B4C/TiB2 composite powders prepared by carbothermal reduction method

B₄C–(10–20 vol%)TiB₂ composite powders have been synthesized with the temperature of 1650–1800 °C by carbothermal reduction process using boron acid, carbon black and TiO₂ powder as the starting materials. B/C mole ratio of the starting materials is ascertained, thermodynamics temperature of the reactions is calculated and the effect of ball milling on the composite powders is discussed. The experimental results indicate that B/C mole ratio of the starting materials and composite powders are 4.4 and 3.98–4.03, respectively. The purity of the gained powders is more than 99 wt%. Wet ball milling eliminates the size of the B₄C/TiB₂ composite powders from 30–40 to 3–5 μm by decreasing the conglomeration of the composite powders. XRD and EDS results show that the composite powders are composed of B₄C and TiB₂.     

Mechanical properties and microstructure of TiB2–TiC composite ceramic cutting tool material

TiB₂–TiC composite ceramic cutting tool material was prepared by sintering during hot-pressing in vacuum. The effects of nano-scale Ni and Mo additives and sintering heating rate on mechanical properties and grain characteristics were investigated. TiB₂ and TiC grains exhibited prismatic and equiaxed shapes respectively. The diameter and aspect ratio of prismatic TiB₂ grains were influenced by nano-scale Ni/Mo additives. A higher heating rate could cause a higher aspect ratio of prismatic TiB₂ grains. The good mechanical properties of TN1((TiB₂–TiC)/Ni composite ceramic sintered at a heating rate of 50 °C/min) were ascribed to a relatively fine and homogenous microstructure. And a brittle B₄MoTi solid solution phase and wider distribution of grain size induced the lower flexural strength of TNM2((TiB₂–TiC)/(Ni,Mo) composite ceramic sintered at heating rate of 100 °C/min), but the higher aspect ratio of TiB₂ grains could prevent cracks from propagating and ameliorated the fracture toughness. The optimum resultant mechanical properties were obtained by (TiB₂–TiC)/Ni composite ceramic sintered at a heating rate of 50 °C/min.     

Preparation,mechanical properties and microstructure of TiB2 based ceramic cutting tool material toughened by TiC whisker

TiC whiskers were synthesized by carbothermal reduction process. By using these whiskers as the toughening phase, a novel TiB₂ based ceramic cutting tool material was prepared. Due to that the thermal expansion coefficient of TiC is close to that of TiB₂, the addition of no more than 30 vol% TiC whisker not only has little adverse effect on the density and flexure strength of the composite, but also can refine the grains, reduce the defects and improve the grain strength. As a result, both the fracture toughness and flexure strength of the TiB₂ based ceramic composite can be significantly improved. Appropriate sintering temperature and holding time can reduce defects, improve the strength of grains and grain boundaries and enhance the toughening effect of TiC whiskers. Experimental results showed that when the whisker content was 30 vol%, the sintering temperature was 1700 °C and the holding time was 30 min, the flexure strength, fracture toughness and Vickers hardness of the TiB₂ based ceramic cutting tool material was 860 MPa, 7.9 MPa·m^1/2 and 22.6GPa, respectively.     

Densification and compressive strength ofin-situ processed Ti/TiB composites by powder metallurgy

