A new TiB2 + CrSi2 composite – Densification,characterization and oxidation studies

A new composite of TiB₂ with CrSi₂ has been prepared with excellent oxidation resistance. Dense composite pellets were fabricated by hot pressing of powder mixtures. Microstructural characterization was carried out by XRD and SEM with EDAX. Mechanical and physical properties were evaluated. Extensive oxidation studies were also carried out. A near theoretical density (99.9% TD) was obtained with a small addition of 2.5 wt.% CrSi₂ by hot pressing at 1700 °C under a pressure of 28 MPa for 1 h. The microstructure of the composite revealed three distinct phases, (a) dark grey matrix of TiB₂, (b) black phase – rich in Si and (c) white phase – Cr laden TiB₂. Hardness and fracture toughness were measured as 29 ± 2 GPa and 5.97 ± 0.61 MPa m^1/2, respectively. Crack branching, deflection and bridging mechanisms were responsible for the higher fracture toughness. With increase in CrSi₂ content, density, hardness and fracture toughness values of the composite decreased. Thermo gravimetric studies revealed the start of oxidation of the composite at 600 °C in O₂ atmosphere. Isothermal oxidation of these composites showed better oxidation resistance by formation of a protective oxide layer. TiO₂, Cr₂O₃ and SiO₂ phases were identified on the oxidized surface. Effects of CrSi₂ content, temperature and duration of oxidation on the oxide layer formation are reported. Activation energy of the composite was calculated as ∼110 kJ/mol using Arrhenius equation. Diffusion controlled mechanism of oxidation was observed in all the composites.     

Effects of sintering additives on microstructure and mechanical properties of TiB2-WC ceramic-metal composite tool materials

TiB₂-WC ceramic-metal composite tool materials were fabricated using Co, Ni and (Ni, Mo) as sintering additives by vacuum hot-pressing technique. The microstructure and mechanical properties of the composite were investigated. The composite was analyzed by the observations of scanning electron microscope (SEM), X-ray diffraction (XRD) and energy dispersive spectrometry (EDS). The microstructure of TiB₂-WC ceramic-metal composites consisted of the fine WC grains and uniform TiB₂ grains. The brittle phase of Ni₃B₄ and a few pores were found in TiB₂-WC-Ni ceramic-metal composite. A lot of pores and brittle phases such as W₂CoB₂ and Co₂B were formed in TiB₂-WC-Co ceramic-metal composite. The liquid phase of Co was consumed by the reaction which led to the formation of the pores and the coarse grains of TiB₂. The pores, brittle phases and coarse grains of TiB₂ were harmful to the improvement of the mechanical properties of the composite. The sintering additive of (Ni, Mo) had a significant effect on the density and the mechanical properties of TiB₂-WC ceramic-metal composite. The formation of intermetallic compound of MoNi₄ inhibited the consumption of liquid phase of (Ni, Mo). The liquid phase of (Ni, Mo) not only inhibited the formation of the pores and the coarse grains of TiB₂ but also strengthened the interface energy between WC and TiB₂ grains. The grain size was fine and the average relative density of TiB₂-WC-(Ni, Mo) ceramic-metal composite reached 99.1%. The flexural strength, fracture toughness and Vickers hardness of TiB₂-WC-(Ni, Mo) ceramic-metal composite were 1307.0 ± 121.4 MPa, 8.19 ± 0.29 MPa m^1/2 and 22.71 ± 0.82 GPa, respectively.     

Synthesis and consolidation of TiN/TiB2 ceramic composites via reactive spark plasma sintering

The simultaneous synthesis and densification of TiN/TiB₂ ceramic composites via reactive spark plasma sintering (RSPS) was investigated. Different component ratios (TiH₂/BN (TiN, B)) and heating rates (112.5-300 °C/min) were used to initiate the chemical reaction for TiN/TiB₂ synthesis. The omit RSPS process was revealed to have three stages, which are described separately. The relationships between the RSPS conditions, the microstructure and the properties of sintered ceramic composites were established. A Vickers hardness of 16-25 GPa and a fracture toughness of 4-6.5 MPa m^1/2 were measured for various compositions. Sintered ceramic composites containing 36 wt% TiB₂ with the highest relative density of 97.4 ± 0.4% and an average grain size of 150-550 nm have been obtained.     

