Microstructure and mechanical properties of Cf/ZrC composites fabricated by reactive melt infiltration at relatively low temperature

Carbon fiber-reinforced zirconium carbide matrix composites (C_f/ZrC) were prepared by vacuum infiltrating porous carbon/carbon preforms with molten Zr₂Cu alloy at 1200 °C. X-ray diffraction, scanning electron microcopy and transmission electron microscopy analysis were used to characterize the composition and microstructure of the final composites. It was found that the matrix of the composites were composed of the Cu–Zr–C amorphous phase dispersed with either single- or polycrystalline ZrC. Based on the microstructural analysis, the formation mechanism of the matrix was proposed to be a solution-precipitation and grain coalescence process. The influence of the heat treatment at 1800 °C was also investigated. Results indicated that at very high temperature the volatilization of residual metal somewhat deteriorated the flexural strength and the elastic modulus, but the fracture toughness of the composites was improved due to the sintering of ZrC grains.     

Effect of Cu on the ablation properties of Cf/ZrC composites fabricated by infiltrating Cf/C preforms with Zr-Cu alloys

C_f/ZrC composites were fabricated by reactive melt infiltration at 1200 °C, Low melting Zr₇Cu₁₀, ZrCu and Zr₂Cu alloys were used as infiltrators and the effect of Cu on ablation properties of the composites was investigated. The results show that the C_f/ZrC composites exhibit excellent anti-ablative properties affected apparently by the Cu contents. With the increase of Cu in infiltrators, the linear recession rates decrease from 0.0019±0.0006 to −0.0006±0.0002 mm s⁻¹, whereas the mass loss rates increase from 0.0006±0.0003 to 0.0047±0.0009 g s⁻¹. The formation of a dense ZrO₂ protective layer and the evaporation of residual Cu are in favor of their ablation resistance.     

Effects of ZrC content and mechanical alloying on the microstructural and mechanical properties of hypoeutectic Al-7 wt.% Si composites prepared by spark plasma sintering

This paper reports on the preparation of ZrC particulate-reinforced Al-7 wt.% Si composites by using a consecutive method of mechanical alloying (MA) and spark plasma sintering (SPS). Al, Si (7 wt.%), and ZrC (0, 2, 5, and 10 wt.%) powders were blended and mechanically alloyed (MA'd) for 4 h in a high-energy vibratory ball mill. Subsequently, SPS (at 450 °C for 210 s) was carried out on non-MA'd and MA'd powders. Dissimilar to the inhomogeneous microstructure of the non-MA'd powders, the 4 h MA'd powders exhibited a homogeneous morphology with semi-equiaxed particles that revealed a lower average crystallite size and higher average lattice strain. Furthermore, microstructural, physical, and mechanical characterizations were performed on the spark plasma sintered (SPS'd) composites. The mechanical characterizations showed that MA'd/SPS'd Al-7 wt.% Si-5 wt.% ZrC composite displayed the highest hardness and strength values among all the fabricated composites. It exhibited a hardness of 1.52 ± 0.16 GPa, yield strength of 327.56 ± 7.16 MPa, and compressive strength of 406.42 ± 2.82 MPa. Besides, the MA'd/SPS'd Al-7 wt.% Si-10 wt.% ZrC composite exhibited the lowest wear rate of 0.0022 mm³/N.m, which was approximately 46% of that of the unreinforced composite (0.0048 mm³/N.m). It can be stated that the addition of ZrC and application of MA effectively improved the microstructural and mechanical properties of the composites.     

Mechanical property and microstructure evolutions of Cf/SiOC composites with increasing annealing temperature in reduced pressure environment

Three-dimensional (3D) carbon fiber reinforced silicon oxycarbide (C_f/SiOC) composites were fabricated through precursor impregnation and pyrolysis process using siloxane resin as precursor. These composites were further annealed at various temperatures to follow their mechanical properties and microstructure evolutions in reduced pressure environment. The decrease in strength of those composites could be attributed mainly to the decomposition of matrixes. When the annealing temperature increased from 1000 to 1250 °C, the mechanical properties of composites did not change too much, despite the matrixes underwent a redistribution of Si-O bonds and Si-C bonds. At temperature above 1300 °C, due to the weight loss and volume shrinkage of matrixes caused by carbothermal reduction, both the flexural strength and elastic modulus of C_f/SiOC composites decreased rapidly.     

