Effects of Al and Al4C3 contents on combustion synthesis of Cr2AlC from Cr2O3-Al-Al4C3 powder compacts

Preparation of the ternary carbide Cr₂AlC was conducted by combustion synthesis in the mode of self-propagating high-temperature synthesis (SHS) from the Cr₂O₃-Al-Al₄C₃ powder compact. Effects of the contents of Al and Al₄C₃ on the product composition and combustion behavior were studied by formulating the reactant mixture with a stoichiometric proportion of Cr₂O₃:Al:Al₄C₃ = 3:5x:y, where x and y varied from 1.0 to 1.5. When compared to those of the powder compact with Cr₂O₃:Al:Al₄C₃ = 3:5:1 (i.e., x = y = 1.0), the combustion temperature and reaction front velocity increased with content of Al, but decreased with that of Al₄C₃. Besides Cr₂AlC and Al₂O₃, the final products always contained a secondary phase Cr₇C₃ that was substantially reduced by adopting additional Al and Al₄C₃ in the reactant compacts. For the sample with Cr₂O₃:Al:Al₄C₃ = 3:7.5:1 (x = 1.5), solid state combustion reached a peak temperature of 1245 °C and yielded Cr₂AlC with a trivial amount of Cr₇C₃. Although Cr₇C₃ was lessened by introducing extra Al₄C₃, the increase of Al₄C₃ from y = 1.1 to 1.5 produced almost no further reduction of Cr₇C₃ in the final product. This is partly attributed to the low combustion temperature in the range of 1065-1095 °C for the samples with additional Al₄C₃, and in part, due to the role of Al₄C₃ which might react with Cr to form Cr₇C₃, Cr₂Al, and Cr₂AlC.     

Effects of Al content on formation of Ta2AlC by self-propagating high-temperature synthesis

Preparation of the ternary carbide Ta₂AlC was conducted by combustion synthesis in the mode of self-propagating high-temperature synthesis (SHS) from elemental powder compacts of different compositions. The synthesis reaction is characterized by a nearly planar combustion front traversing the entire sample in a self-sustaining manner. When compared with those of the reactant compact with stoichiometry of Ta:Al:C = 2:1:1, lower combustion front velocities and temperatures were observed for the samples containing more Al than the stoichiometric amount. The as-synthesized products are generally composed of Ta₂AlC as the dominant phase along with two minor carbides Ta₂C and Ta₄AlC₃, both of which can be reduced by increasing the amount of Al in the sample. On the other hand, an aluminide compound Ta₂Al was detected in the final product when the green compact contained carbon less than the stoichiometric quantity. Finally, an optimum composition arrived at Ta:Al:C = 2:1.6:1, with which the powder compact produced single-phase Ta₂AlC through SHS. The grains of Ta₂AlC are typically plate-like with a size of 5–10 μm and the layered structure consisting of closely packed Ta₂AlC is evident in the product obtained from the sample with sufficient Al. In addition, a set of possible reaction paths to produce Ta₂AlC was proposed, including the reactions of Ta₂C with Al and Ta₂Al with carbon, as well as the interaction between Ta₄AlC₃, Ta₂Al, and Al.     

Effects of TiC addition on formation of Ti3SiC2 by self-propagating high-temperature synthesis