Investigations on synthesis of ZrB2 and development of new composites with HfB2 and TiSi2

This paper presents the results of experimental investigations carried out on the synthesis of pure ZrB₂ by boron carbide reduction of ZrO₂ and densification with the addition of HfB₂ and TiSi₂. Process parameters and charge composition were optimized to obtain pure ZrB₂ powder. Monolithic ZrB₂ was hot pressed to full density and characterized. Effects of HfB₂ and TiSi₂ addition on densification and properties of ZrB₂ composites were studied. Four compositions namely monolithic ZrB₂, ZrB₂ + 10% TiSi₂, ZrB₂ + 10% TiSi₂ + 10% HfB₂ and ZrB₂ + 10% TiSi₂ + 20% HfB₂ were prepared by hot pressing. Near theoretical density (99.8%) was obtained in the case of monolithic ZrB₂ by hot pressing at 1850 °C and 35 MPa. Addition of 10 wt.% TiSi₂ resulted in an equally high density of 98.9% at a lower temperature (1650 °C) and pressure (20 MPa). Similar densities were obtained for ZrB₂ + HfB₂ mixtures also with TiSi₂ under similar conditions. The hardness of monolithic ZrB₂ was measured as 23.95 GPa which decreased to 19.45 GPa on addition of 10% TiSi₂. With the addition of 10% HfB₂ to this composition, the hardness increased to 23.08 GPa, close to that of monolithic ZrB₂. Increase of HfB₂ content to 20% did not change the hardness value. Fracture toughness of monolithic sample was measured as 3.31 MPa m^1/2, which increased to 6.36 MPa m^1/2 on addition of 10% TiSi₂. With 10% HfB₂ addition the value of K_IC was measured as 6.44 MPa m^1/2, which further improved to 6.59 MPa m^1/2 with higher addition of HfB₂ (20%). Fracture surface of the dense bodies was examined by scanning electron microscope. Intergranular fracture was found to be a predominant mode in all the samples. Crack propagation in composites has shown considerable deflection indicating high fracture toughness. An oxidation study of ZrB₂ composites was carried out at 900 °C in air for 64 h. Specific weight gain vs time plot was obtained and the oxidized surface was examined by XRD and SEM. ZrB₂ composites have shown a much better resistance to oxidation as compared to monolithic ZrB₂. A protective glassy layer was seen on the oxidized surfaces of the composites.     

Characterization and properties of quaternary Mo-Si-C-N coatings synthesized by magnetron sputtering technique

In this paper the direct current unbalanced reactive magnetron sputtering and composite target techniques were exploited to deposit quaternary Mo-Si-C-N coatings on Si wafer and stainless steel (1Cr18Ni9) in an Ar/N₂ gaseous mixture. The chemical composition, microstructure, morphology, hardness, and friction coefficient of these films were characterized by means of X-ray diffraction, XPS, field emission scanning electron microscopy, TEM and nanoindentation. With the increase of C content in the range of C/(C + Mo + Si + N) = 0-12 at.%, the crystallite size decreases from 32 nm to 5 nm and the average friction coefficient of Mo-Si-C-N coatings decreases from 0.24 to 0.17, while the hardness increases at first and then decreases after passing a maximum value of about 27 GPa at 9 at.% C. It was suggested that in the Mo-Si-C-N coatings C atoms substitute for the N atoms in the nano-sized crystalline Mo₂N to form Mo₂N(C) solid solution phase and the microstructure of the Mo-Si-C-N coatings may be nano-sized crystalline Mo₂N(C) embedded in the amorphous SiNx and CNx phases.     

