Microstructure and properties of Al2O3-TiC-Ti3SiC2 composites fabricated by spark plasma sintering

Abstract

Abstract

Highly densified Al₂O₃-TiC-Ti₃SiC₂ composites were fabricated by spark plasma sintering technique and subsequently characterised. From fracture surface observation, it is found that Al₂O₃ is 0·2-0·4?μm, TiC is 1-1·5?μm and Ti₃SiC₂ is 1·5-5?μm in grain size. With the increase in Ti₃SiC₂ volume contents, Vickers hardness of the composites decreases because of the low hardness of monolithic Ti₃SiC₂. The fracture toughness rises remarkably when the contents of Ti₃SiC₂ increase, which is attributed to the pullout and microplastic deformation of Ti₃SiC₂ grains. At the same time, the flexural strength of the composites shows a considerable improvement as well. The electrical conductivity rises significantly as the Ti₃SiC₂ contents increase because of the formation of Ti₃SiC₂ network and the increase in conductive phase contents.     

Effect of Ge on microstructure and mechanical properties of Ti3SiC2/Al2O3 composites

Owing to the good physicochemical compatibility and complementary mechanical properties of Ti₃SiC₂ and Al₂O₃, Ti₃SiC₂/Al₂O₃ composites are considered as ideal structural materials. However, TiC and TiSi₂ typically coexist during the synthesis of Ti₃SiC₂/Al₂O₃ composites through an in-situ reaction, which adversely affects the mechanical properties of the resulting composites. In this study, Ti₃SiC₂/Al₂O₃ composites were prepared via in-situ hot pressing sintering at 1450 °C. Ge, which was used as a sintering aid, improved the purity and mechanical properties of the Ti₃SiC₂/Al₂O₃ composites. This is because Ge replaced some of the Si atoms to compensate the evaporation loss of Si to form Ti₃(Si_1-xGe_x)C₂, which showed a crystal structure similar to that of Ti₃SiC₂. Furthermore, the molten Ge accelerated the diffusion reaction of the raw materials, increasing the overall density of the Ti₃SiC₂/Al₂O₃ composites. The optimum Ge amount for improving the mechanical properties of the composites was found to be 0.3 mol. The flexural strength, fracture toughness, and microhardness of the composite with the optimum Ge amount were 640.2 MPa, 6.57 MPa m^1/2, and 16.21 GPa, respectively. The formation of Ti₃(Si_1-xGe_x)C₂ was confirmed by carrying out X-ray diffraction, energy dispersive spectroscopy, and transmission electron microscopy analyses. A model crystal structure of Ti₃(Si_1-xGe_x)C₂ doped with 0.3 mol Ge was established by calculating the solid solubility of Ge.     

Flexible and stretchable Ti3SiC2-based composite films for efficient electromagnetic wave absorption

Ti₃SiC₂, as ternary layered ceramic with good electrical and thermal conductivity, has great application potential in the field of absorbing materials. Absorbing materials are also increasingly required to be lightweight, ultrathin, and flexible. Herein, Ti₃SiC₂/poly (TEP, DOP and PVB) composite film was biomimetically designed and fabricated by type casting process. As-fabricated composite film with 38% content of Ti₃SiC₂ was only 1.62 mm in thickness but exhibited excellent absorbing performance. The maximum reflection loss value of Ti₃SiC₂-based films was as high as −38.41dB and absorption bandwidth below −10 dB was 2.480 GHz. Polymer matrix wrapped around Ti₃SiC₂ not only enhanced the flexibility of the film, but also regulated its impedance matching and complex dielectric constant compared with pure Ti₃SiC₂. Superior wave absorption and flexibility imply excellent potential of this Ti₃SiC₂-based composite film for eliminating electromagnetic interference.     