The effects of phenolic resin-derived PyC interlayers on microstructure and mechanical properties of Cf/SiC composites

A novel, easy and cost-effective way, infiltration and pyrolysis of phenolic resin solution, was exploited to prepare pyrolytic carbon (PyC) interlayers for carbon fiber/silicon carbide (Cf/SiC) mini-composites. X-ray photoelectron spectroscopy, dynamic contact angle measurement and scanning electron microscope were carried out to characterize chemical structure of carbon fibers (CFs), wetting properties between CFs and phenolic resin solution and microstructure of CFs and their composites, respectively. Remarkably, SEM results showed regulation of uniformity and thicknesses of PyC interlayer could be achieved through controlling the concentration of phenolic resin solution and oxidation condition of CFs. When CFs were treated by 10?min' oxidation with 40?mg/L ozone followed by dip-coating with 4?wt% phenolic solution, uniform PyC interlayer with approximately 120?nm were prepared on CFs. The corresponding Cf/SiC specimens had the largest increase in tensile strength and work of fracture with the improvement of 26.2% and 71.6% from the PyC-free case.     

Mechanical properties and microstructures of Cf/SiC-ZrC composites using T700SC carbon fibers as reinforcements

C_f/SiC-ZrC composites were fabricated through mold-pressing and polymer infiltration and pyrolysis (PIP) process using T700SC carbon fibers as reinforcements. The effects of interphases on the mechanical properties and microstructures of composites were studied. Composite showed brittle fracture behavior and low bending stress of 81 ± 24 MPa when no interphase was deposited on the fiber surface. With the deposition of a PyC/SiC interphase, composite showed typical non-brittle fracture behavior and the bending stress increased to 401 ± 64 MPa and a large amount of pulled-out fibers could be observed on the fracture surface. Meanwhile, it could also be concluded from the microstructures of the composites that the existed interphases had a great hindering effect on the infiltration of ZrC into the intra-bundle zones in the slurry infiltration process. The TEM analysis results showed that the carbon fibers were almost not eroded and the brittle fracture behavior may be mainly ascribed to the strong bonding between fibers and matrix.     

Fabrication,microstructure and mechanical properties of co-continuous TiCx/Cu-Cu4Ti composites prepared by pressureless-infiltration method

The co-continuous TiC_x/Cu-Cu₄Ti composites were prepared by infiltrating melting Cu into TiC_0.5 porous preforms. TiC_0.5 porous preforms were firstly synthesized by in-situ solid reaction process using powder Ti and carbon black as the starting materials, PVB as shaping and pore-forming agent. The prepared TiC_0.5 preforms showed 3D-connected visible pores characterized with two classes of sizes, i.e. intergranular pores with size of 10–30?µm and intracrystalline pores with 2–3?µm. Microstructure and phase compositions of the composites were detected by scanning electron microscopy (SEM) equipped with EDS and X-ray diffraction (XRD). Metal region of the composites contained Cu as well as a new phase Cu₄Ti, which was formed by reaction of Cu and TiC_0.5. Composites prepared by this method had a compact structure and strong interface. Meanwhile, metal phase and ceramic phase maintained a co-continuous structure in three dimensions. Cu-Cu₄Ti entered into the TiC_x ceramic particles like root structure during the infiltration process. Flexural strength, fracture toughness and Vickers hardness of the composites reached 948.20?±?124.04?MPa, 12.62?±?0.37?MN?m^?3/2 and 606.4?±?36.7 respectively when content of TiC_x was 71.22?vol%.     

Influence of molybdenum addition on the microstructure and mechanical properties of TiC-based cermets with nano-TiN modification

Effect of Mo addition on the microstructure and mechanical properties of TiC–TiN(nm)–WC–Co–Ni–C system cermets was studied in the work. Specimens were fabricated by conventional powder metallurgy techniques. The microstructure was investigated using transmission electron microscope (TEM) and the scanning electron microscope (SEM). Chemical compositions of different phases such as ceramic phase with core/rim structure [the core being TiC and rim being (Ti,W,Mo)(C,N)] and metallic phase were analyzed quantitatively by EDX. Mechanical properties such as flexural strength, fracture toughness and hardness were also measured. Results show that flexural strength and fracture toughness have a trend to decline with increasing Mo addition, but the change of hardness is not apparent with the increase of Mo addition. Results also reveal that finer microstructure and thicker rim phase will be obtained with the increase of Mo addition. The optimal addition of Mo can be estimated to be 4 wt.% with respect to TiC–10TiN(nm)–15WC–5Co–Mo–5Ni–1C system cermets. Fracture micrographs show that main failure mode of the cermets is a mixed one, i.e., trans-granular and inter-granular fractures both exist.     

