CN108754371B - A preparation method for refining near-alpha high temperature titanium alloy grains - Google Patents
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Abstract
Description
技术领域technical field
本发明属于钛合金技术领域,具体涉及一种细化近α高温钛合金晶粒的制备方法。The invention belongs to the technical field of titanium alloys, and in particular relates to a preparation method for refining near-alpha high temperature titanium alloy crystal grains.
背景技术Background technique
近α高温钛合金是现代航空发动机的关键材料之一,它主要用做航空发动机的压气机盘叶片、机匣,以减轻发动机质量,减小推重比。发动机对高温钛合金的性能要求是非常苛刻的,它要求要求钛合金结构材料具有高比强度、高比刚度、高韧性、高损伤容限以及可焊接等优良的综合性能匹配。由于这些性能指标对材料的成分与微观组织要求往往是矛盾的,因此单纯的改善成分已经无法满足钛合金作为结构材料朝着高速化、大型化、结构复杂化等方向的跨越式发展、航空航天、兵器、船舶等武器装备各承力构件、承力螺栓等紧固件均对高强钛合金及超高强度钛合金提出了明确需求。近年来,传统的热加工技术如锻造、轧制及挤压等材料成形方法逐渐用到钛合金中以调控优化其组织性能,在一定程度上实现了强度与塑形的同时优化,但大量研究已经证明,传统热变形工艺在改善钛合金的组织性能方面存在功率损耗大、提升性能效果不理想等缺点,目前仍然不能突破钛合金发展应用的“瓶颈”,而大量的研究证明α相晶粒尺寸的大小对钛合金的强度和塑形有显著影响,细化α相晶粒尺寸被证明能够有效地增强钛合金的强度和塑性,与此同时,对热加工后的钛合金材料进行一系列的热处理逐渐获得了研究者的青睐,其中快速热处理以其在短时间的热处理过程中使得晶粒来不及长大而细化晶粒而慢慢被人们所看重。Near-alpha high temperature titanium alloy is one of the key materials of modern aero-engines. It is mainly used as compressor disc blades and casings of aero-engines to reduce the mass of the engine and reduce the thrust-to-weight ratio. The performance requirements of high-temperature titanium alloys for engines are very demanding. It requires titanium alloy structural materials to have high specific strength, high specific stiffness, high toughness, high damage tolerance, and weldability. Excellent comprehensive performance matching. Since these performance indicators often contradict the requirements for the composition and microstructure of the material, simply improving the composition can no longer meet the leap-forward development of titanium alloys as structural materials in the direction of high speed, large size, and complex structure. , weapons, ships and other weapons and equipment, all load-bearing components, load-bearing bolts and other fasteners have put forward clear requirements for high-strength titanium alloys and ultra-high-strength titanium alloys. In recent years, traditional hot processing techniques such as forging, rolling and extrusion have been gradually used in titanium alloys to control and optimize their microstructure and properties, and to a certain extent, the simultaneous optimization of strength and plasticity has been achieved, but a large number of researches It has been proved that the traditional hot deformation process has disadvantages such as large power loss and unsatisfactory performance improvement effect in improving the microstructure and properties of titanium alloys. At present, it is still unable to break through the "bottleneck" of the development and application of titanium alloys, and a large number of studies have proved that the α-phase grains The size of the titanium alloy has a significant effect on the strength and plasticity of the titanium alloy. Refining the grain size of the α phase has been proved to effectively enhance the strength and plasticity of the titanium alloy. At the same time, a series of The rapid heat treatment has gradually gained the favor of researchers, and the rapid heat treatment has gradually been valued by people because it makes the grains have no time to grow and refines the grains in the short-term heat treatment process.
发明内容SUMMARY OF THE INVENTION
本发明针对现有近α高温钛合金强度-塑性-韧性的匹配性较低的问题,提供一种细化近α高温钛合金晶粒的制备方法。Aiming at the problem of low strength-plasticity-toughness matching of existing near-α high temperature titanium alloys, the present invention provides a preparation method for refining near-α high temperature titanium alloy crystal grains.
