Synthesis of high pure Ti3AlC2 and Ti2AlC powders from TiH2 powders as Ti source by tube furnace

Titanium aluminum carbide (Ti₃AlC₂ and Ti₂AlC) powders were synthesized from TiH₂ powders instead of Ti powders as Ti source by a tube furnace under argon atmosphere without preliminary dehydrogenation. 95 wt% pure Ti₃AlC₂ powders were synthesized from TiH₂/1.1Al/2TiC at 1 450 °C for 120 min. High-purity Ti₂AlC powders were also prepared from 3TiH₂/1.5Al/C and 2TiH₂/1.5Al/TiC powders at 1 400 °C for 120 min. The as-synthesized samples were porous and easy to be ground into powders. Sn or Si additives in starting materials increased the purity of synthesized Ti₃AlC₂ obviously and expanded the temperature range for the synthesis of Ti₃AlC₂. With Si or Sn as additives, high pure Ti₃AlC₂ was synthesized at 1 200 °C for 60 min from TiH₂/x Si/Al/2TiC and TiH₂/x Sn/Al/2TiC (x = 0.1, 0.2), respectively.     

Physical, antioxidant and thermal shock properties of Cu/Ti2AlC conductive composites

Cu/Ti₂AlC composites were fabricated by vacuum hot-pressing technique. Phase composition was analyzed by XRD and morphology of fracture was observed by SEM. Physical performance such as density, resistivity, hardness and friction coefficient with different volume fraction of Cu/Ti₂AlC composites were studied. When the content of Ti₂AlC increased from 10% to 70%, the relative density reduced from 99.38% to 90.56% and the resistivity increased significantly. Hardness reached the maximum value when Ti₂AlC was at 60% and friction coefficient declined with the increasing of Ti₂AlC. Cu/Ti₂AlC composites, showing good conductivity properties and friction performance. Oxidation resistance enhanced obviously with the content of Ti₂AlC increasing. Cu-60%Ti₂AlC sample possessed optimum thermal shock resistance, and no cracking was found at 600 °C cycled for 10 times and 900 °C cycled for 1 time.     

Fabrication of in situ Ti2AlN/TiAl composites by reaction hot pressing and their properties

Ti2AIN/TiAI composites with different volume fractions of reinforcement were successfully fabricated by hot-pressing sintering method （reaction hot pressing） using Ti, Al and TiN powders as starting materials. The synthesis process includes four stages： first, the reactions between Al and Ti powers and between Al and TiN powders respectively occur and result in TiAl3 phase; secondly, AI powders in the sample are exhausted; the remaining Ti cores react with TiAl3 layer to form Ti-Al intermetallics; moreover, a few Ti2AlN particles precipitate from the TiAl3 phase; thirdly, Ti-Al intermetallics react with the remaining Ti cores to form Ti3Al and TiAl phases. TiAl phase and original TiN powers are in direct contact each other; finally, the residual TiN powers react with TiAl phase and result in a plenty of TizAIN phase. Compared with TiAl matrix, the hardness, elastic modulus and high-temperature compressive strength of Ti2AlN/TiAl composite are improved obviously and they are all enhanced with increasing the volume fraction of Ti2AlN phase.     

Gradient Structure of Ti-Al-C Ternary Carbide Prepared by Hot-pressing Sintering

X-ray diffraction ( XRD ) analysis on different polished surfaces normal to the hot pressing direction reveals that the phase compositions of the polished surfaces from the outside to the inside are pure TiC,Ti3 AlC2 TiC, pure Ti3 AlC2 and Ti2 AlC Ti3 AlC2 , no matter elemental powder or TiC is used as raw materials, It is found that ternary-la2ered carbide Ti2 AlC samples synthesized at 1500℃ by hot-pressing sintering are inhomogeneous and have a gradient structure. Electron probe X-ray micro-analysis ( EPMA ) indicates that the Al content along the hot pressing axis is parabolic, it is the highest in the center and the lowest at the both ends,while the Ti content is constant along the axis. The experimental result reveals that the evaporation of Al in samples in an open ,system during hot pressing sintering results in a gradient structure.     

