原位热压TiC/Ti/Al合成Ti2AlC的研究

本以TiC／Ti／Al为原料，采用热压T艺在1400℃原位合成和烧结含少量第二相Ti3AlC2的Ti2AlC材料。通过不同温度和不同热压时间下合成试样的XRD分析探讨了Ti2AlC的合成过程。结果表明，高温下Ti与Al反应生成中间相TiAl金属间化合物，然后TiC与TiAl金属间化合物反应生成Ti2AlC。不同温度下合成的Ti2AlC颗粒具有不同的形貌特征。     

原位热压TiC/Ti/Al合成Ti2AlC的研究

以TiC／Ti／Al为原料，采用热压工艺在1400℃原位合成和烧结了含少量第二相Ti3AlC2的Ti2AlC材料。通过不同温度和不同热压时间下合成试样的：XRD分析探讨了Ti2AlC的合成过程。结果表明，高温下Ti与Al反应生成中间相TiAl金属间化合物，然后TiC与TiAl金属间化合物反应生成Ti2AlC。初期反应非常迅速，大部分Ti2AlC在此阶段生成。反应后期反应物减少，速度变慢，同时生成少量第二相Ti3AlC2。不同温度下合成的Ti2AlC颗粒具有不同的形貌特征。     

工艺调控对原位合成Ti3AlC2陶瓷的影响

以TiC、Ti和Al粉为原材料,采用冷压预成型-热压辅助工艺原位制备Ti3 AlC2陶瓷.借助反应吉布斯自由能分析TiC-Ti-Al体系的合成机制,采用XRD和SEM分析工艺因素如升温速率、Al含量、烧结温度和压坯尺寸对原位合成Ti3 AlC2陶瓷的影响.结果表明,通过调控工艺,成功合成了高纯度Ti3 AlC2陶瓷,Ti3 AlC2具有典型的层状结构.该反应体系的最佳升温速率为:1000℃之前,20℃/min; 1000℃之后,10℃/min.用纳米TiC粉替代微米TiC粉,烧结温度由1450℃降至1350℃,且Ti3 AlC2的合成纯度更高.当采用大尺寸压坯时,发生了“热爆”现象,非平衡相较多,Ti3 AlC2的生成含量较低,且样品开裂严重.Ti3 AlC2的合成过程为:Ti与Al反应生成TiAl金属间化合物,接着TiAl与TiC反应生成Ti3AlC2.     

放电等离子烧结致密单相钛三铝碳二的反应机理

以3Ti/1.1Al/1.9C混合粉末为原料,采用放电等离子烧结(SPS)技术,利用X射线衍射仪、扫描电子显微镜和透射电子显微镜等分析方法,研究了致密单相Ti3AlC2三元层状化合物的合成机理,详细探讨了烧结温度对产物合成的影响,提出了一种SPS制备致密单相Ti3AlC2的反应机理。结果表明:利用SPS技术,在1 350℃保温10min的条件下,可以获得致密度大于99%的层状致密单相Ti3AlC2材料。最终产物中TiC的残留与原料中C含量有密切关系,适当降低原料中C含量有利于最终产物中TiC的消除。致密单相三元层状化合物Ti3AlC2的合成过程中,AlTi3和TiAl是形成TiC和Ti2AlC的主要中间相,而Ti3AlC2是由TiC与Ti2AlC反应生成的。     

Ti_2AlC/TiAl_3复合材料的制备及其性能研究

利用Ti-Al-TiC-CNTs体系的原位反应结合热压技术制备Ti2AlC/TiAl3复合材料。研究产物的相组成、结构和力学性能。结果表明:产物主要由TiAl3和Ti2AlC相组成,增强相Ti2AlC主要分布在基体晶界处,并形成了明显的搭接层状结构。产物的弯曲强度和断裂韧性分别为343.21 MPa和6.5 MPa·m1/2,远高于TiAl3合金的弯曲强度(162 MPa)和断裂韧性(2 MPa·m1/2),较TiAl3合金分别提高了111.86%和225%。     

Ti-Al-C三元系统中Ti3AlC2,Ti2AlC和TiC物相含量的测定

研究了Ti-Al-C三元体系中X射线衍射定量相分析方法,提出了Ti3AlC2,Ti2AlC和TiC这3种物相的特征衍射峰Ti3AlC2的(002)衍射峰,2θ=9.5°;Ti2AlC的(002)衍射峰,2θ=13.0°;TiC的(111)衍射峰,2θ=35.9°.采用混样无标样法推导了一套Ti3AlC2,Ti2AlC和TiC的定量计算公式,根据其特征衍射峰的强度就可计算这3个物相的相对含量.因为该公式推导过程本身就验证了其正确性(即自验证性),所以这个公式可以广泛用于Ti-Al-C三元体系中Ti3AlC2,Ti2AlC和TiC物相的定量测定.因此,这种方法非常简便、易行.     

