原位自生Ti_2AlN/TiAl复合材料制备与高温性能研究
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摘要
本文设计并制备了原位自生Ti_2AlN/TiAl复合材料。利用扫描电镜(SEM)、透射电镜(TEM)、X射线衍射(XRD)、差热分析(DSC)等多种手段对材料微观组织及合成机理进行了系统研究；采用三点弯曲、氧化、热压缩和摩擦磨损等实验等手段测试了材料的综合性能，并分析了相关的影响因素。
原材料Ti、Al和TiN颗粒，采用热压烧结工艺，合成制备出增强相体积分数为20%和50%的Ti_2AlN/TiAl复合材料。该复合材料合成过程分为四个阶段：第一阶段Al粉完全熔化(>665℃)，此时在Ti颗粒表面形成TiAl3相；第二阶段Al粉参与合成反应而耗尽，Ti颗粒周围形成多层Ti-Al系化合物包围的层状结构，在TiAl3层边缘位置通过熔析反应形成了少量细小的Ti_2AlN颗粒；第三阶段(1100~1300℃期间)，高温下基体材料转变为TiAl(芯部为Ti3Al)，此时的TiN颗粒与TiAl紧密接触；第四阶段(1300℃保温、保压1小时处理)，TiN颗粒与TiAl完全反应得到大量Ti_2AlN颗粒，基体均匀化转变成TiAl相，最终得到Ti_2AlN/TiAl复合材料。
Ti_2AlN/TiAl复合材料的基体合金可通过热处理转变成全片层、双态和近γ相组织。其中，全片层TiAl基体组织的Ti_2AlN/TiAl复合材料硬度和弹性模量随Ti_2AlN颗粒体积分数增加而升高；高温(800℃)下，弯曲强度随Ti_2AlN颗粒体积分数增加而先升高后降低， Ti_2AlN颗粒体积分数占20%的复合材料弯曲强度最高，Ti_2AlN颗粒体积分数过高对强度不利。
氧化试验在800~900℃空气条件下进行。900℃下，Ti_2AlN/TiAl复合材料的典型氧化过程分为2个阶段：初期为相（晶）界和表面层快速氧化阶段，随后进入氧化层不断增厚的受扩散控制氧化阶段，随着氧化层厚度的增加氧化速率逐渐减缓。900℃空气条件下，氧化层自外向内分为两层，分别为TiO2层和(Al2O3+TiO2+Ti5Al3O2)混合层。
热压缩试验结果表明：随温度升高，TiAl合金和Ti_2AlN/TiAl复合材料的压缩强度均降低，而随着应变速率增加压缩强度升高；在高温高应变速率和低温低应变速率条件下，Ti_2AlN/TiAl复合材料的强度比基体TiAl合金提高40~50%。Ti_2AlN/TiAl复合材料热压缩变形方式除滑移外，还有TiAl片层组织晶界滑动、片层弯曲、片层间滑动、孪晶、再结晶等。低体积分数Ti_2AlN/TiAl复合材料中，位于晶界处的Ti_2AlN颗粒能够阻碍TiAl晶界滑动，有利于提高材料强度；高体积分数的Ti_2AlN/TiAl复合材料中，联接成三维网络结构的Ti_2AlN增强体能够有效承载，明显提高了复合材料压缩强度。
摩擦磨损试验结果表明：Ti_2AlN/TiAl复合材料与镍基合金组成的摩擦副，室温摩擦过程主要分为两个阶段：Ⅰ阶段为非稳态摩擦阶段，镍基合金是主要磨损方，磨损类型是镍基合金附着在复合材料磨面上的粘着磨损；Ⅱ阶段为稳态摩擦阶段，镍基合金仍然是主要磨损方，磨损方式是Ti_2AlN/TiAl复合材料对其产生的磨粒磨损，同时Ti_2AlN/TiAl复合材料发生粘着磨损。室温下，载荷增加，摩擦系数和磨损量均升高；滑动速度加快，Ti_2AlN/TiAl复合材料总磨损量增加，摩擦系数和复合材料的磨损率降低。
高温下摩擦副发生氧化，镍基合金氧化产物为NiO，Ti_2AlN/TiAl复合材料的氧化产物为Al_2O_3和TiO_2。Ti_2AlN/TiAl复合材料-镍基合金高温摩擦过程主要分为三个阶段：Ⅰ阶段为非稳态-摩擦系数上升阶段，镍基合金发生粘着磨损；Ⅱ阶段为非稳态-摩擦系数下降阶段，镍基合金的磨损方式从粘着磨损向磨粒磨损转变，复合材料磨损方式主要是粘着磨损；Ⅲ阶段为稳态-摩擦系数平稳阶段，镍基合金是主要磨损方，磨损类型为磨粒磨损。高温下，随着滑动速度增加，摩擦系数和复合材料磨损率均降低，复合材料的总磨损量上升；温度升高，摩擦系数和复合材料磨损量均下降。不论在室温还是高温摩擦试验中，复合材料磨损量均低于TiAl基体合金，Ti_2AlN体积分数增加，复合材料的磨损量随之降低。
In this paper, in situ Ti_2AlN/TiAl composites were designed and fabricated.Microstructure and synthesis mechanism of Ti_2AlN/TiAl composites weresystematically investigated by scanning electron microscope(SEM), transmissionelectron microscope(TEM), X ray diffraction(XRD), differential scanningcalorimetry(DSC) and so on. Properties of Ti_2AlN/TiAl composites were tested bythree-point bending, oxidation, hot compression and friction and wear, relatedfactors were also analyzed.