Fabrication of Ti3SiC2-Ti4SiC3-SiC ceramic composites through carbosilicothermic reduction of TiO2

Dense Ti₃SiC₂-SiC, Ti₄SiC₃-SiC, and Ti₃SiC₂-Ti₄SiC₃-SiC ceramic composites were fabricated through carbosilicothermic reduction of TiO₂ under vacuum, followed by hot pressing of the as-synthesized products under 25 MPa at 1600°C. In the reduction step, SiC either alone or in combination with elemental Si was used as a reductant. A one-third excess of SiC was added in the reaction mixtures in order to ensure the presence of approximately 30 vol.% SiC in the products of synthesis. During the hot pressing step, the samples that contained Ti₃SiC₂ showed better densification compared to those containing Ti₄SiC₃. The obtained composites exhibited the strength properties typical of coarse-grained MAX-phase ceramics. The flexural strength values of 424 and 321 MPa were achieved in Ti₃SiC₂-SiC, and Ti₃SiC₂-Ti₄SiC₃-SiC composites, respectively. The fracture toughness values were 5.7 MPa·m^1/2.     

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.     

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.     

Interface properties of Ti3SiC2/Al2O3 ceramics: Combined experiments and first-principles calculations

The synthesis, characterization, and first-principles calculations of Ti₃SiC₂/Al₂O₃ ceramics were reported. X-ray diffraction measurements showed that the composite ceramics were highly pure. Scanning electron microscopy and transmission electron microscopy were used to characterize the interface information for Ti₃SiC₂ and Al₂O₃ crystals. Surface energies and interface properties were calculated using the first-principles method. The results suggested that Ti₃SiC₂ with Ti terminations and Al₂O₃ with O terminations are more stable than other terminations crystals. Thus powerful attraction between the coordinatively unsaturated Ti and O atoms on the Ti₃SiC₂∥Al₂O₃ interface would result in higher work of adhesion (Wad) and shorter boundary distance, demonstrating the intercrystalline strengthening of Ti₃SiC₂/Al₂O₃ composite ceramics.     

In situ synthesis,mechanical and cyclic oxidation properties of Ti3AlC2/Al2O3 composites

ABSTRACT

Ti₃AlC₂/Al₂O₃ composite materials were successfully fabricated from TiO₂/TiC/Ti/Al powders by the in situ reactive hot pressed technique. The microstructure, mechanical and oxidation properties of the composites were investigated in the paper. Vickers hardness increased with the Al₂O₃ content. The relative density of Ti₃AlC₂/Al₂O₃ composites exhibits a declining tendency with Al₂O₃ content especially exceeds 10 vol.?%. The Ti₃AlC₂/Al₂O₃ composites show excellent electrical conductivity. The flexural strength and fracture toughness of Ti₃AlC₂/10 vol. % Al₂O₃ are 461 ± 20?MPa and 6.2?±?0.2?MPa m^1/2, respectively. The cyclic oxidation behaviour of resistance of Ti₃AlC₂/10 vol. % Al₂O₃ composites at 800–1000°C generally obeys a parabolic law. The oxide scale of sample consists of a mass of α-Al₂O₃ and TiO₂, forming a dense and adhesive protect layer. The result indicates that the Al₂O₃ can greatly improve the oxidation resistance of Ti₃AlC₂.     

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.     

Microstructure evolution,mechanical and tribological properties of Ti3(Al,Sn)C2/Al2O3 composites

In this paper, in situ formed Ti₃(Al,Sn)C₂/Al₂O₃ composites were fabricated by sintering the mixture of Ti₃AlC₂ and SnO₂. The Al atoms could diffuse out of the Ti₃AlC₂ layered structure to react with SnO₂, resulting in the formation of Ti₃(Al,Sn)C₂ solid solution and Al₂O₃. When the SnO₂ content was 20?wt.%, the sintered Ti₃(Al,Sn)C₂/Al₂O₃ composite exhibited the best overall mechanical properties, because of the optimized cooperative strengthening effect of solution strengthening and Al₂O₃ enhancement. When the SnO₂ content increased up to 30?wt.%, the flexural strength and fracture toughness of Ti₃(Al,Sn)C₂/Al₂O₃ composite dramatically decreased on account of the large accumulation of generated Al₂O₃. Moreover, according to the SiC ball-on-flat wear tests, it was found that the wear resistance of Ti₃(Al,Sn)C₂/Al₂O₃ composites was significantly improved as the SnO₂ content increased.     