In the present study, the densification of Ti/TiB composites, the growth behavior ofin-situ formed TiB reinforcement, the effects of processing variables — such as reactant powder (TiB₂, B₄C), sintering temperature and time — on the microstructures and the mechanical properties ofin-situ processed Ti/TiB composites have been investigated. Mixtures of TiB₂ or B₄C powder with pure titanium powder were compacted and presintered at 700°C for 1 hr followed by sintering at 900, 1000, 1100, 1200, and 1300°C, respectively, for 3hrs. Some specimens were sintered at 1000°C for various times in order to study the formation behavior of TiB reinforcementin-situ formed within the pure Ti matrix. TiB reinforcements were formed through different mechanisms, such as the formation of fine TiB and the formation of coarse TiB by Ostwald ripening or the coalescence of fine TiB. There was no crystallographic relationship between TiB reinforcement and the matrix. There were voids at the interface between the TiB reinforcement and the Ti matrix due to the preferential growth of coarse TiB without a particular crystallographic relationship with pure Ti matrix and the surface energy between the Ti matrix and TiB reinforcements. Therefore, the densification of Ti/TiB₂ compacts was hindered by the preferential growth of coarse TiB reinforcements. The mechanical properties ofin-situ processed composites were evaluated by measuring the compressive yield strength at ambient and high temperatures. The compressive yield strength of thein situ processed composites was higher than that of the Ti-6A1-4V alloy. It was also found that the compressive yield strength of the composite made from TiB₂ reactant powder was higher than that of the composite made from B₄C at the same volume fraction of reinforcement. A crack path examination suggested that the bonding nature of interface between matrix and reinforcement made from TiB₂ reactant powder was better than that made from B₄C.     

Combustion synthesis of TiC–TiB2 composites

An experimental study on formation of TiC–TiB₂ in situ composites with a broad range of compositions was conducted by self-propagating high-temperature synthesis (SHS) using the reactant compacts from different combinations of Ti, B₄C, C, and B powders. Direct reaction of Ti with B₄C at stoichiometry of Ti:B₄C = 3:1 yields a TiB₂-rich composite with TiC:TiB₂ = 1:2. Formation of the products containing 20, 33.3, and 50 mol% of TiB₂ was achieved by the Ti–B₄C–C reactants. In addition, the test specimen composed of Ti, B₄C, and B was employed for the synthesis of a composite with 80 mol% TiB₂. Among three different types of the powder compacts, the boron-containing sample was characterized by the fastest combustion wave and the highest reaction temperature. The lowest combustion temperature and wave velocity were observed in the Ti–B₄C compact. When fine Ni particles were added to the Ti–B₄C reactant, it was found that the propagation rate of the reaction front was increased and the densification of the end product was enhanced significantly. This was attributed to formation of the Ti–Ni eutectic liquid during the reaction. As a result, the relative density of a TiC + 2TiB₂ composite increases from 30 to 86% with the Ni content from 0 to 20 mol%. Based upon the XRD analysis, small amounts of TiNi₃ and TiB were detected in the Ni-reinforced TiC–TiB₂ composites.     

Synthesis of B4C-Nano TiB2 Composite Powder by Sol-Gel Method

Production of (B₄C-nano TiB₂) composite powder by chemical method was evaluated in this study. Starting materials were boron carbide, carbon, and titanium (IV) iso propoxide (TTIP). Water was used as a hydrolyser agent. TTIP was hydrolyzed with water and, consequently, amorphous Ti(OH)₄ was formed. Heat-treatment of Ti(OH)₄ at 100 and 850 °C led to the production of TiO₂ and TiB₂ phases, respectively. The effect of heat-treatment time and temperature on the phase transformation and size of the produced nano powder were investigated. The produced nano powder was characterized by XRD, SEM, and DTA. It was found that heat-treatment time and temperature have significant effects on the amount and size of the produced TiB₂ powder. The data also reveal that the minimum temperature for TiB₂ formation is 650 °C.     

Pressureless Sintering of TiB<Subscript>2</Subscript>-B<Subscript>4</Subscript>C Ceramic Matrix Composite

The effect of TiB₂ addition on sinterability and mechanical properties of B₄C material was investigated. It was found that addition of TiB₂ aids the sintering process and permits pressureless sintering at temperatures between 2050 and 2150 °C. This also alleviates grain growth during sintering. The relative density reaches 98.5% of the theoretical density by increasing the percentage of TiB₂ in the composition. The mechanical properties such as hardness, fracture toughness, and bending strength were improved remarkably by addition of TiB₂.     