Ti, Al and TiN particles were raw materials, used hot-pressing technique tofabricated Ti_2AlN/TiAl composites with20%and50%reinforcing phase volumefraction. the synthesis process of Ti_2AlN/TiAl composites were divided into fourstages: the first stage began with Al completely melted(>665℃), TiAl3layer formedat Ti particles surface were the main new phase; in the second stage, Al powderparticipated in synthesis reaction and were depleted, multilayer Ti-Al compoundsbounding Ti particles, minor amounts of small-grained Ti_2AlN particles formed atTiAl3layer edge by liquation reaction; the third stage was at temperature1100℃to1300℃, the base material transformed into TiAl(the core were Ti3Al) at hightemperature, at this time, TiN particles closely contacted with TiAl; at the fourthstage, kept the temperature at1300℃for1h, TiN completely reacted with TiAl andformed many Ti_2AlN particles, the base material homogenizing transformed intoTiAl phase, finally obtained Ti_2AlN/TiAl composites.
The base TiAl of Ti_2AlN/TiAl composites could transformed to full lamellar,duplex and near γ phase microstructure after heat treatment. For Ti_2AlN/TiAlcomposites that with full lamellar microstructure TiAl base, the hardness and elasticmodulus increased with the increase of Ti_2AlN volume fraction; at high temperature(800℃), bending strength increased at first and then decreased with Ti_2AlN volumefraction increased, the maximum bending strength of the composites happenedwhen Ti_2AlN volume fraction was20%, too high Ti_2AlN volume fraction wasunfavorable to bending strength.
Oxidation test was carried out at800℃to900℃in air. At900℃, the typicaloxidation process of Ti_2AlN/TiAl composites were divided into two stages: initial stage was fast oxidation stage of phase (or grain) boundary and surface layer, thencarried out the oxide layer continuously thickened oxidation stage, which wascontrolled by diffusion, the oxidation rate decreased with the thickness of the oxidelayer increased. At900℃in air, from outer to inner, the oxide layer were dividedinto two layers, they were TiO2layer and (Al2O3+TiO2+Ti5Al3O2) mixed oxide layer.