Densification and mechanical properties of fine-grained Al2O3-ZrO2 composites consolidated by spark plasma sintering

Alumina matrix composites containing 5 and 10 wt% of ZrO₂ were sintered under 100 MPa pressure by spark plasma sintering process. Alumina powder with an average particle size of 600 nm and yttria-stabilized zirconia with 16 at% of Y₂O₃ and with a particle size of 40 nm were used as starting materials. The influence of ZrO₂ content and sintering temperature on microstructures and mechanical properties of the composites were investigated. All samples could be fully densified at a temperature lower than 1400 °C. The microstructure analysis indicated that the alumina grains had no significant growth (alumina size controlled in submicron level 0.66-0.79 μm), indicating that the zirconia particles provided a hindering effect on the grain growth of alumina. Vickers hardness and fracture toughness of composites increased with increasing ZrO₂ content, and the samples containing 10 wt% of ZrO₂ had the highest Vickers hardness of 18 GPa (5 kg load) and fracture toughness of 5.1 MPa m^1/2.     

Bulk WC-Al2O3 composites prepared by spark plasma sintering

WC and WC-Al₂O₃ materials without metallic binder addition were densified by spark plasma sintering in the range of 1800-1900 °C. The densification behavior, phase constitution, microstructure and mechanical properties of pure WC and WC-Al₂O₃ composite were investigated. The addition of Al₂O₃ facilitates sintering and increases the fracture toughness of the composites to a certain extent. An interesting phenomenon is found that a proper content of Al₂O₃ additive helps to limit the formation of W₂C phase in sintered WC materials. The pure WC specimen possesses a hardness (HV₁₀) of 25.71 GPa, fracture toughness of 4.54 MPa·m^1/2, and transverse fracture strength of 862 MPa, while those of WC-6.8 vol.% Al₂O₃ composites are 24.48 GPa, 6.01 MPa·m^1/2, and 1245 MPa respectively. The higher fracture toughness and transverse fracture strength of WC-6.8 vol.% Al₂O₃ are thought to result from the reduction of W₂C phase, the crack-bridging by Al₂O₃ particles and the local change in fracture mode from intergranular to transgranular.     

Effect of ultrasonic vibration on microstructural evolution of the reinforcements and degassing of in situ TiB2p/Al-12Si-4Cu composites

Some issues such as clustering of TiB₂ particles, formation of long rod-like Al₃Ti particles, as well as high porosity level usually associate with the fabrication of in situ TiB_2p/Al-alloy composites via conventional stir casting technique using Ti and B as reactants. High-intensity ultrasonic vibration was introduced in our research to solve the above issues. The process involved that the original in situ TiB_2p/Al-12Si-4Cu sample with large clusters of TiB₂ particles, large long rod-like Al₃Ti particles and high porosity was remelted at 850 °C, and then ultrasonic vibration was applied to the melt with an ultrasonic probe. The microstructural evolution of the samples treated by ultrasonic vibration with different time was examined by using SEM. After treated by ultrasonic vibration for 12 min, large clusters of TiB₂ particles were broken up effectively and TiB₂ particles were dispersed uniformly in the matrix, and long rod-like Al₃Ti particles were turned into blocky ones with the size of 10 μm due to the effect of ultrasonic stirring. In the meantime, the porosity in the composites decreased from about 6.5% to 0.86% due to the effect of ultrasonic degassing. Microhardness test suggested that a homogeneous microstructure of the composite was achieved after ultrasonic treatment. An effective approach using high-intensity ultrasonic vibration to optimize the microstructures of the particulate reinforced Al-alloy composites was proposed, and the mechanism of the effect of high-intensity ultrasonic vibration on the microstructural evolution of the reinforcements and degassing of composites was also discussed in our research.     