本发明采用如下技术方案:The present invention adopts following technical scheme:
一种细化近α高温钛合金晶粒的制备方法,包括如下步骤:A preparation method for refining near-alpha high temperature titanium alloy grains, comprising the following steps:
第一步,通过金相法测定近α高温钛合金的α+β/β相变点;The first step is to determine the α+β/β transformation point of the near-α high temperature titanium alloy by metallographic method;
第二步,低温多道次单辊角轧:将近α高温钛合金在α+β/β相变点以下300-400℃进行变形量为70%的快速锻造,为了获得较高的畸变能,为后续的晶粒的析出提供更多能量,将变形速率为1mm/s;将快速锻造后的试样在相同的温度进行轧制,将试样的厚度控制在1mm,以便进行单辊角轧;使用电火花线切割在轧制后的试样上切取长度为200mm,宽度为20mm的试样,在α+β/β相变点以下300-400℃进行低温多道次单辊角轧;The second step, multi-pass single roll angle rolling at low temperature: rapid forging of nearly α high temperature titanium alloy at 300-400 °C below the α+β/β transformation point with a deformation amount of 70%, in order to obtain higher distortion energy, for the follow-up The precipitation of the grains provides more energy, and the deformation rate is 1mm/s; the sample after rapid forging is rolled at the same temperature, and the thickness of the sample is controlled at 1mm for single-roll angle rolling; use Wire-cut EDM Cut a sample with a length of 200mm and a width of 20mm from the rolled sample, and perform low-temperature multi-pass single-roll angle rolling at 300-400°C below the α+β/β transformation point;
第三步,在α+β/β相变点附近的快速热处理:将低温多道次单辊角轧后的试样通过电火花线切割一定尺寸的试样,分别在α+β/β相变点以上15℃、α+β/β相变点处、α+β/β相变点以下15℃保温2min后,水淬冷却至室温。The third step, rapid heat treatment near the α+β/β transformation point: the sample after low-temperature multi-pass single-roll angle rolling is cut to a certain size by EDM, and the samples are respectively 15 above the α+β/β transformation point. ℃, at the α+β/β phase transition point, and at 15°C below the α+β/β phase transition point for 2 minutes, then water quenched and cooled to room temperature.
第二步中所述低温多道次单辊角轧的过程如下:首先将轧制后的近α高温钛合金轧片在高压扭转机中进行环向剪切变形,试样初始厚度为1mm,经环向剪切变形后厚度为0.96mm,随后将试样进行等通道角挤压,通道高度为1mm,即试样经等通道角挤压后的厚度仍为1mm,其中试样所经受的环向剪切变形与等通道角挤压相继进行,均在高压扭转机中进行。The process of the low-temperature multi-pass single-roll angle rolling in the second step is as follows: first, the rolled near-α high-temperature titanium alloy sheet is subjected to hoop shear deformation in a high-pressure torsion machine, and the initial thickness of the sample is 1 mm. After the hoop shear deformation, the thickness is 0.96mm, and then the sample is subjected to equal channel angular extrusion, and the channel height is 1 mm, that is, the thickness of the sample after the equal channel angular extrusion is still 1 mm. Circumferential shear deformation and equal channel angular extrusion are successively performed in a high-pressure torsion machine.
第三步中所切割的试样尺寸为60mm*15mm*1mm。The size of the sample cut in the third step is 60mm*15mm*1mm.
由于变形道次对试样的显微组织与力学性能均有影响,为避免变量过多,采用3道次的的单辊角轧。Since the deformation passes have an effect on the microstructure and mechanical properties of the samples, in order to avoid too many variables, three passes of single-roll angle rolling are used.
