Microstructure and mechanical properties of multi-walled carbon nanotubes containing Al2O3–C refractories with addition of polycarbosilane

Carbon nanotubes (CNTs) are a promising reinforcement for fabricating Al₂O₃–C refractories. However, CNTs are prone to agglomerate or react with antioxidants or reactive gaseous phases such as Al (g), Si (g) and SiO (g), etc. at high temperatures. To overcome the problems above, polycarbosilane (PCS) and multi-walled carbon nanotubes (MWCNTs) were firstly mixed with micro-alumina powder in a liquid medium and then incorporated into Al₂O₃–C refractories. Then the microstructure and mechanical properties of Al₂O₃–C refractories fired in the temperature range from 800 °C to 1400 °C were investigated in this work. The results showed that the MWCNTs were well dispersed in the specimens with addition of PCS in contrast to the specimens without PCS due to the PCS adsorption on the surface of MWCNTs during the mixing process. And the mechanical properties, such as cold modulus of rupture (CMOR), flexural modulus (FM), forces and displacements of Al₂O₃–C refractories with PCS were much higher than those without PCS, which was attributed to more homogeneous dispersion of MWCNTs, more residual MWCNTs as well as different morphologies of ceramic whiskers. Meanwhile, the oxidation resistance of Al₂O₃–C refractories with PCS was improved greatly, which was supposed that the in situ formed SiC_xO_y coating prevented the oxidation of MWCNTs to some extent.     

Microstructural and mechanical behavior of multi-walled carbon nanotubes reinforced Al–Mg–Si alloy composites in aging treatment

Microstructural and mechanical behavior of heat treatable Al–Mg–Si (6XXX series) alloy composites reinforced with multi-wall carbon nanotubes (MWCNTs) fabricated by powder metallurgy process were investigated by SEM-EDS, XRD, tensile test and Vicker’s hardness test. As-extruded P/M 6063 alloy composites with CNT reinforcements indicated a small increment of mechanical strength compared to the monolithic 6063 alloy with no CNT before T6 heat treatment. When T6 heat treatment was applied to the specimens, the 6063 composite with CNTs showed a noticeable decrease of yield stress (YS) improvement, compared to the monolithic Al alloy. It means that Mg₂Si precipitates hardening effect by the artificial aging treatment was insufficient for the composite containing CNTs. This was mainly because Mg alloying elements were diffused around CNTs and consumed to form Al₂MgC₂ compounds, and resulted in the incomplete matrix strengthening behavior by Mg₂Si precipitation after the aging treatment.     

Fabrication of Nd-doped Ni–Zn ferrite/multi-walled carbon nanotubes composites with effective microwave absorption properties

The electromagnetic materials are featured by good magnetic permeability and dielectric constant characteristics, which are of significant importance in solving the pollution problem of electromagnetic. In this study, after the complete of the use of sol-gel method, argon gas was then introduced for calcination, and eventually a new type of MWCNTs/Ni_0.5Zn_0.5Nd_0.04Fe_1.96O₄ composites was synthesized after the above mentioned procedures. The synthesized MWCNTs were able to be adsorbed on the surface of Ni_0.5Zn_0.5Nd_0.04Fe_1.96O₄ and could form a good conductive work of 3D. Also, the effect of additional MWCNTs on microwave absorption properties of MWCNTs/Ni_0.5Zn_0.5Nd_0.04Fe_1.96O₄ composites were also observed in this study. The results indicate that the additional MWCNTs function to significantly improve the microwave absorption property of MWCNTs/Ni_0.5Zn_0.5Nd_0.04Fe_1.96O₄. Through altering the amount of MWCNTs, the microwave attenuation performance and impedance matching coefficient of this electromagnetic materials can be effectively improved. The S2 sample presented a minimum reflection loss of ?35.05 dB when its thickness reached 1.6 mm, meanwhile, the effective absorption bandwidth achieved 4.55 GHz. The prepared composites perform well in microwave absorption, which can attribute to the reasonable ratio of composites as well as its interaction with both of the magnetic and dielectric components. This research paved the way for novel ideas to be put in the electromagnetic absorption materials with high-efficient.     