Hot compression test results showed that, compressive strength of TiAl alloyand Ti_2AlN/TiAl composites were all decreased with temperature increased, andwere increased with strain rates increased; at high temperature high strain rates andlow temperature low strain rates, compressive strength of composites increased40%~50%compared with TiAl. Besides sliding, hot compressive deformationmethod of Ti_2AlN/TiAl composites also contained grain boundary sliding oflamellar microstructure, lamellar bending, interlamellar sliding, twin crystal andrecrystallization and so on. In low Ti_2AlN volume fraction composites, Ti_2AlNparticles that were at grain boundary could hinder grain boundary sliding, this washelpful to enhance material strength; In high Ti_2AlN volume fraction composites,Ti_2AlN that were connected to hard frame could effectively carrying strength, thatsignificantly enhanced the compressive strength of Ti_2AlN/TiAl composites.
In friction and wear test, room temperature friction process of Ti_2AlN/TiAlcomposites-nickel base alloy friction pair were divided into two stages: Ⅰ stage wasunsteady state friction, nickel base alloy was the wore side, adhesive wear of nickelbase alloy adhered on composites wear face was the wear type; Ⅱ stage was steadystate friction, nickel base alloy still was the main wore side, wear type was abrasivewear of Ti_2AlN/TiAl composites to nickel base alloy, at the same time, Ti_2AlN/TiAlcomposites was adhesive wear. At room temperature, coefficient of friction andwear loss of friction pair increased with load increased; with sliding speedincreased, total wear loss of composites increased, coefficient of friction and wearrate of Ti_2AlN/TiAl composites decreased.
At high temperature, the friction pair happened oxidation reaction, Ni alloyoxide to NiO, Ti_2AlN/TiAl composites oxide to Al_2O_3and TiO_2. Friction process ofTi_2AlN/TiAl composites-nickel base alloy friction pair were divided into threestages: Ⅰ stage was unsteady state-coefficient of friction increase stage, occurredadhesive wear of nickel base alloy; Ⅱ stage was unsteady state-coefficient offriction decrease stage, wear type of nickel base alloy changed from adhesive wearto abrasive wear, wear type of composites mainly were adhesive wear; Ⅲ stage was steady state-coefficient of friction stable stage, nickel base alloy was the main woreside, abrasive wear was the wear type. At high temperature, with the increase ofsliding speed, coefficient of friction and wear rate decreased, and total wear loss ofcomposites increased; with temperature increased, coefficient of friction and wearloss of composites were all decreased. No matter at room temperature or hightemperature friction test, the wear loss of composites were lower than that of TiAlbase alloy, with the increase of Ti_2AlN volume fraction, the wear loss of compositesdecreased.