Effects of precursor concentration on the microstructure and properties of ZrC modified C/C composites prepared by precursor infiltration and pyrolysis

To improve the ablation resistance of C/C composites, ZrC modified composites were fabricated by precursor infiltration and pyrolysis combined with gradient chemical vapor infiltration process. The effects of ZrC precursor concentration on the microstructure, mechanical and ablation properties of the composites were studied. Results showed that with the increase of ZrC precursor concentration, the ZrC content and macroscopic uniformity of the composites increased but with obvious ZrC particle aggregation and the flexural strength decreased gradually. As the concentration of ZrC precursor improved to 60%, the fracture mode of the composites transformed from toughness to brittleness which was mainly attributed to the improved graphitization degree and reaction damage of carbon fiber in the precursor pyrolysis process. However, the ablation resistance was enhanced with the increasing precursor concentration which was resulted from the formation of ZrO₂ in center ablation region and continuous ZrO₂ coating in brim region serving as a barrier to heat and oxygen transfer.     

Vacuum infiltration of copper aluminate by liquid aluminium

This paper studies attained microstructures and reactive mechanisms involved in vacuum infiltration of copper aluminate preforms with liquid aluminium. At high temperatures, under vacuum, the inherent alumina film enveloping the metal is overcome, and aluminium is expected to reduce copper aluminate, rendering alumina and copper. Under this approach, copper aluminate toils as a controlled infiltration path for aluminium, resulting in reactive wetting and infiltration of the preforms.Ceramic preforms containing a mixture of Al₂O₃ and CuAl₂O₄ were infiltrated with aluminium under distinct vacuum levels and temperatures, and the resulting reaction and infiltration behaviour is discussed. Copper aluminates stability ranges depend on vacuum level and oxygen partial pressure, which determine both CuAl₂O₄ and CuAlO₂ ability for liquid aluminium infiltration. At 1100 °C and 0.76 atm vacuum level CuAl₂O₄ is stable, indicating pO₂ above 0.11 atm. Reactive infiltration is achieved via reaction between aluminium and CuAl₂O₄; however, fast formation of an alumina film blocking liquid aluminium wicking results in incipient infiltration. At 1000 °C and 3.8 × 10⁻⁷ atm vacuum level, CuAlO₂ decomposes to Cu and Al₂O₃ indicating a pO₂ below 6.0 × 10⁻⁷ atm; infiltration of the ceramic is hindered by the non-wetting behaviour of the resulting metal alloy. At 1000 °C and 1.9 × 10⁻⁶ atm vacuum level CuAlO₂ is stable, indicating pO₂ above 6.0 × 10⁻⁷ atm. Extensive infiltration is achieved via redox reaction between aluminium and CuAlO₂, rendering a microstructure characterised by uniform distribution of alumina particles amid an aluminium matrix.This work evidences that liquid aluminium infiltration upon copper aluminate-rich preforms is a feasible route to produce Al-matrix alumina-reinforced composites. The associated reduction reaction renders alumina, as fine particulate composite reinforcements, and copper, which dissolves in liquid aluminium contributing as a matrix strengthener.     

Microstructure and mechanical properties of SiC platelet reinforced BaOAl2O32SiO2 (BAS) composites

BaOAl₂O₃2SiO₂ (BAS) glass–ceramic powders were prepared by sol–gel technique. SiC platelet reinforced BAS glass–ceramic matrix composites with high density and uniform microstructure were fabricated by hot-pressing. The effect of additional crystalline seeds on hexagonal to monoclinic phase transformation of Barium aluminosilicate was studied. The effects of SiC platelet content on the microstructure and mechanical properties of the composites were also investigated. The results showed that the flexural strength and fracture toughness of the BAS glass–ceramic matrix composites can be effectively improved by the addition of silicon carbide platelets. The main toughening mechanism was crack deflection, platelets' pull-out and bridging. The increased value of flexural strength is contributed to the load transition from the matrix to SiC platelets.     