Formation of Ti₃SiC₂ was conducted by self-propagating high-temperature synthesis (SHS) from both the elemental powder compacts of Ti:Si:C = 3:1:2 and the TiC-containing samples compressed from powder mixtures of Ti/Si/C/TiC with TiC content ranging from 4.3 to 33.3 mol%. The effect of TiC addition was studied on combustion characteristics and the degree of phase conversion. For the elemental powder compacts, with the progress of combustion wave the sample experiences substantial deformation, including axial elongation and radial contraction. The extent of sample deformation and flame-front propagation velocity were considerably reduced for the samples with TiC addition, because the dilution effect of TiC lowered the reaction temperature. Two reaction mechanisms were adopted to explain the formation of Ti₃SiC₂, one involving the reaction of a Ti–Si liquid phase with solid reactants for the elemental powder compact and the other dominated by the interaction of solid-phase species for the TiC-containing sample. For all products synthesized in this study, the XRD analysis identifies formation of Ti₃SiC₂ along with a major impurity TiC and a small amount of Ti₅Si₃. The resulting Ti₃SiC₂ is typically elongated grains. Based upon the XRD profile, the Ti₃SiC₂ content at a level of 71.5 vol.% was obtained in the product from the elemental powder compact. With the addition of TiC, an improvement in the yield of Ti₃SiC₂ was observed and an optimal conversion reaching 85 vol.% was achieved by the sample with 20 mol% of TiC. However, further increase of the TiC amount led to a decrease in the Ti₃SiC₂ content, because of the low reaction temperature around 1150 °C.     

Combustion synthesis of Ti3Si1−xAlxC2 solid solutions from TiC-, SiC-, and Al4C3-containing powder compacts

Preparation of the Ti₃Si_1−xAl_xC₂ solid solution with x = 0.2-0.8 was investigated by self-propagating high-temperature synthesis (SHS) using TiC-, SiC-, and Al₄C₃-containing powder compacts. Due to the variation of reaction exothermicity with sample stoichiometry, the combustion temperature and reaction front velocity decreased with increasing Al content of Ti₃Si_1−xAl_xC₂ for the TiC- and Al₄C₃-added samples, but increased for the samples with SiC. In contrast to the formation of Ti₃(Si,Al)C₂ as the dominant phase for the TiC- and SiC-added samples, TiC was identified as the major constituent in the final products of samples adopting Al₄C₃. In addition, the evolution of Ti₃(Si,Al)C₂ was improved by increasing the Al content of the TiC- and SiC-added powder compacts, but deteriorated considerably upon the increase of Al₄C₃ in the Al₄C₃-containing sample.     

Ti3AlC2掺杂SPS法制备Ti2AlC/TiAl复合材料的研究

通过2TiC-Ti-1.2Al体系的原位热压反应制备了Ti₃AlC₂陶瓷,然后以59.2Ti-30.8Al-10Ti₃AlC₂(wt%)为反应体系,采用放电等离子烧结技术制备出Ti₂AlC/TiAl基复合材料。借助XRD、SEM分析了产物的相组成和微观结构,并测量了其室温力学性能。结果表明：原位热压烧结产物由Ti₃AlC₂和TiC相组成,Ti₃AlC₂呈典型的层状结构,TiC颗粒分布在其间。SPS法制备的Ti₂AlC/TiAl基复合材料主要由TiAl、Ti₃Al和Ti₂AlC相组成,Ti₂AlC增强相主要分布于基体晶界处,表现为晶界/晶内强化作用。力学性能测试表明：Ti₂AlC/TiAl基复合材料的密度、维氏硬度、断裂韧性和抗弯强度分别为3.85 g/cm₃、5.37 GPa、7.17 MPa?m_1/2和494.85 MPa。     

Strengthening of Ti2AlC by substituting Ti with V

Ti₂AlC is strengthened by substituting Ti with V to form (Ti,V)₂AlC solid solutions. The Vickers hardness, flexural strength, shear strength and compressive strength are enhanced by 29%, 36% and 45% for (Ti_0.8,V_0.2)₂AlC solid solution, respectively. The strengthening mechanism is discussed.     