原材料Ti、Al和TiN颗粒，采用热压烧结工艺，合成制备出增强相体积分数为20%和50%的Ti_2AlN/TiAl复合材料。该复合材料合成过程分为四个阶段：第一阶段Al粉完全熔化(>665℃)，此时在Ti颗粒表面形成TiAl3相；第二阶段Al粉参与合成反应而耗尽，Ti颗粒周围形成多层Ti-Al系化合物包围的层状结构，在TiAl3层边缘位置通过熔析反应形成了少量细小的Ti_2AlN颗粒；第三阶段(1100~1300℃期间)，高温下基体材料转变为TiAl(芯部为Ti3Al)，此时的TiN颗粒与TiAl紧密接触；第四阶段(1300℃保温、保压1小时处理)，TiN颗粒与TiAl完全反应得到大量Ti_2AlN颗粒，基体均匀化转变成TiAl相，最终得到Ti_2AlN/TiAl复合材料。
Ti_2AlN/TiAl复合材料的基体合金可通过热处理转变成全片层、双态和近γ相组织。其中，全片层TiAl基体组织的Ti_2AlN/TiAl复合材料硬度和弹性模量随Ti_2AlN颗粒体积分数增加而升高；高温(800℃)下，弯曲强度随Ti_2AlN颗粒体积分数增加而先升高后降低， Ti_2AlN颗粒体积分数占20%的复合材料弯曲强度最高，Ti_2AlN颗粒体积分数过高对强度不利。
氧化试验在800~900℃空气条件下进行。900℃下，Ti_2AlN/TiAl复合材料的典型氧化过程分为2个阶段：初期为相（晶）界和表面层快速氧化阶段，随后进入氧化层不断增厚的受扩散控制氧化阶段，随着氧化层厚度的增加氧化速率逐渐减缓。900℃空气条件下，氧化层自外向内分为两层，分别为TiO2层和(Al2O3+TiO2+Ti5Al3O2)混合层。
热压缩试验结果表明：随温度升高，TiAl合金和Ti_2AlN/TiAl复合材料的压缩强度均降低，而随着应变速率增加压缩强度升高；在高温高应变速率和低温低应变速率条件下，Ti_2AlN/TiAl复合材料的强度比基体TiAl合金提高40~50%。Ti_2AlN/TiAl复合材料热压缩变形方式除滑移外，还有TiAl片层组织晶界滑动、片层弯曲、片层间滑动、孪晶、再结晶等。低体积分数Ti_2AlN/TiAl复合材料中，位于晶界处的Ti_2AlN颗粒能够阻碍TiAl晶界滑动，有利于提高材料强度；高体积分数的Ti_2AlN/TiAl复合材料中，联接成三维网络结构的Ti_2AlN增强体能够有效承载，明显提高了复合材料压缩强度。
摩擦磨损试验结果表明：Ti_2AlN/TiAl复合材料与镍基合金组成的摩擦副，室温摩擦过程主要分为两个阶段：Ⅰ阶段为非稳态摩擦阶段，镍基合金是主要磨损方，磨损类型是镍基合金附着在复合材料磨面上的粘着磨损；Ⅱ阶段为稳态摩擦阶段，镍基合金仍然是主要磨损方，磨损方式是Ti_2AlN/TiAl复合材料对其产生的磨粒磨损，同时Ti_2AlN/TiAl复合材料发生粘着磨损。室温下，载荷增加，摩擦系数和磨损量均升高；滑动速度加快，Ti_2AlN/TiAl复合材料总磨损量增加，摩擦系数和复合材料的磨损率降低。
高温下摩擦副发生氧化，镍基合金氧化产物为NiO，Ti_2AlN/TiAl复合材料的氧化产物为Al_2O_3和TiO_2。Ti_2AlN/TiAl复合材料-镍基合金高温摩擦过程主要分为三个阶段：Ⅰ阶段为非稳态-摩擦系数上升阶段，镍基合金发生粘着磨损；Ⅱ阶段为非稳态-摩擦系数下降阶段，镍基合金的磨损方式从粘着磨损向磨粒磨损转变，复合材料磨损方式主要是粘着磨损；Ⅲ阶段为稳态-摩擦系数平稳阶段，镍基合金是主要磨损方，磨损类型为磨粒磨损。高温下，随着滑动速度增加，摩擦系数和复合材料磨损率均降低，复合材料的总磨损量上升；温度升高，摩擦系数和复合材料磨损量均下降。不论在室温还是高温摩擦试验中，复合材料磨损量均低于TiAl基体合金，Ti_2AlN体积分数增加，复合材料的磨损量随之降低。
In this paper, in situ Ti_2AlN/TiAl composites were designed and fabricated.Microstructure and synthesis mechanism of Ti_2AlN/TiAl composites weresystematically investigated by scanning electron microscope(SEM), transmissionelectron microscope(TEM), X ray diffraction(XRD), differential scanningcalorimetry(DSC) and so on. Properties of Ti_2AlN/TiAl composites were tested bythree-point bending, oxidation, hot compression and friction and wear, relatedfactors were also analyzed.
Ti, Al and TiN particles were raw materials, used hot-pressing technique tofabricated Ti_2AlN/TiAl composites with20%and50%reinforcing phase volumefraction. the synthesis process of Ti_2AlN/TiAl composites were divided into fourstages: the first stage began with Al completely melted(>665℃), TiAl3layer formedat Ti particles surface were the main new phase; in the second stage, Al powderparticipated in synthesis reaction and were depleted, multilayer Ti-Al compoundsbounding Ti particles, minor amounts of small-grained Ti_2AlN particles formed atTiAl3layer edge by liquation reaction; the third stage was at temperature1100℃to1300℃, the base material transformed into TiAl(the core were Ti3Al) at hightemperature, at this time, TiN particles closely contacted with TiAl; at the fourthstage, kept the temperature at1300℃for1h, TiN completely reacted with TiAl andformed many Ti_2AlN particles, the base material homogenizing transformed intoTiAl phase, finally obtained Ti_2AlN/TiAl composites.