Mechanical properties of the SiCf/SiC composites reinforced with KD-I and KD-II fibers fabricated assisted by a microwave heating method

SiC_f/SiC composites using KD-I and KD-II SiC fibers braided preforms as the reinforcements were fabricated by applying the polymer impregnation and pyrolysis (PIP) technique with a microwave heating assistance. The microwave heating temperature was 1100 °C, 1200 °C, 1300 °C, and 1400 °C, respectively. Microstructures, flexure properties, and fracture behaviors of the composites were investigated. The KDIISiC_f/SiC composites exhibited higher flexure properties and improved non-brittle fracture characteristics than those of the KD-ISiC_f/SiC composites. The differences in the flexural properties, fracture behaviors and microstructures between the KD-I and KDIISiC_f/SiC composites were discussed based on the tensile properties of the SiC filaments and the interfacial bonding statues in the composites.     

Al2O3/Cu-O composites fabricated by pressureless infiltration of paper-derived Al2O3 porous preforms

Al₂O₃/Cu-O composites were fabricated from the paper-derived alumina matrix infiltrated with a Cu-3.2?wt% O alloy. Paper-derived alumina preforms with an open porosity ranging from ～ 14 to ～ 25?vol% were prepared by sintering of alumina-loaded preceramic papers at 1600?°C for 4?h. Pressureless infiltration at 1320?°C for 4?h of the preforms with Cu–O alloy resulted in the nearly dense materials with good mechanical and electrical properties, e.g. fracture toughness up to 6?MPa?m^0.5, four-point-bending strength up to 342?MPa, Young's modulus up to 281?GPa and electrical conductivity up to 2?MS/m depending on the volume fraction of copper alloy in the composites. The technological capability of this approach was demonstrated using prototypes in various engineering fields fabricated by lamination, corrugating and Laminated Object Manufacturing (LOM) methods.     

Mechanical and thermophysical properties of carbon/carbon composites with hafnium carbide

Carbon/carbon (C/C) composites with addition of hafnium carbide (HfC) were prepared by immersing the carbon felt in a hafnium oxychloride aqueous solution, followed by densification and graphitization. Mechanical properties, coefficients of thermal expansion (CTE), and thermal conductivity of the composites were investigated. Results show that mechanical properties of the composites decrease dramatically when the HfC content is greater than 6.5 wt%. CTE of the composites increases with the increase of HfC contents. The composites with addition of 6.5 wt% HfC show the highest thermal conductivity. The high thermal conductivity results from the thermal motion of CO in the gaps and pores, which can improve phonon–defect interaction of the C/C composites. Thermal conductivities of the composites decrease when the HfC content is greater than 6.5 wt%, which is due to formation of a large number of cracks in the composites. Cracks increase the phonon scattering and hence restrain heat transport, which results in the decrease of thermal conductivity of the composites.     

Characterization and mechanical properties of Cf/ZrB2-SiC composites fabricated by a hybrid technique based on slurry impregnation,polymer infiltration and pyrolysis and low-temperature hot pressing

The continuous carbon fiber reinforced ZrB₂-SiC composite was fabricated successfully via a hybrid technique based on nano ceramic slurry impregnation, polymer infiltration and pyrolysis and low-temperature hot pressing. The C_f/ZrB₂-SiC composites exhibited non-brittle fracture modes and the chemical interaction at the fiber/matrix interfaces was effectively inhibited owing to the low sintering temperature. The S2-C_f/ZrB₂-SiC composite presented the highest mechanical properties with fracture toughness of 4.47?±?0.15?MPa?m^1/2 and the work of fracture of 877?J/m², which was attributed to the multiple length-scale toughening mechanisms including the macroscopic toughening mechanisms of crack deflection and crack branching, the micro toughening mechanisms of fiber bridging and fiber pull-out. This work presented a novel and effective method to fabricate high-performance continuous carbon fiber reinforced ceramic matrix composites.     