Microstructure evolution and densification kinetics of Al2O3/Ti(C,N) ceramic tool material by microwave sintering

The microstructure evolution and densification kinetics of Al₂O₃/Ti(C,N) ceramic tool material during microwave sintering were studied. The density and grain growth significantly increases at the temperatures higher than 1400 °C. The calculated kinetics parameter n indicates that volume diffusion is the main densification mechanism when the sintering temperature is below 1300 °C, while grain boundary diffusion plays a leading role in the densification process when the sintering temperature is higher than 1300 °C. The grain growth activation energy of Al₂O₃/Ti(C,N) composite is 48.82 KJ/mol, which is much lower than those of monolithic Al₂O₃ in the microwave sintering and conventional sintering. The results suggested that the Al₂O₃/Ti(C,N) ceramic tool material with nearly full densification and fine grains can be prepared by two-step microwave sintering.     

Flexural strength behavior of a ZrB2–TaB2 composite consolidated by non-reactive spark plasma sintering at 2300 °C

A bulk zirconium–tantalum diboride ceramic composite was consolidated by non-reactive spark plasma sintering (SPS) at 2300 °C. In order to consolidate the ZrB₂–44 wt% TaB₂ composite and restrict grain-growth, a special loading procedure was used. Pressure was applied and released at 2150 °C and 1250 °C, respectively. These SPS conditions allowed us to obtain a crack-free bulk composite with a grain size of 4–8 μm. Flexural strength at temperatures up to 1800 °C was measured for the ZrB₂–TaB₂ composite. Importantly, at 1600 °C, the strength was 336 ± 23 MPa, which is superior to that of monolithic ZrB₂. Moreover, the ZrB₂–TaB₂ composite only showed plastic behavior at 1800 °C, a finding that is atypical for ZrB₂-based ceramics.     

Investigation on Addition of Kaolinite on Sintering Behavior and Mechanical Properties of B4C

The objective of the present investigation was to study the effect of kaolinite addition on sintering behavior and mechanical properties of pressureless sintered B₄C ceramic. Different amounts of kaolinite, mainly 5 to 30 wt.%, were added to the base material. The in situ reaction of kaolinite with B₄C generates SiC and Al₂O₃, which aid the sintering process and permit pressureless sintering at temperatures between 2050 and 2150 °C. Addition of 30 wt.% kaolinite and sintering at 2150 °C resulted in improving the density of the samples to about 98.5% of the theoretical density. The composite samples exhibited very good mechanical properties (hardness, flexural strength, and fracture toughness). As wt.% Kaolinite increases, strength and toughness increase, and hardness first increases and then decreases.     

Microstructure and mechanical properties of TiB2–SiC ceramic composites by Reactive Hot Pressing

TiB₂–SiC ceramic composites with different contents of Ni as additive were prepared by the Reactive Hot Pressing (RHP) process at 1700 °C under a pressure of 32 MPa for 30 min. For comparison, a monolithic TiB₂ ceramic and TiB₂–SiC ceramic composite were also fabricated under the identical temperature, pressure and holding time by the Hot Pressing (HP) process. The effects of the fabrication process and Ni on the microstructure and mechanical properties of the composites were investigated. About 8 vol.% of elongated TiB₂ grains with an aspect ratio of 3–6 and a diameter of 0.5–1 μm were produced in the composite prepared by the RHP process. The improvement of the fracture toughness was attributed to the toughening and strengthening effects of SiC particles and the elongated TiB₂ grains such as crack deflection. The TiB₂–SiC–5 wt.% Ni ceramic composite had the optimum mechanical properties with a flexural strength of 858 ± 87 MPa, fracture toughness of 8.6 ± 0.54 MPa·m^1/2 and hardness of 20.2 ± 0.94GPa. The good mechanical properties were ascribed to the relatively fine and homogeneous microstructure and the strengthening effect of Ni. Ni inhibited the anisotropic growth of TiB₂.     