Effect of tin on the reaction synthesis of ternary carbide Ti3AlC2

The effect of tin on synthesis of Ti₃AlC₂ by spark plasma sintering (SPS) from TiC/Ti/Al powders was investigated. X-ray diffraction (XRD) and scanning electron microscopy (SEM) were used for phase identification and microstructure evaluation. The experimental results show that addition of tin can considerably accelerate the synthesis reaction of Ti₃AlC₂ and fully dense, essentially single-phase polycrystalline Ti₃AlC₂ could be successfully obtained by sintering 2TiC/1Ti/1Al/0.2Sn powders at 1200–1250 °C under a pressure of 30 MPa. SEM images show that Ti₃AlC₂ samples in about 2–5 μm thick and 10–25 μm long platelets can be obtained. The fracture toughness and flexural strength of Ti₃AlC₂ were 6.5±0.2 MPa·m^1/2 and 560±10 MPa, respectively. Funded by the National Natural Science Foundation of China (No.20771088, No.50572080) and Doctoral Foundation of Wuhan University of Technology (No.471-38650142)     

机械诱发自蔓延反应合成Ti3AlC2的机理研究

以3Ti／Al／2C粉体为原料,采用机械合金化的方法以合成Ti3AlC2材料。研究结果表明,在机械合金化过程中诱发自蔓延反应,反应会产生大量坚硬的小块体颗粒,大小约为0．2-11mm。粉体的组成相为TiC、Ti3AlC2、Ti2AlC,而块体仅含有TiC和Ti3AlC2。获得的粉体和块体产物中Ti3AlC2含量分别约为63wt％和84．8wt％。提出了一个机械诱发自蔓延反应合成Ti3AlC2的反应机制,即Ti3AlC2是从固相TiC与Ti-Al液相中形核并长大。     

Effects of HIPing pressure on microstructures and properties of TiAl alloy

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Fabrication of Ti2AlC by Spark Plasma Sintcring from Elemental Powders and Thermodynamics Analysis of Ti-M-C System

A ternary-layered carbide Ti2AlC material could be synthesized by spark plasma sintering（SPS） technology using elemental powder mixture of Ti, Al and active carbon. By means of XRD and SEM, phases were identified and microscopically evaluated. The experimental results show that the main phase in the product was fully crystallized Ti2AlC with small particle size when sintered at 1200℃. The synthesis temperature of SPS was 200-400℃ lower than that of hot pressing （HP） or hot isostatic pressing （HIP）. Through thermodynamics calculations, the mechanism of Ti2AlC was studied by calculating changes of Gibbs free energy of reactions.     

TiC/Ti-Al基复合材料的燃烧合成

为了改善Ti-Al金属间化合物的脆性,利用SHS/PHIP工艺制备了TiC/Ti-Al基复合材料.理论分析表明,绝热温度随C质量分数的增加而呈升高趋势,当体系中碳的质量分数≥2%时,该体系能完成自蔓延过程.采用电子扫描显微镜,X射线衍射仪对合成产物进行了分析.结果表明,合成产物中除存在基体相Ti3Al和TiAl和增强相TiC外,还存在许多三元相Ti3AlC和Ti2AlC相;随着Al质量分数的增加,增强相的形貌由颗粒状逐渐变成棒状或片状;复合材料的硬度和压缩强度随C质量分数的增加逐渐增加,但密度及相对密度随C质量分数的增加呈先增加后降低的趋势.当C的质量分数达到4%时,其实际密度和相对密度均达到最大.     

Stability of titanium-aluminium nitride (Ti<Subscript>2</Subscript>AlN) at high pressure and high temperatures

The stability of Ti2AlN at high pressure of 5 GPa and different temperatures of 700-1 600 ℃ was investigated using X-ray diffraction (XRD),scanning electron microscopy (SEM) equipped with an energy dispersive spectrometer (EDS).Ti2AlN was found to be stable at temperatures as high as 1 400 ℃under 5 GPa for 20 min,and was proved that it held better structure stability than Ti2AlC under 5 GPa through comparative experiments of Ti2AlN and Ti2AlC (representative compounds of M2AX phases (211 phase)).The reaction process at high pressure had some difference from that at ambient pressure/vacuum,and Ti2AlN directly decomposed to TiN and TiAl at 5 GPa and 1 500 ℃ for 20 min.Moreover,the mechanism of phase segregation was discussed.In addition,the behavior of Ti2AlN contacting with Zr at high pressure and high temperature (HPHT) was also studied.     