Influence of Cu on the mechanical and tribological properties of Ti3SiC2

Ti₃SiC₂/Cu composites with different contents of Cu were fabricated by mechanical alloying and spark plasma sintering method. The phase composition and structure of the composites were analyzed by X-ray diffractometry and scanning electron microscopy equipped with energy dispersive spectroscopy. The mechanical and tribological properties of Ti₃SiC₂/Cu composites were tested and analyzed compared with monolithic Ti₃SiC₂ in details. The results show that the Cu leads to the decomposition of Ti₃SiC₂ to produce TiC_x, Ti₅Si₃C_y, Cu₃Si, and TiSi₂C_z. The friction coefficient and wear rate of the composites are lower than that of monolithic Ti₃SiC₂, which is ascribed to the fixing effect of hard TiC_x, Ti₅Si₃C_y, and Cu₃Si to inhibit the abrasive friction and wear. However, at elevated temperatures (ranging from room temperature to 600 °C) the friction and wear of the composites are higher than those at room temperature. Plastic flowing and tribo-oxidation wear accompanied by material transference contribute to the increased friction and wear at elevated temperatures.     

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.     

The effects of microstructure on mechanical and electrical properties of W dispersed Al2O3 ceramics

This work aims to enhance the fracture toughness of brittle Al₂O₃ ceramics and apply insulated Al₂O₃ ceramics with electrical conductivity by dispersing second tungsten (W) metal particles. In order to investigate the effects of W dispersion on mechanical and electrical properties, Al₂O₃–W composites with various amounts of W (ranging from 5 vol% to 20 vol%) were fabricated by the hot-press sintering method at various sintering temperatures. Microstructure analysis revealed submicron Al₂O₃ matrix grains and W particles. The existence of three phases of Al₂O₃, W, and AlWO₄ was confirmed by X-ray diffraction patterns. All Al₂O₃–W composites showed higher fracture toughness than monolithic Al₂O₃. The toughening mechanism was attributed to crack deflection and crack bridging. Transgranular fracture was visible in all composites. Electrical resistivity dramatically lowered from 2.9 × 10¹² Ω cm of monolithic Al₂O₃ to 4.1 × 10² Ω cm of the composite with 20 vol% W addition. The percolation threshold is calculated as 18.5%. With the increase in sintering temperature, the amount of W particles was decreased and Al₂O₃ grains became large, leading to the reduced number of conductive pathways formed by the dispersed W particles. As a result, electrical conductivity was decreased.     

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.     

Effect of Al2O3 on the microstructure and mechanical properties of Ti3AlC2/Al2O3 in situ composites synthesized by reactive hot pressing

Ti₃AlC₂/Al₂O₃ in situ composites with different Al₂O₃ contents were successfully synthesized from the powder mixture of Ti, TiC, Al and TiO₂ by a reactive hot-pressing method at 1350 °C. The effect of Al₂O₃ on the microstructure and mechanical properties of the composites was investigated in detail. The results indicate that the as-fabricated products mainly consist of Ti₃AlC₂, Al₂O₃ and a small amount of TiC. With increasing the Al₂O₃ content, the flexural strength of Ti₃AlC₂/Al₂O₃ composites increase gradually, the fracture toughness reaches the peak value of 8.21 MPa m^1/2 as the Al₂O₃ content increasing to 9 wt%, the hardness attains the maximum value of 10.16 GPa for 12 wt% Al₂O_3. The strengthening mechanism of the composites was also discussed.     

Preparation of SiC reinforced Ti3SiC2-base composite and its biocompatibility evaluation

Soft Ti₃SiC₂ ceramic is a new class of potential biomaterial for orthopaedic applications and dental implants. Introducing SiC into Ti₃SiC₂ can compensate for the relatively low hardness of the Ti₃SiC₂ implants. In this study, SiC reinforced Ti₃SiC₂-base composites were fabricated by reactive sintering of powder compacts. Mechanical properties and phase constitution of the prepared samples were studied. Biocompatibility of the composite was evaluated by implanting the material onto the shaft surface of the femur of a rabbit, while, biostability was studied by immersing the material into human blood plasma and also into a simulated body fluid (Hank's) for prolonged time.     