本发明的有益效果如下:The beneficial effects of the present invention are as follows:
1. 本发明在不同于传统的热变形工艺的基础上,通过低温多道次单辊角轧,使得晶粒内部获得更多的孪晶、位错,这些缺陷能够储存更多的畸变能,从而显著降低再结晶温度,促进再结晶,进一步通过在β相区或α+β相区快速热处理保留细化的再结晶晶粒,使其来不及长大,从而细化β晶粒。另外,在随后的冷却至室温的过程中,之前低温多道次单辊角轧所保留下来的大量亚晶、孪晶和位错一方面阻碍晶界的移动,另一方面可以作为α相的形核位置,将会显著细化α晶粒从而进一步提高钛合金的强度和塑形。1. The present invention is different from the traditional thermal deformation process, through low-temperature multi-pass single-roll angle rolling, so that more twins and dislocations are obtained inside the grains, and these defects can store more distortion energy, Thereby, the recrystallization temperature is significantly reduced, recrystallization is promoted, and the refined recrystallized grains are retained by rapid heat treatment in the β phase region or the α+β phase region, so that it is too late to grow, thereby refining the β grains. In addition, in the subsequent process of cooling to room temperature, a large number of subgrains, twins and dislocations retained by the previous low-temperature multi-pass single-roller angle rolling hinder the movement of grain boundaries on the one hand, and can act as α phase on the other hand. The nucleation site will significantly refine the α grains to further improve the strength and shape of the titanium alloy.
2. 本发明可制备出β晶粒组织细小、且有优良的强度-塑性-韧性匹配的近α高温钛合金,且加工方法适用于工业化生产。2. The present invention can prepare a near-α high-temperature titanium alloy with fine β-grain structure and excellent strength-plasticity-toughness matching, and the processing method is suitable for industrial production.
3. 本发明得到的近α高温钛合金可将α相的晶粒尺寸细化至1.2μm,再此尺寸下的合金可获得最优的综合力学性能,其抗拉强度可达1126.3MPa,屈服强度可达1097.5 MPa,延伸率可达18.6%。3. The near-α high temperature titanium alloy obtained by the present invention can refine the grain size of the α phase to 1.2 μm, and the alloy under this size can obtain the best comprehensive mechanical properties, and its tensile strength can reach 1126.3MPa, yielding The strength can reach 1097.5 MPa, and the elongation can reach 18.6%.
附图说明Description of drawings
图1为本发明实施例1的快速热处理温度1030℃的试样的SEM图;Fig. 1 is the SEM image of the sample with the rapid heat treatment temperature of 1030 ℃ in Example 1 of the present invention;
图2为本发明实施例2的快速热处理温度1030℃的试样的SEM图;2 is a SEM image of a sample with a rapid heat treatment temperature of 1030° C. in Example 2 of the present invention;
图3为本发明实施例3的快速热处理温度1030℃的试样的SEM图。FIG. 3 is a SEM image of a sample with a rapid heat treatment temperature of 1030° C. in Example 3 of the present invention.
具体实施方式Detailed ways
实施例1Example 1
第一步,近α高温钛合金Ti-1100(Ti–6Al–2.75Sn–4Zr–0.4Mo–0.45Si),α+β/β相变点通过金相法测得为1015℃;In the first step, near α high temperature titanium alloy Ti-1100 (Ti–6Al–2.75Sn–4Zr–0.4Mo–0.45Si), the α+β/β transformation point was measured by metallographic method to be 1015℃;
第二步,低温多道次单辊角轧:将采用真空感应磁悬浮熔炼炉制备出的近α高温钛合金Ti-1100铸锭(φ60mm*40mm)在715℃进行第一步快速锻造,变形量为70%,变形速率为1mm/s;将快速锻造后的试样在715℃进行轧制,将试样的厚度控制在1mm;使用电火花线切割在轧制后的试样上切取长度为200mm,宽度为20mm的试样,放到高压扭转机中进行715℃的低温多道次单辊角轧,上述3个工步的变形称为一轮大塑性变形。由于变形道次对试样的显微组织与力学性能均有影响,为避免变量过多,本次实验均采用3道次的的单辊角轧;The second step, low-temperature multi-pass single-roll angle rolling: the near-α high-temperature titanium alloy Ti-1100 ingot (φ60mm*40mm) prepared by the vacuum induction magnetic levitation melting furnace is subjected to the first step of rapid forging at 715 °C, and the deformation is 70%, and the deformation rate is 1 mm/s; the rapid forging sample is rolled at 715 °C, and the thickness of the sample is controlled at 1 mm; the length of the rolled sample is cut by wire electric discharge cutting: The sample with a width of 200mm and a width of 20mm is placed in a high-pressure torsion machine for multi-pass single-roll angle rolling at a low temperature of 715°C. The deformation of the above three steps is called a round of large plastic deformation. Since the deformation passes have an effect on the microstructure and mechanical properties of the sample, in order to avoid too many variables, three passes of single-roll angle rolling were used in this experiment;
第三步,在α+β/β相变点附近的快速热处理:将低温多道次单辊角轧后的试样在通过电火花线切割切下尺寸为60mm*15mm*1mm的试样,分别在真空电阻炉中快速加热至1030℃、1015℃、1000℃,保温2min后,快速放到水中冷却至室温。The third step, rapid heat treatment near the α+β/β transformation point: cut the sample with a size of 60mm*15mm*1mm from the sample after the low-temperature multi-pass single-roller angle rolling by EDM wire cutting, respectively in Quickly heat to 1030°C, 1015°C, and 1000°C in a vacuum resistance furnace. After holding for 2 minutes, quickly put it in water and cool it to room temperature.