球磨时间对Ti-Al-C系机械合金化粉体相组成和形貌的影响

采用Ti,Al和C元素粉体为反应原料,通过机械合金化方法制备出高纯度Ti3AlC2陶瓷粉体.研究球磨时间对Ti-Al-C系混合粉体相组成和形貌的影响,探讨合成Ti3AlC2的反应机理.研究表明:当机械合金化的其它参数不变,球磨时间4h时,原料粉体仍以单质形式存在;将球磨时间延长至4.5h时,此时混合粉体中Ti3AlC2含量提升到86wt％(质量分数,下同);4.5 h后,混合粉体中Ti3AlC2含量开始下降;通过对实验机理进行分析,单质粉体发生机械诱发自蔓延反应合成Ti3AlC2.     

TiH2做Ti源合成Ti2AlC/Ti3AlC2及热分析

廉价TiH2是制造钛粉的中间产物。本文用TiH2取代钛粉在常压下高温合成一种先进陶瓷材料-钛铝碳(Ti2AlC和Ti3AlC2)。以配料3TiH2/1.5Al/C或2TiH2/1.5Al/TiC为原料,在1400℃保温120 min可合成高纯Ti2AlC。原料3TiH2/1.2Al/2C在1400℃保温120 min和TiH2/1.2Al/2TiC在1350℃保温120 min均可制备高纯的Ti3AlC2。差示扫描量热法(Differential Scanning Calorimetry)被用来分析Ti-Al-C反应体系热量变化。在配料3TiH2/1.5Al/C反应过程中,Ti2AlC合成反应的放热峰消失;表明TiH2脱氢反应所吸收的热量与TiC或Ti2AlC的合成反应所释放的热量相互弥补。以TiH2为Ti源在一定程度上不仅可以降低原料成本,还可以减少或避免大批量生产钛铝碳过程中的热爆现象。     

自蔓延高温合成NiAl基金刚石工具材料的热力学研究

计算了Ni-Al体系及Ni-Al-金刚石体系自蔓延高温合成NiAl金属间化合物的绝热温度,运用物质自由能函数理论,对主要反应进行了热力学计算,结合相图预测了自蔓延高温合成产物,并用自蔓延高温合成实验结果与预测结果进行对比,分析了自蔓延高温合成NiAl金属间化合物的物相生成过程。结果表明:4Ni-2Al反应的驱动力比Ni-Al体系的大,4Ni-2Al体系绝热温度为1816 K,可实现燃烧波自维持,根据相图预测产物是NiAl和Ni_(3)Al,确定最佳的Ni-Al体系配比为4Ni-2Al。4Ni-2Ali-10%(质量分数)金刚石体系与4Ni-2Al-15%(质量分数)金刚石体系的绝热温度分别为1709 K和1655 K,均可实现燃烧波自维持,自蔓延高温合成产物均为NiAl、Ni_(3)Al及部分Ni。热力学分析结果与XRD、FESEM及EDS能谱分析结果是吻合的。     

原位热压2TiC/Ti/Al合成Ti3AlC2陶瓷

以2TiC/Ti/Al为组分采用原位热压技术制备Ti3AlC2陶瓷。采用XRD和SEM分析不同工艺时合成产物的物相组成和显微结构。结果表明：恰当的加压工艺和升温速率控制,能够合成高纯Ti3AlC2陶瓷。用TiC粉替代C和部分Ti粉有利于Ti3AlC2的原位合成。     

Synthesis and reaction path of Ti-Al-C MAX phases by reaction with Ti-Al intermetallic compounds and TiC

In this study, it was verified that the synthesis of Ti-Al-C MAX phases has advantages when using intermetallic compounds rather than using only elemental powders. The formation behavior of the MAX phases was presented through diffusion experiments. In the case of using elemental powder, Ti₂AlC is produced at 1300°C, and Ti₃AlC₂ is produced at 1400°C. When intermetallic compounds are used, Ti₂AlC is produced at 1000°C, and Ti₃AlC₂ is produced at 1300°C. In the case of the elemental powder, it is verified that Ti₃AlC₂ content is decreased and Ti₂AlC is increased when heat treatment is performed at 1400°C for 3 h. Rather Ti₃AlC₂ content is increased when intermetallic compounds are used. When an intermetallic compound is used, synthesis occurs more actively at high temperatures, and the tendency to be thermally decomposed can be prevented. When TiAl and TiC are heat treated, Al of the intermetallic compound is diffused into TiC, and C of TiC is diffused into the intermetallic compound. Furthermore, there are many two-dimensional defects in TiAl, which act as a C diffusion channel. C diffuses into TiAl to produce TiC_X, and the MAX phases is generated by the short-range diffusion of Al. At the region of TiC, TiC transforms into TiC_X after C diffuses into TiAl, which consequently structure of TiC changes from cubic to hexagonal. This is the same crystal structure as the MAX phases, and it is confirmed that the (110) surface is maintained. A Ti-C layer structure of the (110) surface is maintained, and it was determined that Al is diffused during this time to generate the MAX phases.     