团聚粉末制备工艺对冷喷涂Ti2AlC沉积的影响

以热压烧结后球磨粉碎的Ti_2AlC亚微米粉末为原料,通过水热处理使其团聚成微米级粉末,并运用冷喷涂技术在Zr-4合金基体上沉积Ti_2AlC涂层。采用扫描电子显微镜、金相显微镜、XRD衍射仪、激光粒度分析仪等对Ti_2AlC颗粒和涂层微观结构进行表征;采用显微硬度仪和拉伸测试系统对Ti_2AlC涂层的基本力学性能进行测试;采用N2吸附法测涂层孔隙,采用电化学工作站测涂层的贯通孔隙。结果表明:对平均粒径0.3μm的Ti_2AlC粉末进行水热处理时,添加硫酸铵能够促进亚微米颗粒的团聚,团聚粉末的平均粒度可达到6μm。此粉末的冷喷涂特性最好,沉积的Ti_2AlC涂层厚度达到100μm,涂层中有微孔和介孔但没有贯通孔隙,涂层和基体结合强度达到了44MPa。     

Ti3AlC2材料的反应合成及其烧结行为

以Ti,Al和TiC为原材料,用无压煅烧合成法制备三元化合物Ti3AlC2。详细讨论了煅烧温度和铝含量对多晶Ti3AlC2纯度的影响。利用X射线衍射仪、场发射扫描电镜和场发射透射电镜研究了粉末材料的组织结构、晶粒大小、层板厚度和选区电子衍射花样。结果表明1300℃是合成Ti3AlC2粉末的最佳煅烧温度,1:1.2:2是Ti/Al/TiC原材料的最佳摩尔比。用热压法制备了不同烧结温度下的Ti3AlC2块体试样,在1300℃热压制备的Ti3AlC2块体的相对密度可达99.9%,其维氏硬度和三点抗弯强度分别为5.7 GPa和630 MPa。通过场发射扫面电镜观察材料的断口形貌,进一步分析了Ti3AlC2块体材料的强化机理。     

Effect of Cr7C3 on the mechanical, thermal, and electrical properties of Cr2AlC

In this work, phase pure Cr₂AlC and impure Cr₂AlC with Cr₇C₃ have been fabricated to investigate the mechanical, thermal, and electrical properties. The thermal expansion coefficient is determined as 1.25 × 10⁻⁵ K⁻¹ in the temperature range of 25-1200 °C. The thermal conductivity of the Cr₂AlC is 15.73 W/m K when it is measured at 200 °C. With increasing temperature from 25 °C to 900 °C, the electrical conductivity of Cr₂AlC decreases from 1.8 × 10⁶ Ω⁻¹ m⁻¹ to 5.6 × 10⁵ Ω⁻¹ m⁻¹. For the impure phase of Cr₇C₃, it has a strengthening and embrittlement effect on the bulk Cr₂AlC. And the Cr₂AlC with Cr₇C₃ would result in a lower high-temperature thermal expansion coefficient, thermal conductivity, specific heat capacity and electrical conductivity.     

Factors controlling pure-phase magnetic BiFeO3 powders synthesized by solution combustion synthesis

Bismuth ferric oxide nanopowders were prepared through combustion method. Pure phase and well-crystallized BiFeO₃ can be obtained by controlling the combustion process, fuel type and fuel-to-oxidant ratio. The evolutions of phase constitution and structural characteristics of the as-resulted nanopowders were investigated by X-ray diffraction, scanning electron microscope, and simultaneous thermogravimetric analysis. The results revealed that both the type and amount of fuel have to be carefully considered because they play an important role in total reaction characteristics. Among all tested fuels, l-α-alanine and glycine are the suitable fuels for BiFeO₃ synthesis. For α-alanine, the optimal fuel-to-oxidant ratio is 0.22, which results in a suitable flame temperature for BiFeO₃ formation. Still, too little fuel would result in only amorphous phase powders due to the low flame temperature and too much fuel would lead to transformation of the BiFeO₃ phase to impurities because of the high flame temperature involved. The resulting BiFeO₃ nanopowders exhibited strong H₂O₂-activiting ability and weak magnetism. When BiFeO₃ nanopowders were used as a heterogeneous Fenton-like catalyst to degrade rhodamine B (RhB), the apparent rate constant for RhB degradation in the presence of H₂O₂ at pH 5.0 was evaluated to be 0.048 min⁻¹.     