Fabrication of TiC coated short carbon fiber reinforced Ti3SiC2 composites: Process,microstructure and mechanical properties

The C_f/Ti₃SiC₂ composites were fabricated through spark plasma sintering (SPS) and hot isostatic pressing (HIP), TiC coated C_f and Ti₃SiC₂ powder were used as starting materials. The improved fracture toughness (K_IC) and Vickers hardness (HV₁) of the TiC coated C_f/Ti₃SiC₂ composite fabricated by SPS were 7.59 MPa·m^1/2 and 7.28 GPa. On this foundation, taking the advantage of better sintering process of HIP, the highest K_IC and HV₁ achieved 8.32 MPa·m^1/2 and 9.24 GPa with fiber content of 10 vol%, which increased by 40% and 65% compared with that of monolithic Ti₃SiC₂. The reasonable control of reactive interface is the main factor for the improved mechanical properties of the composites, the TiC coating effectively protected the fiber structure from interfacial reaction compared with that of the non-coated C_f/Ti₃SiC₂. Meanwhile, the artificially designed and weakly bonded TiC coated C_f can fully exert the toughening mechanisms like fiber pull-out and debonding.     

High-temperature mechanical property and thermal shock resistance of Al2O3f/Al2O3 composites

Continuous alumina fiber–reinforced alumina matrix composites (Al₂O_3f/Al₂O₃ composites) were produced via sol–gel process, then the high-temperature mechanical property and thermal shock resistance of Al₂O_3f/Al₂O₃ composites were investigated. The results showed that the composites exhibited excellent high-temperature properties. The mechanical property of the composites was affected by heat treatment (prepared at 1100°C exhibited the most desirable mechanical property). The tensile strength of the composites abruptly decreased at higher temperatures. Although the mechanical property of the composites deteriorated after the thermal shock test was conducted at high temperatures, they exhibited excellent thermal shock resistance. After 50 thermal shock tests conducted at 1300 and 1500°C, the flexural strength of the composites was found to be 124.34 and 93.04 MPa, thus showing a decrease in strength with the increasing temperature.     

Microstructure and mechanical properties of Ti3SiC2/3Y-TZP composites by spark plasma sintering

Ti₃SiC₂/3Y-TZP (3 mol% Yttria-stabilized tetragonal zirconia polycrystal) composites were fabricated by spark plasma sintering (SPS). The effect of Ti₃SiC₂ content on room-temperature mechanical properties and microstructures of the composites were investigated. The Vickers hardness and bending strength of the composites decreased with the increasing of Ti₃SiC₂ content whereas the fracture toughness increased. The maximum fracture toughness of 9.88 MPa m^1/2 was achieved for the composite with 50 vol.% Ti₃SiC₂. The improvement of the fracture toughness is owing to the crack deflection, crack bridging, the transformation toughening effects.     

Fabrication of Ti3SiC2-based pastes for screen printing on paper-derived Al2O3 substrates

This paper describes the development and fabrication of pastes suitable for screen printing process using Ti₃SiC₂ as the ceramic filler and ethyl cellulose as the binder. With the aim of obtaining high quality screen printed films, the influence of different amounts of Ti₃SiC₂ filler (20–40?vol%) and binder (0–5?vol%) on the rheological properties of the pastes was investigated. Samples with higher viscosity, such as pastes containing 30?vol% and 40?vol% Ti₃SiC₂ filler, regardless of the amount of ethyl cellulose, showed a higher printing quality compared to the samples with other compositions. The different paste compositions were screen printed onto paper-derived Al₂O₃ substrates containing 28.6 ± 4.8% open porosity and sintered for 1?h under an argon atmosphere at 1600?°C. X-ray diffraction (XRD) measurements and scanning electron microscopy (SEM) analysis showed that the sintered films contained TiC as a primary phase and Ti₃SiC₂ as a secondary phase. The partial decomposition of Ti₃SiC₂ after sintering can be attributed to residual carbon from the organic additives, which decreases the thermal stability of this material.