The study of NiAl-TiB2 coatings prepared by electro-thermal explosion ultrahigh speed spraying technology

NiAl-TiB₂ composite coatings with 0, 10 and 20 wt.% TiB₂ were synthesized on the Ni-based superalloy substrate using electro-thermal explosion ultrahigh speed spraying technology. The microstructure analysis shows that the coatings consist of submicron grains. The bond between coatings and substrate is metallic cohesion. TiB₂ as a powerful reinforcement is doped in NiAl for increasing its hardness. The isothermal oxidation test is carried out for the composite coatings at 1100 °C in air. The result shows that the oxidation resistance of NiAl coating is higher than that of NiAl-10TiB₂ and NiAl-20TiB₂ coatings. The phases of oxides on the coatings during the process at high temperature have been analyzed by X-ray diffraction. The results show that Al₂O₃ and Cr₂O₃ coexistence on surface of NiAl coating, while Al₂O₃, Cr₂O₃, TiO₂ and a small amount of NiO form on surface of NiAl-10TiB₂ and NiAl-20TiB₂ coatings after oxidation for 4 h.     

Oxidation resistance and mechanical property of cosputtered quasi-amorphous Ta-Si-N films under vacuum rapid thermal annealing

The oxidation resistance and mechanical properties of Ta-Si-N films at high temperature are important issues for application. In this paper, quasi-amorphous Ta-Si-N thin films were fabricated by using reactive magnetron co-sputtering at different Si/Ta power ratios and nitrogen flow ratios (FN₂% = FN₂/(FAr + FN₂) × 100%). Vacuum rapid thermal annealing at 600-900 °C at 2.6 Pa was performed to investigate the oxidation resistance of films. At the higher Si/Ta power ratio and increased FN₂%, there is low oxygen fraction (O/(O + N) ≤ 0.2) of films at high annealing temperature which corresponds to benefit oxidation resistance. The crystalline δ-Ta₂O₅ phase was formed at 900 °C for all films. The islands of oxide were formed on the surface of films at low-Si-content (≤ 20 at.%) after 900 °C annealing. The hardness of all as-deposited Ta-Si-N films was between 16 and 24 GPa. The low-Si-content Ta-Si-N films has higher hardness than high-Si-content (≥ 20 at.%) ones due to lower fraction of soft amorphous SiN_x. The effect of annealing temperature on the correlation among process parameters, microstructure, phase transformation and hardness is discussed. The Ta-Si-N formed at 6 FN₂% and Si/Ta power ratio of 2/1 can be the best candidate for good oxidation resistance with appropriate mechanical property.     

Synthesis of Ti3SiC2 by infiltration of molten Si

High-purity Ti₃SiC₂ compounds have been fabricated by infiltration of molten Si into a precursor, a partially sintered TiC_x (x = 0.67) preform. The Si source and the TiC_x preform were placed side by side on carbon cloth, and the system was heated to 1550 °C. Molten Si infiltrated the preform through the carbon cloth, and a direct reaction between TiC_x and molten Si immediately occurred at the reaction temperature to yield pure Ti₃SiC₂. We could observe phase formation and the microstructure of the bulk products with time, which were investigated by X-ray diffraction (XRD) and scanning electron microscopy (SEM) equipped with energy-dispersive spectroscopy (EDS). Pure Ti₃SiC₂ compounds were formed on the exterior of the TiC_x preform at 1550 °C when the sintered TiC_x:Si ingot molar ratio was 3:1.4. At 1550 °C, no other minor phases were detected for any of the sintering time ranges.     