Microstructure and mechanical properties of Al2O3–YSZ spherical polycrystalline composites

The mechanical behavior and microstructure of highly densified, spherically shaped, polycrystalline Al₂O₃–YSZ composites, processed from pseudoboehmite powders by sol–gel is reported here. Processing was carried out by combining nanometric sized α-Al₂O₃ (120 nm) seeds and YSZ particles of tetragonal structure. The YSZ particles were homogeneously distributed in a coarse-grained matrix of alumina, both inside grains and along grain boundaries. Fracture surfaces, achieved by impact tests showed toughening effects of the zirconia particles. The tetragonality of the YSZ phase stability even after fracture events and fracture toughness measurements by Vickers indentation, where the crack tip interacts with YSZ particles, are all provided and discussed. The local mechanical properties, such as elastic modulus, indentation hardness and the onset of plastic deformation or fracture contact pressure of both YSZ particles and the Al₂O₃ matrix were quantified by nanoindentation. Evidence of coercive contact pressure was observed in YSZ from indentation stress–strain curves.     

High temperature mechanical properties of Al2O3/TiC micro–nano-composite ceramic tool materials

A type of Al₂O₃-based composite ceramic tool material simultaneously reinforced with micro-scale and nano-scale TiC particles was fabricated by the hot-pressing technology with different contents of cobalt additive. The effects of cobalt on the ambient temperature mechanical properties and high temperature flexural strength were investigated. The flexural strength and fracture toughness of the composite with 3 vol% cobalt as a function of temperature were investigated. Cobalt greatly enhanced the ambient temperature flexural strength and fracture toughness, while further increasing the content of cobalt led to a dramatic strength degradation, especially at high temperature. The flexural strength of the composite containing 3 vol% cobalt decreased as the temperature increased from 20 to 1200 °C, and the fracture toughness decreased as a function of the temperature up to 1000 °C but increased at 1200 °C. The degradation of high temperature flexural strength was ascribed to the change of the fracture mode, the grain and grain boundary oxidation, the decrease of elastic modulus and the grain boundary sliding.     

Synthesis,microstructure, and mechanical properties of WC–TiC–Co ceramic composites

A ceramic composite constituting the formula 78 wt% WC–16 wt% TiC–6 wt% Co denoted as the 78WC–16TiC–6Co ceramic composite was fabricated using a powder metallurgy process, by utilising commercially available WC and Co powders, and laboratory produced TiC powders. TiC powders were produced from machining chips of Grade 4 Titanium. Five different procedures were followed for the manufacturing process by altering the amount of the binding agent (stearic acid) and/or compacting pressure and/or sintering regime (temperature and time) and/or mixing process (dry mixing and mechanical alloying). Characterisation investigations conducted on the sintered samples revealed that stearic acid as the binding agent resulted in the decrease of the relative density while mechanical alloying (MA) induced finer microstructures. The 78WC–16TiC–6Co composites manufactured from commercially available and laboratory produced TiC powders using similar process procedures (including MA) exhibited similar characteristics in terms of relative density, hardness, and wear performance.     

Sintering,mechanical, electrical and oxidation properties of ceramic intermetallic TiC–Ti3Al composites obtained from nano-TiC particles

The paper discusses the development of a new material system for interconnect application in Solid Oxide Fuel Cells (SOFC) based on TiC–Ti₃Al. Nano-sized TiC powders utilized in this research were synthesized using carbon coated TiO₂ precursors from a patented process. The pressureless sintering of TiC–Ti₃Al in a vacuum was applied at temperatures between 1100 °C and 1500 °C and content of Ti₃Al was varied in the range of 10–40 wt%. X-ray diffraction (XRD) and scanning electron microscope (SEM) were used for phase evaluation and sintering behavior. Relative density increased markedly with increasing sintering temperature because of grain growth and formation of the Ti₃AlC₂ secondary phase. Dense products (>95% TD) were prepared from nanosized TiC powders with 10 and 20 wt% Ti₃Al, but with about 8 to 10% porosity for 30 and 40 wt% Ti₃Al. The mechanical properties were determined from Vickers hardness and fracture toughness calculations. Vickers hardness decreased and fracture toughness increased with increasing Ti₃Al content. The electrical conductivity and oxidation behavior of TiC–Ti₃Al composites were investigated to evaluate the feasibility for SOFC interconnect application. The electrical conductivity measurements in the air at 800 °C for 100 h were made using the Kelvin 4-wire method.     

Load-dependence of Knoop hardness of Al2O3–TiC composites

Nine samples of Al₂O₃–30 wt.% TiC composites were prepared by hot-pressing the Al₂O₃ powder mixed with TiC particles. The average sizes of the TiC particles used for preparing the nine samples were different with each other. Knoop hardness measurements were conducted on these nine samples, respectively, in the indentation load range from 1.47 to 35.77 N. For each sample, the measured Knoop hardness decreases with the increasing indentation load. The classical Meyer's power law and an empirical equation proposed originally by Bückle were verified to be sufficiently suitable for describing the observed load-dependence of the measured hardness. Analysis based on Meyer's law can not provide any useful information about the cause of the observed ISE while true hardness values, which are load-independent, can be deduced from the Bückle's equation. It was found that the deduced true hardness increases with the average size of TiC particles existing in the sample.     