An experimental approach to delineate the reaction mechanism of Ti3AlC2 MAX-Phase formation

A comprehensive reaction mechanism of Ti₃AlC₂ MAX-phase formation from its elemental powders while spark plasma sintering has been proposed. Microstructural evaluation revealed that Al-rich TiAl₃ intermetallic forms at around 660 °C once Al melts. Gradual transition from TiAl₃ to Ti-rich TiAl and Ti₃Al intermetallic phases occurs between 700 °C and 1200 °C through formation of layered structure due to diffusion of Al from periphery toward the centre of Ti particles. Formation of TiC and Ti₃AlC transient carbide phases were observed to occur through two different reactions beyond 1000 °C. Initially, TiC forms due to interaction of Ti and C, which further reacts with TiAl and Ti and gives rise to Ti₃AlC. Later, Ti₃AlC also forms due to diffusion of C into Ti₃Al above 1200 °C. Above 1300 °C, Ti₃AlC phase decomposes into Ti₂AlC MAX-phase and TiC in presence of unreacted C. Finally, Ti₂AlC and TiC reacts together to from Ti₃AlC₂ MAX-phase above 1350 °C and completes at 1500 °C.     

Ti_3AlC_2陶瓷的热压合成

以TiC-Ti-Al为反应体系,采用原位热压技术制备Ti3AlC2陶瓷。借助XRD分析相组成,并对实验现象进行分析。结果表明,TiC的加入,避免了Ti和C粉之间强烈的放热反应。通过降低初始压坯尺寸抑制了"热爆行为",有利于合成高纯Ti3AlC2。用大压坯时,"热爆行为"明显,产物由Ti3AlC2、TiC和Ti3Al相组成,Ti3AlC2含量少;用小压坯时,未发生"热爆行为",产物由Ti3AlC2和TiC相组成,Ti3AlC2相含量较高。     

Lamellar structure and effect of Ti2AlC on properties of prepared in-situ TiAl matrix composites

TiAl matrix composites, reinforced with varying Ti₂AlC content levels, were synthesized by vacuum arc melting by use of Ti, Al and graphite powders as raw materials. The effects of varied Ti₂AlC content from 0 to 100 mol% on the phases, microstructures, fracture behaviors and mechanical properties of resulting products were analyzed. Phase transformation was characterized by X-ray diffraction (XRD) and microstructures were measured by scanning electron microscopy (SEM), equipped with energy-dispersive spectroscopy (EDS). Results show that the products are composed primarily of TiAl, Ti₃Al, Ti₂AlC and small amounts of TiC. The unreacted TiC phase is due mainly to evaporation of Al. The Vickers hardness value of TiAl matrix composite was increased by adding Ti₂AlC, while the TiAl/Ti₂AlC composite fracture behaviors were improved in terms of crack deflection, trans-lamellar cracking and extraction of carbide reinforcements.     

Molten salt shielded synthesis and formation mechanism of Ti2AlC in NaCl–KCl medium

Herein, a highly crystalline Ti₂AlC was synthesized via the improved molten salt synthesis method called molten salt shielded synthesis. To achieve this goal, the mixture of Ti, Al, and graphite and KCl–NaCl eutectic composition salt was heated at 1000, 1050, and 1100 °C for 0.5, 1, and 1.5 h. The X-ray diffraction (XRD) patterns showed that the optimum condition for obtaining the more crystalline Ti₂AlC was achieved at 1100 °C for 1.5 h. Such phase identification, and transmission electron microscopy (TEM) images, proved that applying a protective carbon layer on the surface of salt led to inhibiting the diffusion of oxygen into the surface of the green pellet. As a result, the crystallinity of Ti₂AlC improved, while the content of undesirable compounds such as Al₂O₃ and Ti_xO_y decreased drastically. In order to shed light on the Ti₂AlC synthesis mechanism, differential thermal analysis (DTA) was employed. The DTA curve revealed that the Ti₂AlC formation completed in three levels. First, the partial dissolution of Ti in KCl–NaCl salt followed by a reaction with liquid Al resulted in the TiAl formation. Next, Ti(II) reacted in-situ on the surface of graphite that resulted in the non-stoichiometric TiC (TiC_1-x) formation, and, at last in a reaction between TiAl and TiC_1-x, Ti₂AlC phase formation took place at 940 °C.     