Thermal and electrical properties of TiB2–MoSi2

The present communication reports the effect of MoSi₂ addition on high temperature thermal conductivity and room temperature (RT) electrical properties of TiB₂. The thermal diffusivity and the thermal conductivity of the hot pressed TiB₂–MoSi₂ samples were measured over a range from room temperature to 1000 °C using the laser-flash technique, while electrical resistivity was measured at RT using a four linear probe method. The reciprocal of thermal diffusivity of TiB₂ samples exhibit linear dependence on temperature and the measured thermal conductivity of TiB₂-2.5% MoSi₂ composites correlate well with the theoretical predictions from Hashin’s model and Hasselman and Johnson’s model. A common observation is that the thermal conductivity of all the samples slightly increases with temperature (up to 200 °C) and then decreases with further increasing temperature. It is interesting to note that both the thermal conductivity and electrical conductivity of TiB₂ samples enhanced with the addition of 2.5 wt.% MoSi₂ sinter additive. Among all the samples, TiB₂-2.5 wt.% MoSi₂ ceramics measured with high thermal conductivity (77 W/mK) and low electrical resistivity (12 μΩ-cm) at room temperature. Such an improvement in properties can be attributed to its high density and low volume fraction of porosity. On the other hand, both the thermal and electrical properties of TiB₂ were adversely affected with further increasing the amount of MoSi₂ (10 wt.%).     

Thermal plasma CVD and wear resistance of double layered Ti-Si-B-C/Ti-B-C coatings on WC-Co cutting tools with various roughness

The double-layer deposition of composite SiC-TiBC (Ti-Si-B-C) films with various Si contents (0, 40, 55, 60 and 100 mol%) on Ti-B-C was achieved from mixtures of titanium tetra-ethoxide, boron tri-ethoxide, and/or hexa-methyl-disiloxane solutions at about 700 °C on WC-Co cutting tools by Ar/H₂ thermal plasma CVD. The crystalline phases of TiB₂, TiC, and SiC were identified in the coatings by thin film grazing incidence X-ray diffraction. The surfaces and cross-sections of the double-layer coatings were observed by scanning electron microscopy to reveal their microstructure. Cutting tests of the double-layer Ti-Si-B-C/Ti-B-C were carried out by determining the flank and crater wear. The wear rate of the double-layer formed with the Ti-Si-B-C composite over-layer with 55 mol% Si was the slowest of the five samples. In addition, the effect of surface roughnesses (Ra (μm) = 0.03, 0.20 and 0.55) on the coating and wear resistance of the double-layer Ti-Si-B-C/Ti-B-C with 55 mol% Si was investigated by cross-sectional SEM observation and cutting tests.     

Thixoforming of AA 2017 aluminum alloy composites

A comparative evaluation has been carried out on the microstructure of aluminum based SiC and Al₂O₃ particle reinforced composites produced by semi-solid direct squeeze forming of composite powder at temperatures of 635-645 °C. The study is focused on the distribution of the reinforcement and the intermetallic phases, the porosity content, the microstructure of the matrix phase, the interfacial state and mechanical properties. The particle size of the reinforcements, the time of the high-energy ball milling procedure for the fabrication of composite powder and the semi-solid forming temperature had a strong influence on the quality of sample in terms of distribution of reinforcement and interfacial interaction. Ball milling improves the interface formation between reinforcement and matrix and influences the remelting behaviour. Increasing ball milling time and decreasing semi-solid forming temperature with isothermal holding time resulted in relatively homogenous microstructures and in a reduced amount of interaction between SiC and metal matrix. Best results were obtained for 5 vol.% SiC_p composites after 3 h ball milling, semi-solid formed at 635 °C and held for 10 min.     

