(TiB+La_2O_3)增强高温钛基复合材料组织和性能研究
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摘要
钛基复合材料是指在钛或钛合金中引入增强体的一种复合材料。它把基体的延展性、韧性与增强体的高强度、高模量结合起来，从而获得比钛或钛合金更高的比强度、比刚度和抗高温性能，有望应用在超高音速宇航飞行器和先进航空发动机上。为了更好发挥钛基复合材料的潜力，需要采用合理的热加工工艺和热处理工艺。其中，关于钛基复合材料热处理方面的研究很少。目前常用的α+β热处理工艺的蠕变性能不佳，β热处理工艺的塑性不理想。所以，本文设计了新型的热处理工艺，以期能提高钛基复合材料综合力学性能，主要开展了以下研究工作：
利用Ti与LaB6之间的反应，采用熔铸法成功制备了以IMI834为基体，增强体TiB体积分数为1.26%，La_2O_3为0.582%的原位自生的钛基复合材料。铸锭直径为φ580mm，增强体TiB呈长条状随机分布，La_2O_3以纳米级的小颗粒弥散分布在基体中。热加工采用了等温快锻工艺，在β相区开坯，在两相区终锻为φ70mm的棒材，加工后增强体TiB沿加工方向定向分布。
研究了近α钛合金的相变规律，设计出了新型的热处理工艺，即β三段热处理工艺，也就是在β相区固溶处理后，在α+β两相区上部进行第二次热处理，然后时效。其中在β相区加热保温后采取了不同的冷却方式：水冷、油冷和空冷。同时还制定了常用的α+β热处理工艺和β热处理工艺。经β三段热处理后材料的组织为α片层组织，α片层长径比较大，并且在β相区热处理时采用的冷却速率越快，α片层宽度越小。α+β热处理后组织为双态组织，β热处理后的组织为魏氏组织。β热处理与β三段热处理相比，α片层宽度从小到大的工艺依次为β三段水冷、β三段油冷、β热处理、β三段空冷热处理。在热处理过程中，增强体稳定，形态上基本没有变化，并且增强体与基体的界面清晰没有界面反应。但是在β相区热处理过程中，增强体TiB和La_2O_3阻碍β晶界运动，从而减弱了β相区加热时β晶粒长大。增强体能促进形核，α相在TiB周围以一定的取向析出长大，增强体密集的区域晶粒较小，取向差较大。
热处理后的性能比较，经α+β、β三段水冷和β三段油冷热处理后的材料具有良好的室温和高温拉伸性能，β三段空冷热处理的次之，β热处理的较差。室温时，经α+β、β三段水冷和β三段油冷热处理后材料的延伸率较β热处理的约提高了1倍。高温时随着温度升高，材料的抗拉强度都下降，延伸率都升高。β三段水冷热处理后材料的高温延伸率最好，β三段油冷和α+β热处理的次之，β热处理的最差。在700℃拉伸时，β三段水冷热处理后材料的抗拉强度较β热处理的减少30MPa时，延伸率则较β热处理的提高2.06倍。材料高温热暴露100小时后室温抗拉强度稍有提高，延伸率显著下降，热处理对材料热稳定性影响与室温拉伸一致。材料α+β热处理后的蠕变速率最高，β热处理的最低，β三段油冷热处理的较β热处理的稍高，但大部分仍然在一个数量级，α片层越粗大蠕变速率越低。材料β热处理后的断裂韧性值最低，β三段油冷热处理后的最高。β三段油冷热处理后的断裂韧性较β热处理后的提高了47%。双态组织由于初生α相分布在β转变组织上，所以其塑性好，蠕变性能差。β热处理和β三段热处理得到的魏氏和α片层组织，α片层越粗大蠕变性能越好，而α片层、α＋β集束宽度和β晶粒越小，塑性越好。
钛基复合材料中增强体TiB短纤维在室温和高温拉伸时的断裂机理为大于临界长径比的TiB短纤维承载断裂。由于临界长径比随着温度升高而增大，高温时有很少量的TiB短纤维端部脱粘现象。在高温热暴露100h后增强体形态基本没有变化，界面依然整洁，增强体稳定。蠕变后观察到大量的晶间断裂和TiB增强体与基体脱粘，说明在长时间高温暴露服役后，晶界强度和增强体与基体界面强度都降低，增强体与基体界面强度同晶界强度相近。La由于吸收了基体合金中的氧生成了的La_2O_3小颗粒弥散分布在材料中，起弥散强化作用。La_2O_3小颗粒有利于提高材料的强度、热稳定性和蠕变抗力。
Titanium matrix composites (TMCs), reinforced with ceramic particles, haveconsiderable potential for improving properties and service temperature and can beextensively applied in areas such as aerospace, advanced weapon systems, because oftheir high specific strength, good specific modulus and resistance to elevated temperatures.With the development of titanium matrix composites, the researches on improving alloy’schemical composition, reinforcement choice and prepared of titanium matrix compositesare much more than heat treatment about titanium matrix composites. However, it iswell-known that heat treatments can improve effectively Ti alloys’ properties. Therefore,improving the comprehensive properties of TMCs by heat treatment becomes much moreimportant. A new heat treatment method, TRIPLEX heat treatment, is adopted and theeffects of it on microstructure and properties of TMCs are investigated in my paper.