Thermodynamic analysis of the formation of <Emphasis Type="Italic">In-situ</Emphasis> reinforced phases in cast Al-4.5Cu alloy

The thermodynamic analysis of the formation of in-situ reinforced phases in （TiB2＋Al3Ti）/Al-4.5Cu composites prepared by mixed salts reaction was conducted, and heat changes of mixed salts system were analyzed by differential thermal analysis（DTA）.The results show that although TiB2 possesses the strongest formation ability in Al-Ti-B ternary system, [Ti] is relatively excessive in the in-situ reaction and it combines with Al to form AlaTi phase. The reinforced phases are TiB2 and AlaTi in the produced composites due to the reaction taking place to form reinforced phase with the addition of mixed salts into Al-4.5Cu melt between 900 ℃ and 1 032 ℃.     

Friction and wear properties of TiAl and Ti2AlN/TiAl composites at high temperature

The high-temperature friction and wear properties of TiAl alloys and Ti₂AlN/TiAl composites (TTC) in contact with nickel-based superalloy were studied. The results showed that, at 800 and 1 000 °C, the coefficient of the friction (COF) decreased with the increase of sliding velocity and the wear loss of the TTC decreased with the increase of volume fraction of Ti₂AlN. The wear mechanisms of the pairs are adhesive wear and the wear debris mainly comes from the contacting nickel-based superalloy. The intergranular fracture and the cracking of the phase boundary in the lamellar structure are the wear mode of TiAl alloy. The wear mode of TTC is phase boundary fracture and adhesive spalling. The abrasive resistance of TTC is slightly higher than that of TiAl alloy.     

Eleetronie Structures and Bonding Properties of Ti2AlC and Ti3AlC2

The relation among electronic structure, chemical bond and property of Ti2AlC, Ti3AlC2 and doping Si into Ti2AlC was studied by density function and the discrete variation （DFT-DVM） method. After adding Si into Ti2AlC, the interaction between Si and Ti is weaker than that between Al and Ti, and the strengths of ionic and covalent bonds decrease both. The ionic and covalent bonds in Ti3AlC2, especially in Ti-Al, are stronger than those in Ti2AlC. Therefore, in synthesis of Ti2AlC, the addition of Si enhances the Ti3AlC2 content instead of Ti2AlC. The density of state （DOS） shows that there is mixed conductor characteristic in Ti2AlC and Ti3AlC2. The DOS of Ti3AlC2 is much like that of Ti2AlC. Ti2SiAl1-xC has more obvious tendency to form a semiconductor than Ti2AlC, which is seen from the obvious difference of partial DOS between Si and Al 3/7.     

Instability of TiC and TiAl3 compounds in Al-10Mg and Al-5Cu alloys by addition of Al-Ti-C master alloy

The performance of Al-Ti-C master alloy in refining Al-10Mg and Al-5Cu alloys was studied by using electron probe micro-analyzer （EPMA） and X-ray diffractometer （XRD） analysis. The results indicate that there are obvious fading phenomena in both Al-10Mg and Al-5Cu alloys with the addition of Al-5Ti-0.4C refiner which contains TiC and TiAl3 compounds. Mg element has no influence on the stability of TiC and TiAl3, while TiC particles in Al-10Mg alloy react with Al to form Al4C3 particles, resulting in the refinement fading. However, TiC particles are relatively stable in Al-5Cu alloy, while TiAl3 phase reacts with Al2Cu to produce a new phase Ti（Al, Cu）2, which is responsible for the refinement fading in Al-5Cu alloy. These indicate that the refinement fading will not occur only when both the TiC particles and TiAl3 compound of Al-Ti-C refiner are stable in Al alloys.     

THE PROCESS AND MECHANISM OF TiAl－BASED ALLOY SYNTHESIZED FROM Ti AND AlP OWDERS

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Synthesis and tribological behaviors of Ti3SiC2 material prepared by vacuum sintering technique

The bulk Ti₃SiC₂ specimens with less than 1 wt% TiC impurity were prepared by vacuum sintering technique, and the average grain size was about 5–6 μm in the elongated direction. When the sintering temperature, soaking time and heating rate were 1 400 °C, 1 h and 10 °C·min^?1, respectively, the highest relative density of Ti₃SiC₂ specimens could reach 97.8%. Meanwhile, the lowest coefficient of friction (COF) and wear rate (WR) of the Ti₃SiC₂ samples were 0.55 and 1.37×10^?3 mm³(Nm)^?1 at a sliding speed of 0.35 m/s, load pressure of 10 N and ambient condition, respectively. The COF of the Ti₃SiC₂ sample reduced with the increasing of the load pressure, while the WRs fluctuated little. The WR increased with the increasing of the sliding speed, and weakly influenced the COF. These changing behaviors could be attributed to the presence and coverage of the amorphous mixture oxide film of Ti, Si, Al, and Fe on the Ti₃SiC₂ friction surface. The self-antifriction mechanism led to reducing of the COF. The increasing of the WR was attributed to the wearing consumption.     

