Microstructure and Mechanical Properties of (TiB2 + SiC) Reinforced Ti3SiC2 Composites Synthesized by In Situ Hot Pressing

Fully dense (TiB₂ + SiC) reinforced Ti₃SiC₂ composites with 15 vol% TiB₂ and 0–15 vol% SiC were designed and synthesized by in situ reaction hot pressing. The increase in SiC content promoted densification and significantly inhibited the growth of Ti₃SiC₂ grains. The in situ incorporated TiB₂ and SiC reinforcements showed columnar and equiaxed grains, respectively, providing a strengthening–toughening effect by the synergistic action of particulate reinforcement, grain's pulling out, “self‐reinforcement,” crack deflection, and grain refining. A maximum bending strength of 881 MPa and a fracture toughness of 9.24 MPam^1/2 were obtained at 10 vol% SiC. The Vickers hardness of the composites increased monotonously from 9.6 to 12.5 GPa.     

Fabrication of Ti3SiC2 and Ti4SiC3 MAX phase ceramics through reduction of TiO2 with SiC

Ti₃SiC₂ and Ti₄SiC₃ MAX phase ceramics were fabricated through high-temperature vacuum reduction of TiO₂ using SiC as a reductant, followed by hot pressing of the products under 25 MPa of pressure at 1600 °C. It was found that both Ti₃SiC₂ and Ti₄SiC₃ may be obtained in good yields, depending on the annealing time during the reduction step. In addition to MAX phases, the products contained some amounts of TiC. The hot pressing step did not significantly affect the composition of the products, indicating good stability of Ti₃SiC₂ and Ti₄SiC₃ under these conditions. Analysis of the densification behavior of the samples revealed lower ductility in Ti₄SiC₃ compared to Ti₃SiC₂. The samples prepared herein exhibited the flexural strength, fracture toughness and microhardness typical of coarse-grained MAX-phase ceramics.     

Ti3SiC2 Reinforced ZA27 Alloy Composites with Enhanced Mechanical Properties

This work reports the fabrication and mechanical properties of Ti₃SiC₂ reinforced Zn‐27 wt. % Al alloy (denoted as ZA27). A total of 10–40 vol. % Ti₃SiC₂ reinforced ZA27 alloy composites were synthesized by hot pressing mechanically alloyed mixtures of Ti₃SiC₂ and ZA27 powders. Among the fabricated composites, 20 vol. % Ti₃SiC₂/ZA27 composite possesses the highest room temperature tensile strength, bending strength and Vickers hardness of 339 MPa, 593 MPa, and 1.13 GPa, respectively. The improved mechanical properties of the 20 vol. % Ti₃SiC₂/ZA27 composite are mainly attributed to the effects of fine‐grain strengthening and dispersion strengthening.     

Synthesis,microstructure, and mechanical properties of TiC-SiC-Ti3SiC2 composites prepared by in situ reactive hot pressing

In this work, TiC-SiC-Ti₃SiC₂ composites were synthesized by in situ reactive hot pressing using β-SiC, graphite, and TiH₂ powders as initial materials. Microstructure and mechanical properties of as-prepared dense composites were systematically investigated. It was found that by increasing the initial SiC content the final SiC content in the composites increased in contrast to the decrease in TiC and Ti₃SiC₂ contents. In the dense composites, TiC and Ti₃SiC₂ grains exhibited transgranular fracture, whereas SiC particles showed intergranular fracture. The composite containing 77 vol.% TiC, 4 vol.% SiC, and 19 vol.% Ti₃SiC₂ had the highest flexural strength of 706.6 MPa. The composite consisting of 44 vol.% TiC, 49 vol.% SiC, and 7 vol.% Ti₃SiC₂ exhibited the highest Vickers hardness of 22.3 GPa and the highest fracture toughness of 6.0 MPa·m^1/2.     