In situ synthesized (TiB+La_2O_3)/IMI834composites were prepared in a consumablevacuum arc-remelting furnace as reaction between Ti and LaB6. The theoretical volumefraction of TiB and La_2O_3is1.82%and0.58%respectively. The ingots (Φ580mm) werehot-forged into rods with a diameter of Φ70mm. The majority of the TiB whiskerreinforcements were aligned along the direction of forging. The size of La_2O_3paticals arein the nano-scale. The reinforcements were uniformly distributed in the TMCs.
TRIPLEX heat treatment (β_3HT) is β solution (WQ, OQ, AC), α+β solution, andthen aging. TRIPLEX heat treatment, β heat treatment (βHT) and α+β heat treatment (α+βHT) were adopted in my paper. The microstructure of specimens after β_3HT heattreatment is laminar structure, that of βHT is widmanst tten, and α+βHT is bimodalstructure. The faster the cooling speeds are in β phase district, the thinner α laminar is.The width of α laminar after β_3(WQ, OQ)HT is thinner than that of βHT. The width of αcolony is more; the low angle grain boundaries are more. After heat treatment, theinterface between reinforcement and matrix is clear, so both the TiB whiskers and La_2O_3particles are stable without interfacial reaction. Reinforcements prevent grain boundarymigration during grain growth, β grain decrease. The different of matrix orientationincreases around of reinforcements.
Tensile properties of TMCs after α+βHT, β_3(WQ) HT and β_3(OQ) HT are best, andβ_3(AC) HT the better, and β(AC) the worst one. The elongation of specimens after β_3(OQ,WQ) HT and α+βHT is increase as twice as that of β(AC). With temperature increasing,ultimate strength of specimens decreases, but elongation increases significantly. Theelongation of specimens after β_3(WQ) HT is best, β_3(OQ)HT and α+βHTi is better, thenβ(AC)HT is worst. At700℃, elongation of specimens after β_3(WQ) HT improves no lessthan200%compared with that of β(AC)HT. After thermal exposure, only a slight changeof ultimate strength has been found, however the ductility of specimens is sharply reducedafter thermal exposure. The ductility of all specimens is the worst at650℃thermalexposure. Compared with specimens treated by thermal exposure at600℃and650℃, theductility of specimens thermal exposured at700℃shows an abnormal increase. Afterthermal exposure, the ductility of specimens treated by β_3HT and α+βHT heat treatmentis better than that of β heat treatment. With temperature and stress increasing, the steadystate creep rates increase. The steady state creep rates of specimens treated by α+βHT isfastest, that of β_3(OQ) HT increases slightly compared with β HT. The fracture toughnessof α+Βht, β_3(OQ)HT, β_3(WQ)HT and β_3(AC)HT increases22%,34%,50.5%and34%respectively compared with β HT.
The fracture mechanism of TMCs is that if a short fiber with AR(AR: length-to-diameter ratio) is higher than critical aspect ratio (ARc), TiB whiskers bear tensile stress inthe processing of tensile. Most TiB whiskers of the TMCs are higher than ARc. Withtemperature increasing, ARcof TiB whiskers increase, so few debonding TiB whiskers areobserved. Both the TiB whiskers and La_2O_3particles are stable without interfacial reactionafter hermal exposure at600℃,650℃and700℃for100h, the stable reinforcements can ensure the stability of TMCs. After creep fractured, large numbers of interface debondingsbetween TiB whiskers and matrix are observed. This is attributed to both the interfacestrength and grain boundary strength decrease at high temperature for long time. La canreduce oxygen concentration, depress precipitate of Ti3Al. The reinforcement of La_2O_3canimprove the strength, thermal stability and creep properties of TMCs.
