methacrylated soybean oil, methacrylic anhydride modified soybean oil (MMSO), and acetic anhydride modified soybean oil] were used as matrices. The impact strength of the composites with MMSO resin reinforced with air‐laid flax fibers was 24 kJ/m², whereas that of the MMSO resin reinforced with woven flax fabric was between 24 and 29 kJ/m². The flexural strength of the MMSO resin reinforced with air‐laid flax fibers was between 83 and 118 MPa, and the flexural modulus was between 4 and 6 GPa, whereas the flexural strength of the MMSO resin reinforced with woven fabric was between 90 and 110 MPa, and the flexural modulus was between 4.87 and 6.1 GPa. © 2010 Wiley Periodicals, Inc. J Appl Polym Sci, 2010     

Enhanced mechanical and dielectric properties of SiCf/SiC composites with silicon oxycarbide interphase

SiC_f/SiC composites with silicon oxycarbide (SiOC) interphase were successfully prepared using silicone resin as interphase precursor for dip-coating process and polycarbosilane as matrix precursor for PIP process assisted with hot mold pressing. The effects of SiOC interphase on mechanical and dielectric properties were investigated. XRD and Raman spectrum results show that SiOC interphase is composed of silicon oxycarbide and free carbon with a relatively low crystalline degree. The surface morphology of SiC fibers with SiOC interphase is smooth and homogeneous observed by SEM. The flexural strength and failure displacement of SiC_f/SiC composites with SiOC interphase vary with the thickness of interphase and the maximum value of flexural strength is 289 MPa with a failure displacement of 0.39 mm when the thickness of SiOC interphase is 0.25 µm. The complex permittivity of the composites increases from 8.8-i5.7 to 9.8-i8.3 with the interphase thicker.     

Development and characterization of flax fiber reinforced biocomposite using flaxseed oil‐based bio‐resin

In this study, acrylated epoxidized flaxseed oil (AEFO) resin is synthesized from flaxseed oil, and flax fiber reinforced AEFO biocomposites is produced via a vacuum‐assisted resin transfer molding technique. Different amounts of flax fiber and styrene are added to the resin to improve its mechanical and physical properties. Both flax fiber and styrene improve the mechanical properties of these biocomposites, but the flexural strength decreases with an increase in styrene content. The mass increase during water absorption testing is less than 1.5% (w/w) for all of the AEFO‐based biocomposites. The density of the AEFO resin is 1.166 g/cm³, which increases to 1.191 g/cm³ when reinforced with 10% (w/w) flax fiber. The flax fiber reinforced AEFO‐based biocomposites have a maximum tensile strength of 31.4 ± 1.2 MPa and Young's modulus of 520 ± 31 MPa. These biocomposites also have a maximum flexural strength of 64.5 ± 2.3 MPa and a flexural modulus of 2.98 ± 0.12 GPa. © 2014 Wiley Periodicals, Inc. J. Appl. Polym. Sci. 2015 , 132, 41807.     

Enhanced microwave‐absorbing property of precursor infiltration and pyrolysis derived SiCf/SiC composites at X band: Role of carbon‐rich interphase

Ceramic matrix composites (CMCs) can be microwave‐absorbent when endowing the composite constituents with proper dielectric properties. In this work, we report a new method to enhance the microwave‐absorbing property of CMCs by in situ fabrication of a carbon‐rich interphase at the fiber/matrix interface. This was achieved in a SiC fiber reinforced SiC matrix (SiCf/SiC) composite fabricated by precursor infiltration and pyrolysis (PIP). We found that as the PIP temperature increased from 800 to 1000°C, the microwave‐absorbing property of the SiCf/SiC composite was significantly enhanced at X band, which also surpassed those of the SiC fiber and monolithic SiC ceramic fabricated at the same temperature. The dominant mechanism was studied by decoupling the effect of individual SiC fibers, SiC matrix, and fiber/matrix interface. The results showed that the SiC fiber and SiC matrix were barely microwave‐absorbent, due to their low dielectric losses. The microwave‐absorbing mechanism was finally ascribed to the fiber/matrix interface, which was carbon‐rich, containing Si and O elements. The interphase showed a conductivity that was superior to that of the fiber and the matrix, and mainly dominated the dielectric property of the overall composite. The results highlight the role of carbon‐rich interphase on the microwave‐absorbing property of CMCs.     

Continuous alumina fiber-reinforced yttria-stabilized zirconia composites with high density and toughness

Continuous alumina fiber-reinforced yttria-stabilized zirconia (YSZ) composites with a LaPO₄ fiber coating were fabricated by slurry infiltration and spark plasma sintering (SPS). The LaPO₄ coating was deposited on the reinforcement alumina fabrics by a modified sol-gel method. The YSZ slurry with good dispersion and stability was prepared by optimizing the pH value, dispersant addition and ball milling time. The fabricated composite with a high density of ∼ 92 % has a good flexural strength of 277 ± 43 MPa, and a superior fracture toughness of 15.93 ± 0.75 MPa·m^1/2 exhibiting a non-brittle failure behavior. It was found that the LaPO₄ coating reduced the residual stress near the fiber/matrix interface to 131 ± 41 MPa, which was 369 ± 63 MPa in the composite without the fiber coating. The LaPO₄ coating renders a weak interphase to improve the composite toughness by activating several toughening mechanisms including crack deflection, fiber debonding and pullout, and delamination behavior.     