最后测得不同温度快速热处理的力学性能如表1所示,其中在1030℃快速热处理得到的综合力学性能较好:抗拉强度为1126.3MPa,屈服强度为1097.5MPa,延伸率可达18.6%。α相晶粒尺寸为1.2μm。Finally, the mechanical properties measured by rapid heat treatment at different temperatures are shown in Table 1. The comprehensive mechanical properties obtained by rapid heat treatment at 1030 °C are better: the tensile strength is 1126.3 MPa, the yield strength is 1097.5 MPa, and the elongation can reach 18.6%. The α-phase grain size is 1.2 μm.
表1 715℃变形温度下不同热处理条件的力学性能Table 1 Mechanical properties of different heat treatment conditions at deformation temperature of 715℃
实施例2Example 2
第一步,近α高温钛合金Ti-1100(Ti–6Al–2.75Sn–4Zr–0.4Mo–0.45Si),α+β/β相变点通过金相法测得为1015℃;In the first step, near α high temperature titanium alloy Ti-1100 (Ti–6Al–2.75Sn–4Zr–0.4Mo–0.45Si), the α+β/β transformation point was measured by metallographic method to be 1015℃;
第二步,低温多道次单辊角轧:将采用真空感应磁悬浮熔炼炉制备出的近α高温钛合金Ti-1100铸锭(φ60mm*40mm)在615℃进行第一步快速锻造,变形量为70%,变形速率为1mm/s;将快速锻造后的试样在615℃进行轧制,将试样的厚度控制在1mm;使用电火花线切割在轧制后的试样上切取长度为200mm,宽度为20mm的试样,放到高压扭转机中进行615℃的低温多道次单辊角轧,上述3个工步的变形称为一轮大塑性变形。由于变形道次对试样的显微组织与力学性能均有影响,为避免变量过多,本次实验均采用3道次的的单辊角轧;The second step, low-temperature multi-pass single-roll angle rolling: the near-α high-temperature titanium alloy Ti-1100 ingot (φ60mm*40mm) prepared by the vacuum induction magnetic levitation melting furnace is subjected to the first step of rapid forging at 615 °C, and the deformation is 70%, and the deformation rate is 1 mm/s; the rapid forging sample is rolled at 615 °C, and the thickness of the sample is controlled at 1 mm; the length of the rolled sample is cut by wire electric discharge cutting: The samples with a width of 200 mm and a width of 20 mm are placed in a high-pressure torsion machine for multi-pass single-roll angle rolling at a low temperature of 615 ° C. The deformation of the above three steps is called one round of large plastic deformation. Since the deformation passes have an effect on the microstructure and mechanical properties of the sample, in order to avoid too many variables, three passes of single-roll angle rolling were used in this experiment;
第三步,在α+β/β相变点附近的快速热处理:将低温多道次单辊角轧后的试样在通过电火花线切割切下尺寸为60mm*15mm*1mm的试样,分别在真空电阻炉中快速加热至1030℃、1015℃、1000℃,保温2min后,快速放到水中冷却至室温。The third step, rapid heat treatment near the α+β/β transformation point: cut the sample with a size of 60mm*15mm*1mm from the sample after the low-temperature multi-pass single-roller angle rolling by EDM wire cutting, respectively in Quickly heat to 1030°C, 1015°C, and 1000°C in a vacuum resistance furnace. After holding for 2 minutes, quickly put it in water and cool it to room temperature.