利用Ti与LaB6之间的反应，采用熔铸法成功制备了以IMI834为基体，增强体TiB体积分数为1.26%，La_2O_3为0.582%的原位自生的钛基复合材料。铸锭直径为φ580mm，增强体TiB呈长条状随机分布，La_2O_3以纳米级的小颗粒弥散分布在基体中。热加工采用了等温快锻工艺，在β相区开坯，在两相区终锻为φ70mm的棒材，加工后增强体TiB沿加工方向定向分布。
研究了近α钛合金的相变规律，设计出了新型的热处理工艺，即β三段热处理工艺，也就是在β相区固溶处理后，在α+β两相区上部进行第二次热处理，然后时效。其中在β相区加热保温后采取了不同的冷却方式：水冷、油冷和空冷。同时还制定了常用的α+β热处理工艺和β热处理工艺。经β三段热处理后材料的组织为α片层组织，α片层长径比较大，并且在β相区热处理时采用的冷却速率越快，α片层宽度越小。α+β热处理后组织为双态组织，β热处理后的组织为魏氏组织。β热处理与β三段热处理相比，α片层宽度从小到大的工艺依次为β三段水冷、β三段油冷、β热处理、β三段空冷热处理。在热处理过程中，增强体稳定，形态上基本没有变化，并且增强体与基体的界面清晰没有界面反应。但是在β相区热处理过程中，增强体TiB和La_2O_3阻碍β晶界运动，从而减弱了β相区加热时β晶粒长大。增强体能促进形核，α相在TiB周围以一定的取向析出长大，增强体密集的区域晶粒较小，取向差较大。
热处理后的性能比较，经α+β、β三段水冷和β三段油冷热处理后的材料具有良好的室温和高温拉伸性能，β三段空冷热处理的次之，β热处理的较差。室温时，经α+β、β三段水冷和β三段油冷热处理后材料的延伸率较β热处理的约提高了1倍。高温时随着温度升高，材料的抗拉强度都下降，延伸率都升高。β三段水冷热处理后材料的高温延伸率最好，β三段油冷和α+β热处理的次之，β热处理的最差。在700℃拉伸时，β三段水冷热处理后材料的抗拉强度较β热处理的减少30MPa时，延伸率则较β热处理的提高2.06倍。材料高温热暴露100小时后室温抗拉强度稍有提高，延伸率显著下降，热处理对材料热稳定性影响与室温拉伸一致。材料α+β热处理后的蠕变速率最高，β热处理的最低，β三段油冷热处理的较β热处理的稍高，但大部分仍然在一个数量级，α片层越粗大蠕变速率越低。材料β热处理后的断裂韧性值最低，β三段油冷热处理后的最高。β三段油冷热处理后的断裂韧性较β热处理后的提高了47%。双态组织由于初生α相分布在β转变组织上，所以其塑性好，蠕变性能差。β热处理和β三段热处理得到的魏氏和α片层组织，α片层越粗大蠕变性能越好，而α片层、α＋β集束宽度和β晶粒越小，塑性越好。
钛基复合材料中增强体TiB短纤维在室温和高温拉伸时的断裂机理为大于临界长径比的TiB短纤维承载断裂。由于临界长径比随着温度升高而增大，高温时有很少量的TiB短纤维端部脱粘现象。在高温热暴露100h后增强体形态基本没有变化，界面依然整洁，增强体稳定。蠕变后观察到大量的晶间断裂和TiB增强体与基体脱粘，说明在长时间高温暴露服役后，晶界强度和增强体与基体界面强度都降低，增强体与基体界面强度同晶界强度相近。La由于吸收了基体合金中的氧生成了的La_2O_3小颗粒弥散分布在材料中，起弥散强化作用。La_2O_3小颗粒有利于提高材料的强度、热稳定性和蠕变抗力。
Titanium matrix composites (TMCs), reinforced with ceramic particles, haveconsiderable potential for improving properties and service temperature and can beextensively applied in areas such as aerospace, advanced weapon systems, because oftheir high specific strength, good specific modulus and resistance to elevated temperatures.With the development of titanium matrix composites, the researches on improving alloy’schemical composition, reinforcement choice and prepared of titanium matrix compositesare much more than heat treatment about titanium matrix composites. However, it iswell-known that heat treatments can improve effectively Ti alloys’ properties. Therefore,improving the comprehensive properties of TMCs by heat treatment becomes much moreimportant. A new heat treatment method, TRIPLEX heat treatment, is adopted and theeffects of it on microstructure and properties of TMCs are investigated in my paper.