Microstructure and mechanical properties of Al2O3 ceramic and TiAl alloy joints brazed with Ag–Cu–Ti filler metal

Al₂O₃ ceramic was reliably joined to TiAl alloy by active brazing using Ag–Cu–Ti filler metal, and the effects of brazing temperature, holding time, and Ti content on the microstructure and mechanical properties of Al₂O₃/TiAl joints were investigated. The typical interfacial microstructure of joints brazed at 880 °C for 10 min was Al₂O₃/Ti₃(Cu,Al)₃O/Ag(s.s)+AlCu₂Ti+Ti(Cu,Al)+Cu(s.s)/AlCu₂Ti+AlCuTi/TiAl alloy. With increasing brazing temperature and time, the thickness of the Ti₃(Cu,Al)₃O reaction layer increased, and the blocky AlCu₂Ti compounds aggregated and grew gradually. The Ti dissolved from the TiAl substrate was sufficient to react with Al₂O₃ ceramic to form a thin Ti₃(Cu,Al)₃O layer when Ag–Cu eutectic alloy was used, but the dissolution of TiAl alloy was inhibited with an increase in Ti content in the brazing filler. Ti and Al dissolved from the TiAl alloy had a strong influence on the microstructural evolution of the Al₂O₃/TiAl joints, and the mechanism is discussed. The maximum shear strength was 94 MPa when the joints were brazed with commercial Ag–Cu–Ti filler metal, while it reached 102 MPa for the joint brazed with Ag–Cu+2 wt% TiH₂ at 880 °C for 10 min. Fractures propagated primarily in the Al₂O₃ substrate and partially along the reaction layer.     

Pressureless sintering of carbon nanotube–Al2O3 composites

Alumina ceramics reinforced with 1, 3, or 5 vol.% multi-walled carbon nanotubes (CNTs) were densified by pressureless sintering. Commercial CNTs were purified by acid treatment and then dispersed in water at pH 12. The dispersed CNTs were mixed with Al₂O₃ powder, which was also dispersed in water at pH 12. The mixture was freeze dried to prevent segregation by differential sedimentation during solvent evaporation. Cylindrical pellets were formed by uniaxial pressing and then densified by heating in flowing argon. The resulting pellets had relative densities as high as ～99% after sintering at 1500 °C for 2 h. Higher temperatures or longer times resulted in lower densities and weight loss due to degradation of the CNTs by reaction with the Al₂O₃. A CNT/Al₂O₃ composite containing 1 vol.% CNT had a higher flexure strength (～540 MPa) than pure Al₂O₃ densified under similar conditions (～400 MPa). Improved fracture toughness of CNT–Al₂O₃ composites was attributed to CNT pullout. This study has shown, for the first time, that CNT/Al₂O₃ composites can be densified by pressureless sintering without damage to the CNTs.     

Interface microstructure and mechanical properties of Ni–Co–P alloy coatings modified carbon fibres reinforced 7075Al matrix composites

To optimize interface microstructure between 7075Al matrix and CFs, Ni–Co–P multi-component alloy coatings coated carbon fibres were prepared by electroless plating firstly and then Ni–Co–P coated CFs reinforced 7075Al matrix composites (CF/Al(Ni–Co–P)) with high relative density were fabricated by hot pressing sintering process. After modification of Ni–Co–P coatings, Al–Co–Ni Intermetallic compounds were formed stably between matrix and reinforcement because of the smaller mixing enthalpy values of Al–Co, Al–Ni and Co–Ni, which not only restrained the generation of Al₄C₃ but also improved interfacial bonding strength. Yield strength and ultimate tensile strength of CF/Al(Ni–Co–P) composites with 30 vol% CFs had maximum improvement compared with CF/Al(U) composites than other composites reinforced by 10 vol%, 20 vol% and 30 vol%CFs, which is up to 305.8 MPa and 668.7 MPa respectively, and the fracture mode of composites from accumulation fracture to non-accumulation fracture as the existence of Ni–Co–P coatings.     