Investigation on microstructure and mechanical properties of HfB2-SiC-HfC ternary system with different HfC content prepared by spark plasma sintering

HfB₂-based ultrafine composites with 25 vol% SiC and various volume fractions of HfC (5–20 vol%) have been successfully fabricated using spark plasma sintering. The composites were sintered in both 1800 °C and 1850 °C for different soaking times of 5 and 15 min and flexural strength, hardness and fracture toughness of specimens were measured. Sintering mechanism and mechanical properties of composites and HfC impact on them were investigated. The highest relative density (99.97 ± 0.02%) and the lowest apparent porosity (0.07 ± 0.03) were obtained for the specimen with 15 vol% of HfC. This composite also showed the maximum flexural strength (592 ± 17 MPa) and fracture toughness (4.98 ± 0.12 MPam^1/2), even more than the composite with 20 vol% of HfC which had the highest Vickers hardness (22.7 ± 0.9 GPa).     

Wetting and interfacial phenomena in Ni–HfB2 systems

The wettability and reactivity between polycrystalline hot-pressed HfB₂ and liquid Ni, Ni–Ti and Ni–B alloys have been investigated by the sessile drop method up to 1520 °C. Independently of the sintering aids (B₄C, HfSi₂), high-temperature interactions led to the formation of a bimodal interface profile, due to the competition between the strong dissolution of HfB₂ in the liquid phase and drop spreading along the substrate surface. Ni demonstrates good wetting with the HfB₂ substrates (θ = 20°). Compared to Ni, high Ti-containing alloys reveal much faster wettability kinetics with a final contact angle below 10°, accompanied by the formation of an interfacial Ti-rich reaction product. The eutectic NiB alloy shows complete wetting and fast spreading on HfB₂ and minor dissolution of the ceramic into the liquid, a clear indication that higher B contents could optimize the interfacial structure. These results are of practical interest for liquid-assisted composite synthesis and joining of HfB₂-based ceramics.     

Reaction synthesis of TiB2–TiC composites with enhanced toughness

In situ toughened TiB₂–TiC_x composites were fabricated using reaction synthesis of B₄C and Ti powders at high temperatures. The resulting materials possessed very high relative densities and well developed TiB₂ plate-like grains, leading to a rather high fracture toughness, up to 12.2 MPa⋅m^1/2. The microstructure was examined by means of XRD, SEM, TEM and EDAX. The reaction products mainly consisted of TiB₂ and TiC_x. No other phases, e.g. Ti₃B₄, TiB, Ti₂B₅ and free Ti, were observed regardless of whether the starting composition was Ti:B₄C=3:1 or 4.8:1, and whether the sintering temperature was 1700 or 1800°C. The microstructural morphology is characterised by TiB₂ plate-like grains distributed uniformly in the TiC_x matrix. Some inclusions and defects were found in TiB₂ grains. The very high reaction temperature was believed to be responsible for the formation of plate-like grains, which, in turn, is responsible for the much improved mechanical properties. The main toughening mechanisms were likely to be crack deflection, platelet pull-out and the micro-fracture of TiB₂ grains.     

Microstructure and properties of laser cladded B4C/TiC/Ni-based composite coating

In order to study the effect of TiC/B₄C ceramic particles on the microstructure evolution and microhardness of Ni204-based cladding coating, TiC/B₄C/Ni204-based composite coatings were fabricated by laser cladding. The results showed that the TiC ceramic particles in the 30%TiC+70%Ni204 coating do not decompose. TiC is the main reinforcing phase in the coating; however, in 30%B₄C + 5%TiC+65%Ni204 composite coating, TiB₂ phase was in situ synthesized, and graphite, Fe₂B, Ti-Mo-Nb, (Ti, Nb, Mo)(B, C) were formed simultaneously in the coating. The addition of TiC promoted the dissolution and reaction of B₄C. In the presence of 30%TiC, the average microhardness and friction coefficient of the coating were 966.4 HV_0.5 and 0.198, respectively, which were 3.23 and 0.281 times of the initial Ni204 coating. In the presence of 30%B₄C and 5%TiC, the average microhardness and friction coefficient of the coatings were 1308.2HV_0.5 and 0.530, respectively, which were 4.38 and 0.752 times of the initial coatings. The enrichment of TiC is proportional to the hardness of the coating.     