In situ synthesized (TiB+La_2O_3)/IMI834composites were prepared in a consumablevacuum arc-remelting furnace as reaction between Ti and LaB6. The theoretical volumefraction of TiB and La_2O_3is1.82%and0.58%respectively. The ingots (Φ580mm) werehot-forged into rods with a diameter of Φ70mm. The majority of the TiB whiskerreinforcements were aligned along the direction of forging. The size of La_2O_3paticals arein the nano-scale. The reinforcements were uniformly distributed in the TMCs.
TRIPLEX heat treatment (β_3HT) is β solution (WQ, OQ, AC), α+β solution, andthen aging. TRIPLEX heat treatment, β heat treatment (βHT) and α+β heat treatment (α+βHT) were adopted in my paper. The microstructure of specimens after β_3HT heattreatment is laminar structure, that of βHT is widmanst tten, and α+βHT is bimodalstructure. The faster the cooling speeds are in β phase district, the thinner α laminar is.The width of α laminar after β_3(WQ, OQ)HT is thinner than that of βHT. The width of αcolony is more; the low angle grain boundaries are more. After heat treatment, theinterface between reinforcement and matrix is clear, so both the TiB whiskers and La_2O_3particles are stable without interfacial reaction. Reinforcements prevent grain boundarymigration during grain growth, β grain decrease. The different of matrix orientationincreases around of reinforcements.
Tensile properties of TMCs after α+βHT, β_3(WQ) HT and β_3(OQ) HT are best, andβ_3(AC) HT the better, and β(AC) the worst one. The elongation of specimens after β_3(OQ,WQ) HT and α+βHT is increase as twice as that of β(AC). With temperature increasing,ultimate strength of specimens decreases, but elongation increases significantly. Theelongation of specimens after β_3(WQ) HT is best, β_3(OQ)HT and α+βHTi is better, thenβ(AC)HT is worst. At700℃, elongation of specimens after β_3(WQ) HT improves no lessthan200%compared with that of β(AC)HT. After thermal exposure, only a slight changeof ultimate strength has been found, however the ductility of specimens is sharply reducedafter thermal exposure. The ductility of all specimens is the worst at650℃thermalexposure. Compared with specimens treated by thermal exposure at600℃and650℃, theductility of specimens thermal exposured at700℃shows an abnormal increase. Afterthermal exposure, the ductility of specimens treated by β_3HT and α+βHT heat treatmentis better than that of β heat treatment. With temperature and stress increasing, the steadystate creep rates increase. The steady state creep rates of specimens treated by α+βHT isfastest, that of β_3(OQ) HT increases slightly compared with β HT. The fracture toughnessof α+Βht, β_3(OQ)HT, β_3(WQ)HT and β_3(AC)HT increases22%,34%,50.5%and34%respectively compared with β HT.
The fracture mechanism of TMCs is that if a short fiber with AR(AR: length-to-diameter ratio) is higher than critical aspect ratio (ARc), TiB whiskers bear tensile stress inthe processing of tensile. Most TiB whiskers of the TMCs are higher than ARc. Withtemperature increasing, ARcof TiB whiskers increase, so few debonding TiB whiskers areobserved. Both the TiB whiskers and La_2O_3particles are stable without interfacial reactionafter hermal exposure at600℃,650℃and700℃for100h, the stable reinforcements can ensure the stability of TMCs. After creep fractured, large numbers of interface debondingsbetween TiB whiskers and matrix are observed. This is attributed to both the interfacestrength and grain boundary strength decrease at high temperature for long time. La canreduce oxygen concentration, depress precipitate of Ti3Al. The reinforcement of La_2O_3canimprove the strength, thermal stability and creep properties of TMCs.
引文
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