The phase transformation and microstructure of TiAl/Ti2AlC composites caused by hot pressing

Two series of raw materials were adopted to form TiAl/Ti₂AlC composites: Ti/Al/TiC and Ti/Al/C. Differential thermal analysis (DTA) of starting powers and X-ray diffraction (XRD) of samples sintered at different temperatures from 600 °C to 1300 °C by hot pressing were utilized to analyze the phase transformation and the mechanism of synthesis. Scanning electron microscopy (SEM) coupled with energy-dispersive spectroscopy (EDS) was utilized to investigate the morphology characteristics of the products. The experimental results showed that Ti reacted with Al to form TiAl intermetallics below 900 °C; and above 900 °C, TiAl reacted with TiC to produce dense TiAl/Ti₂AlC composites. The products sintered at 1200 °C had fine crystals and dense fibres, and the distribution of Ti₂AlC particles in TiAl matrix was homogeneous.     

Ti_2AlC陶瓷增强TiAl基材料的研究

国内外很多学者用自蔓延高温合成法、自蔓延高温合成同电弧熔炼铸造技术相结合法、放电等离子烧结等方法合成了TiAl/Ti2AlC复合材料。最近,作者以Ti、Al、TiC粉为原料,用原位热压的方法合成了该复合材料。本文综述了TiAl/Ti2AlC复合材料的几种制备方法、力学及抗氧化性能的研究情况。     

Structure and properties of a composite material obtained by thermal explosion in a mixture of Ni + Al + Cr<Subscript>2</Subscript>O<Subscript>3</Subscript>

The synthesis of a composite material by thermal explosion in a reaction mixture of Ni + Al + Cr₂O₃ was studied. The thermodynamic parameters of combustion of the systems studied were estimated to predict the composition of the inorganic products (condensed or gaseous) of self-propagating high-temperature synthesis and calculate the adiabatic combustion temperature. It is shown that the synthesis process involves competing reactions in the sample volume which are responsible for the formation of a multiphase product. The influence of the content of Cr₂O₃ in the reaction system on the strength characteristics of the product synthesis was studied. The microstructure of the synthesized samples was examined, and their micro-hardness, toughness and residual porosity were determined. The possibility of obtaining a homogeneous material based on NiAl intermetallic compound containing dissolved chromium and chromium oxide nanoparticles is shown.     

添加铝对机械活化辅助合成Ti_3SiC_2粉末的影响(英文)

以Ti,Si,TiC并添加Al的混合粉末为原料,采用机械活化辅助自蔓延合成法制备了Ti3SiC2粉末。研究表明,机械活化过程可将原料的粒度尺寸细化至10μm以下,反应物活性提高,并能激发自蔓延合成反应生成Ti-Si,SiC,TiCx等中间相。在上述条件下,合成单相Ti3SiC2粉末的温度可降至1350℃。反应机理为:Al作为脱氧剂通过抑制其它元素的氧化来促进主相的生成,且在反应物中优先熔化形成局部微小熔池,加速了反应物的扩散并生成TiCx和Ti5Si3中间相,从而促进Ti3SiC2粉末的生成。     

Core-shell ZrC/Ti2AlC reinforced composite coatings prepared by laser cladding on Zr-alloy substrates

Core-shell ZrC/Ti₂AlC reinforced intermetallic composite coatings were successfully prepared by laser cladding in-situ reaction using TiAl–TiC–Al powder preset on R60702 zirconium alloy surface. As-obtained coatings showed good metallurgical bonding with substrates. Composite coatings mainly contained dendritic ZrC/Ti₂AlC reinforced phase with core-shell structure and intermetallic matrix of Ti_xAl_y and Zr_xAl_y, with small amounts of Ti₃AlC. During laser pool solidification, TiC nucleated at boundary of primary precipitated ZrC dendrite. Al atoms then diffused into TiC outer layer during subsequent solidification process to finally form core-shell structure with ZrC as core and Ti₂AlC as outer layer. Ti₂AlC phase of shell structure improved physical performance between hard ZrC particles and matrix in terms of hardness and thermal expansion coefficient. The maximum hardness of cladding layer (848.8 HV) was 5-fold higher than that of zirconium alloy substrate. Also, no cracking was found inside the coatings or at the junction with substrates. In sum, these findings look promising for future applications of MAX phase composite coatings in nuclear power equipment.