Effects of Y2O3 on SiC/MoSi2 composite by mechanical-assistant combustion synthesis

MoSi₂ based materials are considered as a potential high temperature structural parts. In this work, a 0.5 wt% Y₂O₃–20 vol% SiC/MoSi₂ composite was successfully prepared by pressureless sintering from mechanical-assistant combustion synthesized powders. Adding a small amount of Y₂O₃ to the SiC/MoSi₂ composite decreased the apparent activation energy of sintering by 10.4%, resulting in a denser composite with finer grains. The relative density, flexural strength, Vickers hardness and fracture toughness of 0.5 wt% Y₂O₃–20 vol% SiC/MoSi₂ increased by 5.3%, 27.7%, 27.2% and 35.8% as compared to 20 vol% SiC/MoSi₂, respectively. The oxidation mass gain of Y₂O₃–20 vol% SiC/MoSi₂ at 1200 °C was higher than that of 20 vol% SiC/MoSi₂ for 16.9%, while it still exhibited very good oxidation resistance at this temperature.     

Effect of ZrB2 and SiC addition on TiB2-based ceramic composites prepared by spark plasma sintering

TiB₂-based ceramic composites with different amounts of ZrB₂ and SiC were prepared by spark plasma sintering at 1700 °C with an initial pressure of 40 MPa and a holding time of 10 min. The (Ti_xZr_y)B₂ solid solution was found in the sintered TiB₂/ZrB₂/SiC composites by XRD. The microstructural and mechanical properties of the prepared samples were investigated. The composite with the addition of 30 vol.% ZrB₂ shows better comprehensive performances, and the bending strength and the fracture toughness of the composite are 780.5 MPa and 7.34 MPa m^1/2, respectively. The generation of the (Ti_xZr_y)B₂ solid solution makes the microstructures of the composites finer and more homogeneous, which has played a very important role in grain refinement and interface fusion.     

Microstructural characterization and mechanical behaviours of TiN-graphite composites fabricated by spark plasma sintering

The effects of milling time on the particle size distribution (PSD), densification, microstructure, hardness and fracture toughness of spark plasma sintered (SPS) TiN+graphite ceramic were studied. TiN with varying amount of graphite (1, 3, and 5 wt%) were milled at different milling time (8, 24 and 40 h), thereafter sintered at sintering temperature of 1800 °C, holding time of 10 min and pressure of 50 MPa. The relative density and hardness increased as milling time progressed from 24 to 40 h, however, the relative density, hardness, and particle size decreased after 8 h of milling. The microstructural analyses showed that a fully sintered TiN+graphite compact could be achieved at sintering temperature of 1800 °C, with no significant grain growth. Residual stress effect of TiN+5 wt% graphite composite was analyzed using XRD method and the result indicated that there is no significant residual stress on the sample. The relative density, Vickers hardness and fracture toughness of TiN+ 1 wt% Gr, milled for 40 h were 99.24%, 13.90 GPa and 4.0 MPa.m^1/2 respectively.     

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.     

通过调整润湿性开发具有高抗损伤性能的仿珍珠贝壳层状2024Al/B4C复合材料

为了解决复合材料中B4C陶瓷相难以被金属铝润湿的问题,利用TiH2和B4C的原位反应引入TiB2,进而调节其润湿性和界面结合.通过将熔融合金压力浸渗到冷冻铸造法制备的多孔陶瓷支架中,制备具有层状结构的2024Al/B4C?TiB2复合材料.与2024Al/B4C复合材料相比,加入TiH2后复合材料的抗弯强度和裂纹扩展韧...