Microstructure and mechanical properties of hot-pressed SiC nanofiber reinforced SiC composites

This study reports on the preparation and mechanical properties of a novel SiC_nf/SiC composite. The single crystal SiC nanofiber(SiC_nf) reinforced SiC ceramic matrix composites (CMC) were successfully fabricated by hot pressing the mixture of β-SiC powders, SiC_nf and Al–B–C powder. The effects of SiC_nf mass fraction as well as the hot-pressing temperature on the microstructure and mechanical properties of SiC_nf/SiC CMC were systematically investigated. The results demonstrated that the 15 wt% SiC_nf/SiC CMC obtained by hot pressing (HP) at 1850 °C with 30 MPa for 60 min possessed the maximum flexural strength and fracture toughness of 678.2 MPa and 8.33 MPa m^1/2, respectively. The nanofibers pull out, nanofibers bridging and cracks deflection were found by scanning electron microscopy, which are believed can strengthen and toughen the SiC_nf/SiC CMC via consuming plenty of the fracture energy. Besides, although the relative density of the prepared SiC_nf/SiC CMC further increased with the sintering temperature rose to 1900 °C, the further coarsend composites grains results in the deterioration of the mechanical properties for the obtained composites compared to 1850 °C.     

In-situ formation of Ti3SiC2 interphase in SiCf/SiC composites by molten salt synthesis

Titanium silicon carbide (Ti₃SiC₂) film was synthesized by molten salt synthesis route of titanium and silicon powder based on polymer-derived SiC fibre substrate. The pre-deposited pyrolytic carbon (PyC) coating on the fibre was utilized as the template and a reactant for Ti₃SiC₂ film. The morphology, microstructure and composition of the film product were characterized. Two Ti₃SiC₂ layers form the whole film, where the Ti₃SiC₂ grains have different features. The synthesis mechanism has been discussed from the thickness of PyC and the batching ratio of mixed powder respectively. Finally, the obtained Ti₃SiC₂ film was utilized as interphase to prepare the SiC fibre reinforced SiC matrix composites (SiC_f/Ti₃SiC₂/SiC composites). The flexural strength (σ_F) and fracture toughness (K_IC) of the SiC_f/Ti₃SiC₂/SiC composite is 460 ± 20 MPa and 16.8 ± 2.4 MPa?m^1/2 respectively.     

Joining of SiCf/SiC using a layered Ti3SiC2-SiCw and TiC gradient filler

A layered filler consisting of Ti₃SiC₂-SiC whiskers and TiC transition layer was used to join SiC_f/SiC. The effects of SiC_w reinforcement in Ti₃SiC₂ filler were examined after joining at 1400 or 1500 °C in terms of the microstructural evolution, joining strength, and oxidation/chemical resistances. The TiC transition layer formed by an in-situ reaction of Ti coating resulted in a decrease in thermal expansion mismatch between SiC_f/SiC and Ti₃SiC₂, revealing a sound joint without cracks formation. However, SiC_f/SiC joint without TiC layer showed formation of cracks and low joining strength. The incorporation of SiC_w in Ti₃SiC₂ filler showed an increase in joining strength, oxidation, and chemical etching resistance due to the strengthening effect. The Ti₃SiC₂ filler containing 10 wt.% SiC_w along with the formation of TiC was the optimal condition for joining of SiC_f/SiC at 1400 °C, showing the highest joining strength of 198 MPa as well as improved oxidation and chemical resistance.     

Compressive creep of SiC whisker/Ti3SiC2 composites at high temperature in air

The compressive creep of a SiC whisker (SiC_w) reinforced Ti₃SiC₂ MAX phase-based ceramic matrix composites (CMCs) was studied in the temperature range 1100-1300°C in air for a stress range 20-120 MPa. Ti₃SiC₂ containing 0, 10, and 20 vol% of SiC_w was sintered by spark plasma sintering (SPS) for subsequent creep tests. The creep rate of Ti₃SiC₂ decreased by around two orders of magnitude with every additional 10 vol% of SiC_w. The main creep mechanisms of monolithic Ti₃SiC₂ and the 10% CMCs appeared to be the same, whereas for the 20% material, a different mechanism is indicated by changes in stress exponents. The creep rates of 20% composites tend to converge to that of 10% at higher stress. Viscoplastic and viscoelastic creep is believed to be the deformation mechanism for the CMCs, whereas monolithic Ti₃SiC₂ might have undergone only dislocation-based deformation. The rate controlling creep is believed to be dislocation based for all the materials which is also supported by similar activation energies in the range 650-700 kJ/mol.     