Particle occlusion and mechanical properties of Ni–Al2O3 nanocomposites

Polycrystalline alumina, doped with MgO below the solubility limit, was reinforced with sub-micron particles of Ni by infiltration of Ni-nitrate into fired alumina green bodies, followed by reduction and sintering. The Ni particle size and location were monitored both after reduction and after sintering by transmission electron microscopy. Particle occlusion was found to increase with sintering time and temperature, and is correlated with experimentally detected Mg segregation to the Ni–alumina interfaces, resulting in partial depletion of Mg at the alumina grain boundaries and thus their increased mobility. Occlusion of Ni particles reduces the fracture strength and Weibull modulus of the composites, indicating that particle location is a key microstructural parameter for reaching high fracture strengths, and that this can be controlled via grain boundary and interface adsorption.     

Electrical resistivity of Cr–Al2O3 and ZrxAly–Al2O3 composites with interpenetrating microstructure

AC and DC resistivity of Cr–Al₂O₃ and Zr_xAl_y–Al₂O₃ composites with varying metal content were measured. A strong percolation behavior was observed in the Cr–Al₂O₃ system, where the AC resistivity varied nine orders of magnitude close to the percolation threshold of 28 vol.%. AC measurements were less dependant on the contact resistance than DC measurements. The best reproducibility was obtained at a frequency of 100 kHz. AC resistivity values of insulating composites differed from DC values and may also be frequency-dependant. DC measurements up to 600 °C indicate that the intermetallic phases ZrAl₃ and ZrAl are PTC conductors. The electrical properties of Zr_xAl_y–Al₂O₃ samples with a metal content of 29 vol.% were anisotropic, with a much higher resistivity in the pressing direction.     

Epoxy composites with carbon nanotubes and graphene nanoplatelets – Dispersion and synergy effects

Carbon nanotubes (CNTs) and graphene nanoplatelets (GNPs) at different mix ratios were dispersed by ultrasonication into an epoxy matrix and the effects of CNT:GNP ratios on the mechanical and electrical properties of the hybrid composites were investigated. The combination of CNT and GNP in a ratio 8:2 was observed to synergistically increase flexural properties and to reduce the electrical percolation threshold for the epoxy composites, indicating easier formation of a conductive network due to the improved state of CNT dispersion in the presence of GNPs. The state of dispersion was evaluated at different length scales by using optical microscopy, UV–Vis spectroscopy, rheological measurements, scanning electron microscopy, transmission electron microscopy and sedimentation tests. The Fourier transform infrared spectra for CNT and GNP indicate that the GNPs contain oxygen moieties responsible for better interactions with the epoxy matrix.     

Microstructure and improved mechanical properties of Al2O3/Ba-β-Al2O3/ZrO2 composites with YSZ addition

Al₂O₃/Ba-β-Al₂O₃/ZrO₂ composites were fabricated by solid-state reaction sintering of Al₂O₃, BaZrO₃, and yttria stabilized zirconia (YSZ) powders. The effects of YSZ addition on microstructure and mechanical properties have been investigated. The incorporation of YSZ promoted the densification of the composites and formation of tetragonal ZrO₂ phase. The microstructure of the composites was characterized by elongated Ba-β-Al₂O₃ phase and equiaxed ZrO₂ particles including added YSZ and reaction-formed ZrO₂. The Al₂O₃/Ba-β-Al₂O₃/ZrO₂ composites with YSZ addition exhibited improved fracture toughness, as a result of multiple toughening effects including crack deflection, crack bridging, crack branching, and martensitic transformation of ZrO₂ formed by the reactions between Al₂O₃ and BaZrO₃. Moreover, owing to the grain refinement of Al₂O₃ matrix, dispersion strengthening of the added YSZ particles, and an increase in density of the composites, the Vickers hardness and flexural strength of Al₂O₃/Ba-β-Al₂O₃/ZrO₂ composites were dramatically enhanced in comparison with the composites without YSZ addition.     

Fabrication and microwave absorption properties of magnetite nanoparticle–carbon nanotube–hollow carbon fiber composites

Absorbents with “tree-like” structures, which were composed of hollow porous carbon fibers (HPCFs) acting as “trunk” structures, carbon nanotubes (CNTs) as “branch” structures and magnetite (Fe₃O₄) nanoparticles playing the role of “fruit” structures were prepared by chemical vapor deposition technique and chemical reaction. Microwave reflection loss, permittivity and permeability of Fe₃O₄–CNTs–HPCFs composites were investigated in the frequency range of 2–18 GHz. It was proven that prepared absorbents possessed the excellent electromagnetic wave absorbing performances. The bandwidth with a reflection loss less than −15 dB covers a wide frequency range from 10.2 to 18 GHz with the thickness of 1.5–3.0 mm, and the minimum reflection loss is −50.9 dB at 14.03 GHz with a 2.5 mm thick sample layer. Microwave absorbing mechanism of the Fe₃O₄–CNTs–HPCFs composites is concluded as dielectric polarization and the synergetic interactions exist between Fe₃O₄ and CNTs–HPCFs.     