Chemical structure and mechanical properties of Si-containing a-C:H and a-C thin films and their Cr- and W-containing derivatives

Si-containing a-C:H and a-C thin films with nitrogen, oxygen and transition metal (Cr and W) additives were deposited on polished single crystalline silicon substrates at room temperature by plasma activated CVD, magnetron-sputtering PVD and also by combined PACVD-PVD techniques.In particular Si-, Si-O- and Si-N-containing a-C:H films (denoted as a-C-Si, a-C-Si-O and a-C-Si-N) were deposited respectively from tetramethylsilane (TMS), hexamethyldisiloxane and hexamethyldisilazane vapourised precursors in He carrier gas by electron cyclotron wave resonance RF plasma. Cr-containing a-C:H films, further denoted as a-C-Si-Cr, were deposited with combined PVD-PACVD by sputtering chromium and carbon targets in argon and introducing TMS vapour. Wcontaining a-C films (denoted as a-C-Si-W) were deposited by PVD with simultaneous sputtering of the constituents in Ar. Detailed characterisation of the composition and chemical state of the elements present in the films were done by X-ray photoelectron spectroscopy (XPS) and X-ray induced Auger electron spectroscopy. Mechanical properties, hardness (H), reduced modulus (E) and scratch behaviour were studied by depth-sensing nanoindentation and scratch tests.In the a-C:H films, the C/Si ratio varied between 1.5 and 3.5 showing a significant deficiency of C as compared to the composition of the precursors. The Cr and W content in the a-C-Si-Cr and a-C-Si-W films varied in a very broad 2-50 at.% range.The chemical state of carbon was primarily of sp² and partly of sp³ type C-C with XPS chemical shifts for C 1s at 284.3 eV and 285.0 eV, respectively. The Si in the films is bonded predominantly to carbon (Si 2p at 100.8 eV BE) or to nitrogen in N-containing films (Si 2p at 101.3 eV BE). In the a-C-Si-Cr films Cr-C bonding states were determined (Cr 2p_3/2 at 574.5 eV and C 1s at 282.8 eV). Si formed predominantly Si-C and also Si-Cr bonds. In the a-C-Si-W, films C-Si and C-W (W 4f_7/2 at 32.3 eV) chemical bonds could be identified.It was discovered that the modified Auger parameter for silicon, α_Si (derived from the Si 2p electron and Si KLL Auger line energy), sensitively reflects the entire chemical structure of these films, including crosslinking and densification. These spectroscopic data, supported further by the increase of the bulk plasmon loss energy of the C 1s peak, were directly connected with the mechanical properties of these films. The amorphous nature of the films was deduced from the chemical state analysis and was verified also by transmission electron microscopy (TEM) and electron diffraction (ED) studies.Hardness and elastic modulus of the a-C-Si-(O,N) films could be adjusted in a wide range of approx. 5-15 GPa and 40-140 GPa, respectively. Systematic alteration of these values with the composition (C/Si, O/Si and N/Si atomic ratio) and with the chemical structure (α_Si?) was established and their interrelations are discussed. Whilst incorporation of Cr does not alter the mechanical properties, the addition of W increases H and E up to 19 GPa and 210 GPa, respectively.     

Phase constituents and microstructure of laser cladding Al2O3/Ti3Al reinforced ceramic layer on titanium alloy

Laser cladding of the Fe₃Al + TiB₂/Al₂O₃ pre-placed alloy powder on Ti-6Al-4V alloy can form the Ti₃Al/Fe₃Al + TiB₂/Al₂O₃ ceramic layer, which can greatly increase wear resistance of titanium alloy. In this study, the Ti₃Al/Fe₃Al + TiB₂/Al₂O₃ ceramic layer has been researched by means of electron probe, X-ray diffraction, scanning electron microscope and micro-analyzer. In cladding process, Al₂O₃ can react with TiB₂ leading to formation of amount of Ti₃Al and B. This principle can be used to improve the Fe₃Al + TiB₂ laser cladded coating, it was found that with addition of Al₂O₃, the microstructure performance and micro-hardness of the coating was obviously improved due to the action of the Al-Ti-B system and hard phases.     