Fast seamless joining of SiCw/Ti3SiC2 composite using electric field-assisted sintering technique

A pair of Ti₃SiC₂ reinforced with SiC whiskers (SiC_w/Ti₃SiC₂) composites was successfully joined without any joining materials using electric field-assisted sintering technology at a temperature as low as 1090°C (T_i) and a short time of 30 s. The microstructure and mechanical properties of the obtained SiC_w/Ti₃SiC₂ joints were investigated. The solid-state diffusion was the main joining mechanism, which was facilitated by a relatively high current density (~586 A/cm²) at the joining interface. The shear strength of the sample joined at 1090°C was 51.8 ± 2.9 MPa. The sample joined at 1090°C failed in the matrix rather than at the interface, which confirmed that a sound inter-diffusion bonding was obtained. A rapid and high efficient self-joining process may find application in the case of SiC_w/Ti₃SiC₂ sealing cladding tube and end cap.     

Formation of Ti3SiC2 interphase coating on SiCf/SiC composite by electrophoretic deposition

To improve the oxidation resistance of SiC composites at high temperature, the feasibility of using Ti₃SiC₂ coated via electrophoretic deposition (EPD) as a SiC fiber reinforced SiC composite interphase material was studied. Through fiber pullout, Ti₃SiC₂, due to its lamellar structure, has the possibility of improving the fracture toughness of SiC_f/SiC composites. In this study, Ti₃SiC₂ coating was produced by EPD on SiC fiber; using Ti₃SiC₂‐coated SiC fabric, SiC_f/SiC composite was fabricated by hot pressing. Platelet Ti₃SiC₂ powder pulverized into nanoparticles through high‐energy wet ball milling was uniformly coated on the SiC fiber in a direction in which the basal plane of the particles was parallel to the fiber. In a 3‐point bending test of the SiC_f/SiC composite using Ti₃SiC₂‐coated SiC fabric, the SiC_f/SiC composite exhibited brittle fracture behavior, but an abrupt slope change in the strength‐displacement curve was observed during loading due to the Ti₃SiC₂ interphase. On the fracture surface, delamination between each layer of SiC fabric was observed.     

Improving thermal stability of SiC whiskers via nanoscale Ti3SiC2 coatings

Effects of SiC whiskers (SiC_w) on the mechanical properties of composites largely depend on their thermal stability at high temperature. In this study, pure SiC_w and Ti₃SiC₂ coated SiC_w were thermal treated at 1600–1800°C for 1 h. Their phase assemblage, morphology, and structural evolution were investigated. Oxygen partial pressures in the graphite furnace resulted in the breakdown of SiC_w into particles at 1600°C, and the degradation became more pronounced with temperature increasing. The thermal stability of SiC whiskers at 1600–1700°C was significantly improved by a thin Ti₃SiC₂ coating on them, as both thermodynamic calculations and experimental observations suggest Ti₃SiC₂ coating could be preferentially oxidized/decomposed, prior to the active oxidation of SiC. At 1800°C, the protective role of the coating on the whiskers became weakened. SiC was converted into gaseous SiO and CO, with the remaining of interconnected TiC micro-rods and amorphous carbon.     

Investigation of preparation and properties of Ti3SiC2/Al2O3 multilayered composites

Ti₃SiC₂/Al₂O₃ multilayered composites were prepared by the combination of tape casting and hot pressing sintering. The slurry was produced by adjusting the amounts of each organic material, including triethyl phosphate (TEP) as a dispersion, polyvinyl butyrate (PVB) as a binder, dioctyl phthalate (DOP) as a plasticizer, and anhydrous ethanol as an organic solvent. When TEP content was 3 wt.%, PVB content was 4.5 wt.%, R-value (DOP/PVB) was 1.4, and solid content was 38 wt.%; the cast film with a smooth surface, good flexibility, and uniform thickness was obtained after defoaming, tape casting, and drying. Three samples were prepared, namely, S1–S3. The S1 was monolithic Ti₃SiC₂/Al₂O₃ (mass ratio is 1:1) composites. S2 and S3 were Ti₃SiC₂/Al₂O₃ multilayered composites, which matrix layers were Ti₃SiC₂/Al₂O₃ composites (mass ratio is 1:1) and Al₂O₃, respectively, and their interface layer was Ti₃SiC₂. S1–S3 were also sintered at 1550°C. The bending strength of multilayered materials were lower than that of monolithic material, but the fracture toughness of multilayered materials significantly increased. Due to the introduction of Ti₃SiC₂ interface layer, the friction coefficient and wear rate of Ti₃SiC₂/Al₂O₃ multilayered composites were reduced by 30.7% and 33.8%, respectively, compared with monolithic material.     