Effects of pelletization of reactants and diluents on the combustion synthesis of Si3N4 powder

Reactants were pelletized, and then combustion synthesis of Si₃N₄ powder was achieved under the N₂ pressure of 3.0 MPa. Effects of the pelletization of reactants and Si₃N₄ diluents on the combustion process parameters and the characteristics of products were studied. The combustion mode of single reactant pellet was preliminarily discussed. The results indicated that the combustion reaction of single pellet was layer-by-layer from the surface to the core, which led to two peaks on the combustion temperature variation waves. With increasing the diluents content, the morphologies of Si₃N₄ particles changed from short rods into equiaxed grains, and residual Si in the final products obviously decreased. Single phase β-Si₃N₄ powder mainly contained equiaxed grains was prepared when 58 wt.% diluents was added.     

Synthesis and crystal structure of Ba3Si4C2

SiC powder prepared by the Na flux method at 1023 K for 24 h and Ba were used as starting materials for synthesis of tribarium tetrasilicide acetylenide, Ba₃Si₄C₂. Single crystals of the compound were obtained by heating the starting materials with Na at 1123 K for 1 h and by cooling to 573 K at a cooling rate of −5.5 K/h. The single crystal X-ray diffraction peaks were indexed with tetragonal cell dimensions of a = 8.7693(4) and c = 12.3885(6) Å, space group I4/mcm (No.140). Ba₃Si₄C₂ has the Ba₃Ge₄C₂ type structure which can be described as a cluster-replacement derivative of perovskite (CaTiO₃), and contains isolated anion groups of slightly compressed [Si₄]⁴⁻ tetrahedra and [C₂]²⁻ dumbbells. The electrical conductivity measured for a not well-sintered polycrystalline sample was 2.6 × 10⁻²–7 × 10⁻³ S cm⁻¹ in the temperature range of 370–600 K and slightly increased with increasing temperature. The Seebeck coefficient showed negative values of around −200 to −300 μV K⁻¹.     

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.     

Synthesis of Ti3SiC2 bulks by infiltration method

T₃SiC₂ bulks have been synthesized by infiltrating Si liquid into porous precursor pellets composed of solid TiC and Ti powders. Silicon pellets were placed at the bottom of the precursor pellets as the liquid source. The starting compositions can be represented by the formula 2TiC + Ti + xSi, where x = 1.0, 1.2, 1.5 and 1.8, respectively. The phase formation and microstructure of the bulks were investigated by X-ray diffraction (XRD) and scanning electron microscopy (SEM) equipped with energy-dispersive spectroscopy (EDS) system. The results demonstrated that the TiC/Ti precursor pellet could only react with Si completely when the x value is 1.8. Impurities SiC, Ti-Si binary compounds and Ti₈C₅ appeared along the silicon diffusion direction. It is found that the compositions of impurities strongly depended on the Si-concentration. Reaction mechanism of this Ti₃SiC₂ infiltration synthesis has also been discussed based on the Si-concentration changes on the diffusion path.     

Low-temperature fabrication of high purity Ti3SiC2

In this study, we fabricated high purity Ti₃SiC₂ ceramic by mechanical alloying (MA) and spark plasma sintering (SPS), and investigated the effect of trace amount of Al on these processes. Our results show that addition of proper amount of Al significantly increases the purity of Ti₃SiC₂ in the MA and subsequent SPS products, and remarkably reduces the sintering temperature for Ti₃SiC₂. Ti₃SiC₂ sintered compact with a purity of 96.5 wt% was obtained by 10 h of MA and subsequent SPS from a starting mixture composed of n(Ti):n(Si):n(Al):n(c) = 3:1:0.2:2 at 850 °C. At 1100 °C, Ti₃SiC₂ with a purity of 99.3 wt% and a relative density of 98.9% was obtained.     