Sintering,microstructure and mechanical properties of Al2O3–Y2O3–ZrO2 (AYZ) eutectic composition ceramic microcomposites

We report on how the mechanical properties of sintered ceramics (i.e., a random mixture of equiaxed grains) with the Al₂O₃–Y₂O₃–ZrO₂ eutectic composition compare with those of rapidly or directionally solidified Al₂O₃–Y₂O₃–ZrO₂ eutectic melts. Ceramic microcomposites with the Al₂O₃–Y₂O₃–ZrO₂ eutectic composition were fabricated by sintering in air at 1400–1500 °C, or hot pressing at 1300–1400 °C. Fully dense, three phase composites of Al₂O₃, Y₂O₃-stabilized ZrO₂ and YAG with grain sizes ranging from 0.4 to 0.8 μm were obtained. The grain size of the three phases was controlled by the size of the initial powders. Annealing at 1500 °C for 96 h resulted in grain sizes of 0.5–1.8 μm. The finest scale microcomposite had a maximum hardness of 19 GPa and a four-point bend strength of 282 MPa. The fracture toughness, as determined by Vickers indentation and indented four-point bending methods, ranged from 2.3 to 4.7 MPa m^1/2. Although strengths and fracture toughnesses are lower than some directionally or rapidly solidified eutectic composites, the intergranular fracture patterns in the sintered ceramic suggest that ceramic microcomposites have the potential to be tailored to yield stronger, tougher composites that may be comparable with melt solidified eutectic composites.     

Additive manufacturing of continuous carbon fiber–reinforced silicon carbide ceramic composites

A material extrusion (MEX) technology has been developed for the additive manufacturing of continuous carbon fiber–reinforced silicon carbide ceramic (C_f/SiC) composites. By comparing and analyzing the rheological properties of the slurries with different compositions, a slurry with a high solid loading of 48.1 vol% and high viscosity was proposed. Furthermore, several complex structures of C_f/SiC ceramic composites were printed by this MEX additive manufacturing technique. Phenolic resin impregnation–carbonization process reduces the apparent porosity of the green body and protects the C_f. Finally, the reactive melting infiltration (RMI) process was used to prepare samples with different C_f contents from 0 to 2 K (a bundle of carbon fibers consisting of 1000 fibers). Samples with C_f content of 1 K show the highest bending strength (161.6 ± 10.5 MPa) and fracture toughness (3.72 ± 0.11 MPa·m^1/2) while the thermal conductivity of the samples with the C_f content of 1 K reached 11.0 W/(m·K). This study provides a strategy to prepare C_f/SiC composites via MEX additive manufacturing and RMI.     

Microwave hybrid sintering of Al2O3 and Al2O3–ZrO2 composites,and effects of ZrO2 crystal structure on mechanical properties,thermal properties,and sintering kinetics

Structural ceramics such as Al₂O₃ and Al₂O₃–ZrO₂ composites are widely used in harsh environment applications. The conventional sintering process for fabrication of these ceramics is time-consuming method that requires large amount of energy. Microwave sintering is a novel way to resolve this problem. However, to date, very limited research has been carried out to study the effects of different ZrO₂ crystal structures on Al₂O₃–ZrO₂ composites, especially on the sintering kinetics, when fabricated by microwave sintering.The microwave hybrid sintering of Al₂O₃ and Al₂O₃–ZrO₂ composites was performed in this study. Tetragonal zirconia and cubic zirconia were used as two different reinforcements for an α–alumina matrix, and the mechanical and thermal properties were studied. It was found that Al₂O₃ experienced a remarkable increase in fracture toughness of up to 42% when t-ZrO₂ was added. Al₂O₃–c-ZrO₂ also showed increased fracture toughness. The sintering kinetics were also thoroughly investigated, and the average activation energy values for the intermediate stage of sintering were estimated to be 246 ± 11 kJ/mol for pure Al₂O₃, 319 ± 71 kJ/mol for Al₂O₃–c-ZrO₂, and 342 ± 77 kJ/mol for Al₂O₃–t-ZrO₂. These values indicated that the activation energy was increased by the addition of either type of ZrO₂, with the highest value shown by Al₂O₃–t-ZrO₂.