Microstructure and strengthening behavior in high content SiC nanowires reinforced SiC composites

In this study, the high-content SiC_nw reinforced SiC ceramic matrix composites (SiC_nw/SiC CMC) were successfully fabricated by hot pressing β-SiC and sintering additive (Al₂O₃-Y₂O₃) with boron nitride interphase modification SiC_nw. The effects of sintering additive content and mass fraction (5–25 wt%) of SiC_nw on the density, microstructure, and mechanical properties of the composites were investigated. The results showed that with the increase of sintering additives from 10 wt% to 12 wt%, the relative density of the SiC_nw/SiC CMC increased from 97.3% to 98.9%, attributed to the generated Y₃Al₅O₁₂ (YAG) liquid phase from the Al₂O₃-Y₂O₃ that promotes the rearrangement and migration of SiC grains. The comprehensive performance of the obtained composite with 15 wt% SiC_nw possessed the optimal flexural strength and fracture toughness of 524 ± 30.24 MPa and 12.39 ± 0.49 MPa·m^1/2, respectively. Besides, the fracture mode of the composites with 25 wt% SiC_nw content revealed a pseudo-plastic fracture behavior. It concludes that the 25 wt% SiC_nw/SiC CMC was toughened by the fiber pull-outs, debonding, bridging, and crack deflection that can consume plenty of fracture energy. The strategy of SiC nanowires worked as a main bearing phase for the fabrication of SiC/SiC CMC providing critical information for understanding the mechanical behavior of high toughness and high strength SiC nanoceramic matrix composites.     

Fabrication and Properties of Ti3SiC2/SiC Composites

Ti3SiC2/SiC composites were fabricated by reactive hot pressing method. Effects of hot pressing temperature, the content and particle size of SiC on phase composition, densification, mechanical properties and behavior of stress-strain of the composites were investigated. The results showed that ： （ 1 ） Hot-pressing temperature influenced the phase composition of Ti3SiC2/SiC composites. The flexural strength and fracture toughness of composites increased with hot pressing temperature. （2） It became more difficult for the composites to densify when the content of SiC in composites increased. It need be sintered at higher temperature to get denser composite. The flexural strength and fracture toughness of composites increased when the content of SiC added in composites increased. However, when the content of SiC reached 50 wt%, the flexural strength and fracture toughness of composites decreased due to high content of pore in composites. （3） When the content of SiC was same, Ti3SiC2/SiC composites were denser while the particle size of SiC added in composites is 12. 8 μm compared with the composites that the particle size of SiC added is 3 μm. The flexural strength and fracture toughness of composites increased with the increase of particle size of SiC added in composites. （4） Ti3SiC2/SiC composites were non-brittle fracture at room temperature.     

Pore and microstructure change induced by SiC whiskers and particles in porous TiB2–TiC–Ti3SiC2 composites

TiB₂–TiC–Ti₃SiC₂ porous composites were prepared through a plasma heating reaction using powder mixtures of Ti, B₄C SiC whiskers (SiC_w) and SiC particles (SiC_p). The effects of the SiC_w and SiC_p content on pore structures, phase constituents, microstructure, and crystal morphology of TiC were studied. The results show that TiC, TiB, Ti₃B₄ phases are formed within the 5Ti+B₄C system. With the addition of SiC_w and SiC_p, the TiB and Ti₃B₄ phases are reduced, sometimes even disappeared. Interestingly, the content of TiB₂ and TiC increased, resulting in Ti₃SiC₂ and TiSi₂ being formed. The porosity of composites increases notably with the addition of SiC_w. However, with the increase of SiC_p, the porosity of the composites first decreases, followed by an increase. After adding the specified amount of SiC_w/SiC_p, the compressive strength of composites are improved significantly. Additionally, the pore size of the composites are decreased significantly with the addition of SiC_w/SiC_p. During the plasma heating process, some Si atoms will diffuse into the TiC lattice, which in turn made the cubic TiC grains into hexagonal lamellar TiC or Ti₃SiC₂ grains.     