Microstructures and mechanical,electrical, high-temperature properties of Cu/Ti<Subscript>2</Subscript>AlC FGM fabricated by hot-pressing

The microstructure and the electrical, thermal, friction, and mechanical properties of Cu/Ti₂AlC fabricated by hot-pressing at 900 °C for 1 h were investigated in the present work. Microstructural observations have shown that the plate-like Ti₂AlC grains distribute irregularly in the network of Cu grains, and well-structured, crack-free bonds between the layers. With the increase in the content of Ti₂AlC from layer A to layer D, the electrical resistivity increases from 1.381×10^-7 Ω·m to 1.918 ×10^-7 Ω·m, the hardness increases from about 980.27 MPa to about 2196.01 MPa, and the friction coefficient from above 0.20 reduces to about 0.15. Oxidation rate increases with the increases of temperature. Exfoliation was obviously observed on the surface of oxidation layer A. The surface of layer D was still intact and the spalling and other defects were not found. The mass decreases in the acid solution, and increases in the alkaline solution. The largest corrosion rate is found in 6.5% HNO₃ or 4% NaOH solution.     

Ti-C-Al-Fe_2O_3反应体系的热力学及形成产物的分析

针对Ti-C-Al-Fe2O3体系进行了热力学计算,并结合DSC及XRD分析,为研究该体系反应合成TiC,Al2O3提供了理论依据.计算结果表明：该体系在发生SHS反应时,可以生成TiC,Al2O3,Fe2Ti,TiAl3,Fe3C和Al4C3等产物,但TiC,Al2O3的热力学稳定性要远远大于Fe2Ti,TiAl3,Fe3C和Al4C3等相,因此,在1600℃的钢液引燃的SHS反应过程中,只能生成TiC,Al2O3两种产物.通过XRD分析也证明了在反应产物中只有TiC,Al2O3两种物质形成.     

Study on the isothermal oxidation behavior in air of Ti_3AlC_2 sintered by hot pressing

The isothermal oxidation behavior at 900―1300℃ for 20 h in air of bulk Ti3AlC2 with 2.8 wt% TiC sintered by means of hot pressing was investigated in the work. The isothermal oxidation behavior generally followed a parabolic rate law. The parabolic rate constants increased from 1.39×10-10 kg2·m-4·s-1 at 900℃ to 5.56×10-9 kg2·m-4·s-1 at 1300℃. The calculated activation energy was 136.45 kJ/mol. It was demonstrated that Ti3AlC2 had excellent oxidation resistance due to the continuous, dense and adhesive protect scales consisted of a mass of α-Al2O3 and a little of TiO2 and/or Al2TiO5. In principle, the oxide scale was grown by the inward diffusion of O2- and the outward diffusion of Ti4 and Al3 . The rapid outward diffusion of cations usually resulted in the formation of cracks, gaps, and holes.     

Effect of Mg/Al ratios on hydration mechanism of tabular alumina carbon composites reinforced by Al<Subscript>4</Subscript>C<Subscript>3</Subscript> in situ reaction

Hydration mechanism of tabular alumina carbon composites reinforced by Al₄C₃ in situ reaction with Mg and Al was researched in water steam using super automatic thermostatic water bath from 25 °C to 85 °C. It is shown that hydration mechanism of the composites is chemical reaction control at 44.3 °C-84 °C in H₂O(g). The hydration was controlled by diffusion from 24.7 °C to 33 °C. The ratio of added Mg/Al influences the HMOR of the composites.The mechanism of HMOR of the composites with different ratios of Mg/Al can be discovered by means of SEM analysis. The active Mg/Al powder and flake graphite inside give the composites outstanding hot strength resulting from the interlocking structure of Al₄C₃ crystals at high temperature. Besides, the matrix changes into the Al₄C₃ with high refractoriness. The method of preventing the hydration of tabular alumina carbon composites reinforced by Al₄C₃ in situ reaction was immersed in the wax at suitable temperature or storing them below 33 °C in a dry place or storing them with paraffin-coating.