Preparation of Ti3AlC2 by mechanically activated sintering with Sn aids

The mechanically activated sintering process was adapted to synthesize Ti₃AlC₂ using 3Ti/Al/2C/0.05Sn powder mixtures. The result showed that the powders containing TiC, Ti₃AlC₂ and Ti₂AlC were obtained by mechanical alloying (MA) 3Ti/Al/2C powders. Addition of appropriate Sn reduced the content of Ti₂AlC and enhanced the synthesis of Ti₃AlC₂ significantly. The powders with highest content of Ti₃AlC₂ were obtained by MA 3Ti/Al/2C/0.05Sn powders. Through pressureless sintering the mechanical alloyed powders at 900–1100 °C for 2 h, the high purity Ti₃AlC₂ material with fine organization was produced.     

Corrosion behavior of select MAX phases in NaOH, HCl and H2SO4

In this paper we report on the electrochemical corrosion of select MAX phases, namely Ti₂AlC, (Ti,Nb)₂AlC, V₂AlC, V₂GeC, Cr₂AlC, Ti₂AlN, Ti₄AlN₃, Ti₃SiC₂ and Ti₃GeC₂ in 1 M NaOH, 1 M HCl and 1 M H₂SO₄ solutions. Polarization characteristics recorded in 1 M NaOH show that V₂AlC, V₂GeC and Cr₂AlC undergo active dissolution at potentials more positive than the corrosion potential, while Ti₂AlC, (Ti,Nb)₂AlC, Ti₃SiC₂ and Ti₃GeC₂ passivate. In the 1 M HCl solutions, Ti₂AlC, V₂AlC and V₂GeC actively dissolve; Ti₃SiC₂ and Ti₃GeC₂ passivate. Depending on potential, (Ti,Nb)₂AlC and Cr₂AlC showed trans-passive behavior. In 1 M H₂SO₄ solutions, Ti₂AlC, (Ti,Nb)₂AlC, Ti₃SiC₂ and Ti₃GeC₂ passivate, V₂AlC and V₂GeC show active dissolution, while Cr₂AlC exhibits trans-passive behavior. Ti₂AlN and Ti₄AlN₃ were passive in all solutions except in 1 M HCl, where Ti₂AlN showed trans-passive behavior. Given that the corrosion behavior of (Ti,Nb)₂AlC is unlike either Ti or Nb, the behavior of the former cannot be predicted from that of the latter.     

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.     

国外多孔基体氧化铝/氧化铝复合材料工程应用进展

氧化铝/氧化铝复合材料(Al2O3/Al2O3)是20世纪90年代兴起的一类连续陶瓷纤维增强陶瓷基复合材料,已经发展为与SiC/SiC、C/SiC等非氧化物陶瓷基复合材料并列的一类陶瓷基复合材料。与非氧化物陶瓷基复合材料相比,Al2O3/Al2O3具有长时抗氧化、高温耐腐蚀、低成本等独特优势,已经在航空发动机、地面燃气轮机等军民两用热结构材料领域展现出广阔的应用前景。本文从材料应用的角度出发,系统分析阐述了目前在Al2O3/Al2O3占主导地位的多孔基体Al2O3/Al2O3(P-Al2O3/Al2O3)的增韧机制、成型工艺和性能特点,重点归纳了国外近年来P-Al2O3/Al2O3的工程化应用进展及前景,最后指出了P-Al2O3/Al2O3存在的局限性并展望了未来发展方向,旨在为国内Al2O3/Al2O3体系发展提供借鉴和参考。     

Synthesis of MoSi2/WSi2 nanocrystalline powder by mechanical-assistant combustion synthesis method

MoSi₂/WSi₂ nanocrystalline powder has been successfully synthesized by the mechanical-assistant combustion synthesis method. This method includes a ball-milling process followed by combustion synthesis. The composition and microstructure of the as-milled powder mixture were detected by X-ray diffraction and scanning electron microscopy analyses. Their results show that the Mo(W) solid solution and Si nanocrystals could be obtained during the ball-milling process. Compared with normal powder mixture (Mo + Si + W), it could be easily ignited and high maximum combustion temperature was achieved. It was also confirmed that MoSi₂/WSi₂ solid solution powder with nanometric structure could be prepared through combustion synthesis method from the mechanical activated powder mixture.