Residual thermal stress of SiC/Ti3SiC2/SiC joints calculation and relaxed by postannealing

Residual thermal stresses in SiC/Ti₃SiC₂/SiC joining couples were calculated by Raman spectra and simulated by finite element analysis, and then relaxed successfully by postannealing. The results showed that the thermal residual stress between Ti₃SiC₂ and SiC was about on the order of 1 GPa when cooling from 1300°C to 25°C. The thermal residual stresses can be relaxed by the recovery of structure disorders during postannealing. When the SiC/Ti₃SiC₂/SiC joints postannealed at 900°C, the bending strength reached 156.9 ± 13.5 MPa, which was almost twice of the as‐obtained SiC/Ti₃SiC₂/SiC joints. Furthermore, the failure occurred at the SiC matrix suggested that both the flexural strength of joining layer and interface were higher than the SiC matrix.     

Joining of Ti-coated monolithic SiC using a SiCw/Ti3SiC2 filler by electric field-assisted sintering

Monolithic SiC, for the first time, was successfully joined using a SiC whisker-reinforced Ti₃SiC₂ composite (SiC_w/Ti₃SiC₂) filler via electric field-assisted sintering technique. A thin Ti coating layer was formed on the SiC surface to minimize the residual stress at the joint interface by transforming it into a TiC gradient layer. After optimizing process parameters, a joint strength higher than 250 MPa was obtained, which is higher than the other values reported in the literature. Failure occurred at the SiC base rather than the joining interface because of the improved joint strength by the incorporation of SiC_w. The addition up to 15 wt. % SiC_w in the filler layer improved the joint strength by various strengthening mechanisms. On the other hand, the joint strength was lower with 20 wt. % SiC_w addition, indicating the importance of thermal expansion mismatch between SiC_w and Ti₃SiC₂ to obtain a sound SiC joint.     

Si-rich pressureless sintering of the gelcasted Ti3SiC2 bulk ceramic

The Si-rich pressureless sintering was used to fabricate the Ti₃SiC₂ bulk ceramic. The results show that the optimized Ti₃SiC₂ suspension could be prepared at the absolute value of zeta potential, pH level, PAA-NH₄ dosage, and solid loading of 62.1 mV, 11, 2.0 wt%, and 50 vol%, respectively. The channels existing in the Si-free sintered body facilitated the reactants and products to diffuse to the interior and out of the Ti₃SiC₂ matrix, thereby forming the porous reaction layer of TiC-Ti₃SiC₂. The co-effects of the channels and the reaction layer of TiC-Ti₃SiC₂ severely lowered mechanical properties of the Si-free sintered Ti₃SiC₂ ceramic. On the contrary, the Si-rich sintering method isolated the volatile carbon and established a closed Si-rich atmosphere to sinter the green Ti₃SiC₂ cylinder. The porosity, density, fracture toughness, hardness, and flexural strength of the Si-rich sintered Ti₃SiC₂ ceramic reached 0.74 vol%, 4.36 g/cm³, 5.49 MPa·m^1/2, 4.03 GPa, and 383 MPa, respectively.     

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

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

Electrochemical corrosion behaviors of Ti3SiC2/Cu composites in a 3.5% NaCl solution

The electrochemical corrosion behaviors of Ti₃SiC₂/Cu composite and polycrystalline Ti₃SiC₂ in a 3.5% NaCl medium were investigated by dynamic potential polarization, potentiostat polarization, and electrochemical impedance spectroscopy. The polycrystalline Ti₃SiC₂ was tested on the identical condition as a control. The characterizations of XRD, X-ray photoelectron spectroscopy, scanning electron microscope, and energy-dispersive spectrometer were used to study the relevant passivation behavior and corrosive mechanism. The self-corrosion current density of Ti₃SiC₂/Cu (6.46 × 10⁻⁶ A/cm²) was slightly higher than that of Ti₃SiC₂ (1.64 × 10⁻⁷ A/cm²). Under open circuit potential, the corrosion resistance of Ti₃SiC₂/Cu was better than that of Ti₃SiC₂. Ti₃SiC₂/Cu exhibited a typical passivation feature with a narrow passivation interval and a breakdown phenomenon. The better corrosion resistance of Ti₃SiC₂ was due to the more stable Si layer of the former. In comparison, for Ti₃SiC₂/Cu composites, Cu reacted with the reactive Si layers in Ti₃SiC₂ to form Cu–Si compounds and TiC, destroying the weak interaction between Si layers and Ti–C layers. In the other hand, the as-formed Cu–Si compounds and TiC dissolved during the corrosion of Ti₃SiC₂/Cu in the 3.5% NaCl medium, causing to the destruction of the passivation film on its surface.