The base TiAl of Ti_2AlN/TiAl composites could transformed to full lamellar,duplex and near γ phase microstructure after heat treatment. For Ti_2AlN/TiAlcomposites that with full lamellar microstructure TiAl base, the hardness and elasticmodulus increased with the increase of Ti_2AlN volume fraction; at high temperature(800℃), bending strength increased at first and then decreased with Ti_2AlN volumefraction increased, the maximum bending strength of the composites happenedwhen Ti_2AlN volume fraction was20%, too high Ti_2AlN volume fraction wasunfavorable to bending strength.
Oxidation test was carried out at800℃to900℃in air. At900℃, the typicaloxidation process of Ti_2AlN/TiAl composites were divided into two stages: initial stage was fast oxidation stage of phase (or grain) boundary and surface layer, thencarried out the oxide layer continuously thickened oxidation stage, which wascontrolled by diffusion, the oxidation rate decreased with the thickness of the oxidelayer increased. At900℃in air, from outer to inner, the oxide layer were dividedinto two layers, they were TiO2layer and (Al2O3+TiO2+Ti5Al3O2) mixed oxide layer.
Hot compression test results showed that, compressive strength of TiAl alloyand Ti_2AlN/TiAl composites were all decreased with temperature increased, andwere increased with strain rates increased; at high temperature high strain rates andlow temperature low strain rates, compressive strength of composites increased40%~50%compared with TiAl. Besides sliding, hot compressive deformationmethod of Ti_2AlN/TiAl composites also contained grain boundary sliding oflamellar microstructure, lamellar bending, interlamellar sliding, twin crystal andrecrystallization and so on. In low Ti_2AlN volume fraction composites, Ti_2AlNparticles that were at grain boundary could hinder grain boundary sliding, this washelpful to enhance material strength; In high Ti_2AlN volume fraction composites,Ti_2AlN that were connected to hard frame could effectively carrying strength, thatsignificantly enhanced the compressive strength of Ti_2AlN/TiAl composites.
In friction and wear test, room temperature friction process of Ti_2AlN/TiAlcomposites-nickel base alloy friction pair were divided into two stages: Ⅰ stage wasunsteady state friction, nickel base alloy was the wore side, adhesive wear of nickelbase alloy adhered on composites wear face was the wear type; Ⅱ stage was steadystate friction, nickel base alloy still was the main wore side, wear type was abrasivewear of Ti_2AlN/TiAl composites to nickel base alloy, at the same time, Ti_2AlN/TiAlcomposites was adhesive wear. At room temperature, coefficient of friction andwear loss of friction pair increased with load increased; with sliding speedincreased, total wear loss of composites increased, coefficient of friction and wearrate of Ti_2AlN/TiAl composites decreased.
At high temperature, the friction pair happened oxidation reaction, Ni alloyoxide to NiO, Ti_2AlN/TiAl composites oxide to Al_2O_3and TiO_2. Friction process ofTi_2AlN/TiAl composites-nickel base alloy friction pair were divided into threestages: Ⅰ stage was unsteady state-coefficient of friction increase stage, occurredadhesive wear of nickel base alloy; Ⅱ stage was unsteady state-coefficient offriction decrease stage, wear type of nickel base alloy changed from adhesive wearto abrasive wear, wear type of composites mainly were adhesive wear; Ⅲ stage was steady state-coefficient of friction stable stage, nickel base alloy was the main woreside, abrasive wear was the wear type. At high temperature, with the increase ofsliding speed, coefficient of friction and wear rate decreased, and total wear loss ofcomposites increased; with temperature increased, coefficient of friction and wearloss of composites were all decreased. No matter at room temperature or hightemperature friction test, the wear loss of composites were lower than that of TiAlbase alloy, with the increase of Ti_2AlN volume fraction, the wear loss of compositesdecreased.
引文
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