Reactive spark plasma sintering of TiB2–SiC–TiN novel composite

The effects of adding SiC as a reinforcement and TiN as an additive on TiB₂-based composites fabricated by the spark plasma sintering (SPS) technique were investigated. SPS was implemented at the sintering conditions of 1900 °C temperature, 7 min holding time and 40 MPa pressure. Adding these two secondary phases had noticeable effects on the microstructure of TiB₂-based composites. A relative densities of 99.9% was obtained for TiB₂–SiC–TiN composite. Detection of in-situ formed phases and investigation on them were done using SEM, XRD, EDS and thermodynamic assessment. These evaluations proved the formation of in-situ phases of TiC, BN nano-platelets, TiSi and B₄C in the TiB₂-based composite codoped with SiC and TiN. Formation of these in-situ phases had fascinating effects on the sinterability and ultimate microstructure of titanium diboride.     

Microstructure and properties of W-ZrC composites prepared by the displacive compensation of porosity (DCP) method

Tungsten-zirconium carbide composites were fabricated at different temperatures by the displacive compensation of porosity (DCP) method, the microstructure, mechanical properties, and ablation resistance were investigated. It was found that no WC phase was left in the composites prepared at 1400 °C, and a few residual W₂C particles were surrounded in W product. Microstructure analyses revealed that zirconium atoms diffused into tungsten carbide to form ZrC and W₂Zr besides carbon diffused into the Zr₂Cu melt. Composites fabricated at 1400 °C had a flexural strength of 356.7 ± 15.2 MPa, an elastic modulus of 193.7 ± 9.8 GPa, a fracture toughness of 7.0 ± 0.7 MPa m^1/2, and a hardness of 13.6 ± 0.7 GPa. After ablated by an oxyacetylene flame for 30 s, the higher temperature prepared composites had a better ablation resistance, the linear ablation rate was 0.0033 ± 0.0004 mm/s, and the mass ablation rate was 0.0012 ± 0.0001 g/s.     

Electrochemical boriding of titanium for improved mechanical properties

In this study, we introduce a rapid boriding technique that can produce very thick titanium diboride (TiB₂) layers on titanium substrates. We also discuss the effects of process duration on boride layer thickness, chemistry and, morphology. In our experiments, the boriding of commercial purity titanium (CP-Ti) substrates was carried out in an electrochemical cell in which we used a mixture of sodium tetraborate and sodium carbonate as the base ingredients of molten electrolyte at 950 °C and at current density of 300 mA/cm². The titanium test pieces were attached to the cathode holder of the electrochemical cell while a graphite crucible served as the anode. Both TiB and TiB₂ phases were detected by X-ray diffraction method even after 5 min of treatment. Scanning electron microscopy (SEM) images verified that the production of 4.5 µm thick TiB₂ layers was feasible after boriding for an hour. The boride layers consisted of a homogeneous TiB₂ phase on the top and TiB whiskers toward the substrate. The micro-indentation studies indicated that the layer on top has hardness values as high as 40 GPa. The main advantages of this technique are its ability to produce very thick and hard TiB₂ quickly and to create no gaseous emissions or solid wastes during or after the treatment.     

Titanium diboride composite with improved sintering characteristics

Titanium diboride (TiB₂) and its ceramic composites were prepared by hot pressing process. The sintering process, phase evolution, microstructure and mechanical properties of TiB₂ ceramics prepared by using different milling media materials: tungsten carbide (WC/Co) or SiAlON was studied. It was found that the inclusion of WC/Co significantly improved the sinterability of the TiB₂ ceramics. A core/rim structure with pure TiB₂ as the core and W-rich TiB₂, i.e. (Ti,W)B₂ as the rim was identified. Microstructure analysis revealed that this core/rim structure was formed through a dissolution and re-precipitation process. In addition, silicon carbide (SiC) was also introduced to form TiB₂–SiC composites. The addition of SiC as the secondary phase not only improved the sinterability but also led to greatly enhanced fracture toughness. The optimum mechanical properties with Vickers hardness ~ 22 GPa, and fracture toughness ~ 6 MPa m^1/2 were obtained on TiB₂–SiC composites milled with WC/Co.