萘酚改性烯丙基化环保型酚醛树脂的合成及研究

分别以环保型PF(酚醛树脂)和萘酚改性环保型PF为母体,成功合成了烯丙基化PF和萘酚改性烯丙基化PF,并制备了萘酚改性烯丙基化PF/BMI(双马来酰亚胺)共聚树脂;然后分别以上述树脂作为基体树脂,制备了玻璃纤维增强型复合材料。结果表明:当基体树脂为萘酚改性烯丙基化PF/BMI共聚树脂时,相应复合材料的冲击强度(321.6 kJ/m2)和弯曲强度(524.1 MPa)比萘酚改性烯丙基化PF基复合材料提高了11.0%和46.3%,比未改性环保型烯丙基化PF基复合材料提高了42.8%和258.2%,说明萘酚改性烯丙基化PF/BMI共聚树脂的增韧效果优于萘酚改性烯丙基化PF;萘酚改性烯丙基化PF/BMI共聚树脂基复合材料的耐热性能优于未改性烯丙基化PF体系,这是因为前者800℃时的残炭率(39.62%)高于后者(10.92%)所致。     

Microstructure and mechanical properties of carbon/carbon composites with PyC/SiC/TiC multilayer interphases

Carbon/carbon composites with PyC/SiC/TiC multilayer interphases (CCs-PST) have been successfully prepared by a joint process of chemical vapor deposition and carbothermal reduction. Effect of the Ti(OC₄H₉)₄/C₆H₄(OH)₂ molar ratio on the morphology of TiC particles was investigated and the ratio was optimized as 8:1. When the Ti(OC₄H₉)₄/C₆H₄(OH)₂ molar ratio was 8:1, many homogeneously distributed TiC nanoparticles with the sizes of 100–500 nm on the fibers were observed. The structural evolution of CCs-PST was discussed and the mechanical properties of as-prepared materials were investigated by flexural and interlaminar shear tests. The resulted composites demonstrated a PyC and SiC mixed inner interphase with the thickness of 0.5–1 $\mathrm{\mu }\mathrm{m}$ and a TiC outer interphase with a thickness about 0.5 µm. Flexural strength of 201.45 ± 5.27 MPa and modulus of 21.21 ± 1.58 GPa showed a 41.7% and 7.83% improvement respectively as compared with that of the neat CCs. The interlaminar shear strength of CCs-PST was 66.71 ± 4.87 MPa, which was 51.20% higher than that of the CCs. The improved mechanical properties were attributed to the enhanced interface bond between fibers and matrix induced by the PST.     

High-dose,intermediate-temperature neutron irradiation effects on silicon carbide composites with varied fiber/matrix interfaces

SiC/SiC composites are promising structural candidate materials for various nuclear applications over the wide temperature range of 300–1000 °C. Accordingly, irradiation tolerance over this wide temperature range needs to be understood to ensure the performance of these composites. In this study, neutron irradiation effects on dimensional stability and mechanical properties to high doses (11–44 dpa) at intermediate irradiation temperatures (?600 °C) were evaluated for Hi-Nicalon Type-S or Tyranno-SA3 fiber–reinforced SiC matrix composites produced by chemical vapor infiltration. The influence of various fiber/matrix interfaces, such as a 50–120 nm thick pyrolytic carbon (PyC) monolayer interphase and 70–130 nm thick PyC with a subsequent PyC (?20 nm)/SiC (?100 nm) multilayer, was evaluated and compared with the previous results for a thin-layer PyC (?20 nm)/SiC (?100 nm) multilayer interphase. Four-point flexural tests were conducted to evaluate post-irradiation strength, and SEM and TEM were used to investigate microstructure. Regardless of the fiber type, monolayer composites showed considerable reduction of flexural properties after irradiation to 11–12 dpa at 450–500 °C; and neither type showed the deterioration identified at the same dose level at higher temperatures (>750 °C) in a previous study. After further irradiation to 44 dpa at 590–640 °C, the degradation was enhanced compared with conventional multilayer composites with a PyC thickness of ?20 nm. Multilayer composites have shown comparatively good strength retention for irradiation to ?40 dpa, with moderate mechanical property degradation beginning at 70–100 dpa. Irradiation-induced debonding at the F/M interface was found to be the major cause of deterioration of various composites.     

Processing and properties of Nextel™ 720 fiber reinforced alumina-zirconia ceramic matrix composites

The continuous Nextel? 720 fiber-reinforced zirconia/alumina ceramic matrix composites (CMCs) were prepared by slurry infiltration process and precursor infiltration pyrolysis (PIP) process. The introduction of submicron zirconia powders into the aqueous slurry was optimized to offer comprehensively good sintering activity, high thermal resistance and good mechanical properties for the CMCs. Meanwhile, the zirconia and alumina preceramic polymers were used to strengthen the porous ceramic matrix through the PIP process. The final CMC sample achieved a high flexural strength of 200 MPa after one infiltration cycle of alumina preceramic polymer and thermal treatment at 1150 °C for 2 h. The flexural strength retention of the improved CMC sample was 104% and 89% respectively after thermal exposure at 1100 °C and 1200 °C for 24 h.