最后测得不同温度快速热处理的力学性能如表2所示,其中在1015℃快速热处理得到的综合力学性能较好:抗拉强度为1197.9MPa,屈服强度为1142.5MPa,延伸率可达17.5%。α相晶粒尺寸为2.2μm。Finally, the mechanical properties measured by rapid heat treatment at different temperatures are shown in Table 2. The comprehensive mechanical properties obtained by rapid heat treatment at 1015 °C are better: the tensile strength is 1197.9MPa, the yield strength is 1142.5MPa, and the elongation can reach 17.5%. The α-phase grain size is 2.2 μm.
表2 615℃变形温度下不同热处理条件的力学性能Table 2 Mechanical properties of different heat treatment conditions at deformation temperature of 615℃
实施例3Example 3
第一步,近α高温钛合金Ti-1100(Ti–6Al–2.75Sn–4Zr–0.4Mo–0.45Si),α+β/β相变点通过金相法测得为1015℃;In the first step, near α high temperature titanium alloy Ti-1100 (Ti–6Al–2.75Sn–4Zr–0.4Mo–0.45Si), the α+β/β transformation point was measured by metallographic method to be 1015℃;
第二步,低温多道次单辊角轧:将采用真空感应磁悬浮熔炼炉制备出的近α高温钛合金Ti-1100铸锭(φ60mm*40mm)在665℃进行第一步快速锻造,变形量为70%,变形速率为1mm/s;将快速锻造后的试样在665℃进行轧制,将试样的厚度控制在1mm;使用电火花线切割在轧制后的试样上切取长度为200mm,宽度为20mm的试样,放到高压扭转机中进行665℃的低温多道次单辊角轧,上述3个工步的变形称为一轮大塑性变形。由于变形道次对试样的显微组织与力学性能均有影响,为避免变量过多,本次实验均采用3道次的的单辊角轧;The second step, low-temperature multi-pass single-roll angle rolling: the near-α high-temperature titanium alloy Ti-1100 ingot (φ60mm*40mm) prepared by the vacuum induction magnetic levitation melting furnace is subjected to the first step of rapid forging at 665 °C, and the deformation is 70%, and the deformation rate is 1 mm/s; the rapid forging sample is rolled at 665 °C, and the thickness of the sample is controlled at 1 mm; the length of the rolled sample is cut by wire electric discharge cutting: The samples with a width of 200 mm and a width of 20 mm are placed in a high-pressure torsion machine for multi-pass single-roll angle rolling at a low temperature of 665 ° C. The deformation of the above three steps is called one round of large plastic deformation. Since the deformation passes have an effect on the microstructure and mechanical properties of the sample, in order to avoid too many variables, three passes of single-roll angle rolling were used in this experiment;
第三步,在α+β/β相变点附近的快速热处理:将低温多道次单辊角轧后的试样在通过电火花线切割切下尺寸为60mm*15mm*1mm的试样,分别在真空电阻炉中快速加热至1030℃、1015℃、1000℃,保温2min后,快速放到水中冷却至室温。The third step, rapid heat treatment near the α+β/β transformation point: cut the sample with a size of 60mm*15mm*1mm from the sample after the low-temperature multi-pass single-roller angle rolling by EDM wire cutting, respectively in Quickly heat to 1030°C, 1015°C, and 1000°C in a vacuum resistance furnace. After holding for 2 minutes, quickly put it in water and cool it to room temperature.
最后测得不同温度快速热处理的力学性能如表3所示,其中在1030℃快速热处理得到的综合力学性能较好:抗拉强度为1158.4MPa,屈服强度为1121.6MPa,延伸率可达18.2%。α相晶粒尺寸为1.6μm。Finally, the mechanical properties measured by rapid heat treatment at different temperatures are shown in Table 3. The comprehensive mechanical properties obtained by rapid heat treatment at 1030 °C are better: the tensile strength is 1158.4 MPa, the yield strength is 1121.6 MPa, and the elongation can reach 18.2%. The α-phase grain size is 1.6 μm.
表3 665℃变形温度下不同热处理条件的力学性能Table 3 Mechanical properties of different heat treatment conditions at deformation temperature of 665℃
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