Preparation and mechanical properties of alumina composites reinforced with nickel-coated graphene

This paper discusses the influence of nickel–phosphorus coated graphene (Gn–Ni–P) and uncoated graphene (Gn) addition to an alumina matrix and its impact on the mechanical properties of obtained composites. The composites are prepared via powder processing and consolidated using the Spark Plasma Sintering (SPS) method. The effects of the addition of coated graphene and coating thickness on mechanical properties were evaluated. Physical properties such as relative density, hardness and fracture toughness were analyzed. Significant improvement of the fracture toughness (60%) for the composites with 2 vol% Gn–Ni–P compared to reference sample was observed. Moreover, 35% higher K_IC was noticed for Gn–Ni–P reinforced composites than for Al₂O₃–Gn.     

HfB2-CNTs composites with enhanced mechanical properties prepared by spark plasma sintering

HfB₂-x vol%CNTs (x=0, 5, 10, and 15) composites are prepared by spark plasma sintering. The influence of CNTs content and sintering temperature on densification, microstructure and mechanical properties is studied. Compared with pure HfB₂ ceramic, the sinterability of HfB₂-CNTs composites is remarkably improved by the addition of CNTs. Appropriate addition of CNTs (10 vol%) and sintering temperature (1800 °C) can achieve the highest mechanical properties: the hardness, flexural strength and fracture toughness are measured to be 21.8±0.5 GPa, 894±60 MPa, and 7.8±0.2 MPa m^1/2, respectively. This is contributed to the optimal combination of the relative density, grain size and the dispersion of CNTs. The crack deflection, CNTs debonding and pull-out are observed and supposed to exhaust more fracture energy during the fracture process.     

Microstructural evolution and mechanical performances of SiC/SiC composites by polymer impregnation/microwave pyrolysis (PIMP) process

SiC/SiC composites were prepared by polymer impregnation/microwave pyrolysis (PIMP) process, and their microstructural evolution and the mechanical performances were characterized. Using non-coated Tyranno SA fiber preforms as reinforcement and impregnation with only allylperhydropolycarbosilane (AHPCS) into the preforms, Tyranno SA/SiC composite (TSA/SiC) with higher density was obtained. While using carbon-coated Tyranno SA fiber preforms, Tyranno SA/C/SiC composite (TSA/C/SiC) with lower density were also fabricated. In this composite, SiC particulate was loaded with polymer precursor (AHPCS) in the first cycle impregnation. Microstructural observation revealed that pore and crack formation was affected by processing conditions. Bending strength was also dependent on the microstructural evolution of the samples. In TSA/SiC composite, relatively strong interfaces contribute to effective load transfer so that higher bending strength could be reached. In the TSA/C/SiC composite, weak interfaces provide a relatively lower strength. Meanwhile, different microstructural evolution and interfacial properties of the composites lead to the variation of the fracture behaviors.     

Properties and microstructure evolution of Cf/SiC composites fabricated by polymer impregnation and pyrolysis (PIP) with liquid polycarbosilane

In the present study, a novel liquid polycarbosilane (LPCS) with a ceramic yield as high as 83% was applied to develop 3D needle-punched C_f/SiC composites via polymer impregnation and pyrolysis process (PIP). The cross-link and ceramization processes of LPCS were studied in detail by FT-IR and TG-DSC; a compact ceramic was obtained when LPCS was firstly cured at 120 °C before pyrolysis. It was found that the LPCS-C_f/SiC composites possessed a higher density (2.13 g/cm³) than that of the PCS-C_f/SiC composites even though the PIP cycle for densification was obviously reduced, which means a higher densification efficiency. Logically, the LPCS-C_f/SiC composites exhibited superior mechanical properties. The shorter length and rougher surfaces of pulled-out fibers indicated the LPCS-C_f/SiC composites to possess a stronger bonding between matrix and PyC interphase compared with the PCS-C_f/SiC composites.     

Al alloy/Ti3SiC2 composites fabricated by pressureless infiltration with melt-spun Al alloy ribbons

Al alloy/Ti₃SiC₂ composites with compressive strengths ranging from 743 to 932 MPa have been successfully fabricated by a new two-step pressureless infiltration method. 6061 Al alloy ribbons prepared by melt spinning were employed as the Al alloy matrix for melt infiltration. Shifts in phase constitution and reaction mechanisms of Ti₃SiC₂ preforms in molten Al at 950 °C were investigated, and the compression performance of Al alloy/Ti₃SiC₂ composites was tested. The Vickers hardness of the composites was enhanced to a maximum of 751 HV by increasing the Al content.