CN115178598A - Hot processing method for improving high-temperature tensile strength of titanium alloy rolled bar - Google Patents
Hot processing method for improving high-temperature tensile strength of titanium alloy rolled bar Download PDFInfo
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Abstract
本发明提供了一种提高钛合金轧棒高温拉伸强度的热加工方法,将经开坯和中间坯锻造获得的棒材在β单相区加热变形获得终轧棒坯,加热温度设定为相变点以上30~50 oC,保温时间按1min/mm计算,然后径锻或轧制成型,变形量为40%~70%,变形后空冷;然后将获得的棒坯经修磨去除表面缺陷后在α+β两相区低温段加热轧制,将终轧棒坯加热温度设定为相变点以下60~100 oC,保温时间按1min/mm计算,然后轧制成型,轧制变形量为60%~90%,变形后空冷。通过本发明的方法可获得具有均匀、细小的α相的轧态组织,含该组织的轧棒经常规热处理后,室温和600℃高温拉伸强度明显提高且数值稳定。
The invention provides a hot working method for improving the high temperature tensile strength of a titanium alloy rolled bar. The final rolled bar is obtained by heating and deforming a bar obtained by forging a billet and an intermediate billet in a β single-phase region, and the heating temperature is set as The temperature is 30~50 o C above the transformation point, the holding time is calculated as 1min/mm, and then the diameter is forged or rolled, the deformation amount is 40%~70%, and the deformation is air-cooled; then the obtained bar is ground to remove the surface After the defect, it is heated and rolled in the low temperature section of the α+β two-phase region. The heating temperature of the final rolled billet is set to 60~100 o C below the transformation point, and the holding time is calculated as 1min/mm. The deformation amount is 60%~90%, and it is air-cooled after deformation. Through the method of the present invention, a rolled structure with uniform and fine α phase can be obtained. After conventional heat treatment, the tensile strength at room temperature and high temperature of 600°C of the rolled bar containing the structure is obviously improved and the value is stable.
Description
技术领域:Technical field:
本发明属于冶金领域,涉及一种钛合金棒材的热加工技术领域,具体来说是一种提高钛合金轧棒高温拉伸强度的热加工方法。The invention belongs to the field of metallurgy and relates to the technical field of hot processing of titanium alloy rods, in particular to a hot processing method for improving the high temperature tensile strength of titanium alloy rolled rods.
背景技术:Background technique:
钛合金因具有较高的比强度、优异的耐腐蚀性能,在航空航天等领域获得广泛的应用。其中近α型合金具有良好的高温强度和组织稳定性,作为500℃以上使用的高温钛合金。Titanium alloys are widely used in aerospace and other fields because of their high specific strength and excellent corrosion resistance. Among them, the near-α type alloy has good high temperature strength and microstructure stability, and is used as a high temperature titanium alloy above 500 ℃.
高温钛合金小规格棒材传统热加工工艺是α+β两相区锻造或轧制变形制备中间坯,而后在α+β两相区(相变点以下30-50℃)成材,工艺路线见图1。但是,大量的实践结果表明,传统工艺获得棒材初生α相尺寸分布不均匀,在局部位置存在大块α。在材料受到拉伸过程中裂纹易在大块α与基体的界面处萌生,降低了材料的拉伸强度和增加了拉伸性能的分散性,尤其是高温拉伸强度。因此,减小两相区轧制后α相尺寸和提高其尺寸均匀性是近α型高温钛合金轧制棒材需要解决的技术瓶颈。The traditional hot working process of high-temperature titanium alloy small-sized bars is to forge or roll deformation in the α+β two-phase region to prepare the intermediate billet, and then form the bar in the α+β two-phase region (30-50 °C below the transformation point). See the process route. figure 1. However, a large number of practical results show that the size distribution of the primary α phase in the bar obtained by the traditional process is not uniform, and there are large α in the local position. During the tensile process of the material, cracks are easily initiated at the interface between the bulk α and the matrix, which reduces the tensile strength of the material and increases the dispersion of tensile properties, especially the high-temperature tensile strength. Therefore, reducing the size of the α phase after rolling in the two-phase region and improving its size uniformity are the technical bottlenecks that need to be solved in the rolling of near-α type high-temperature titanium alloy bars.
发明内容:Invention content:
针对现有技术中的上述技术问题,本发明提供了一种提高钛合金轧棒高温拉伸强度的热加工方法,所述的这种一种提高钛合金轧棒高温拉伸强度的热加工方法要解决现有技术中的工艺获得棒材降低了材料的拉伸强度、增加了拉伸性能的分散性,尤其是高温拉伸强度的技术问题。In view of the above-mentioned technical problems in the prior art, the present invention provides a hot working method for improving the high temperature tensile strength of a titanium alloy rolled bar, and the described hot working method for increasing the high temperature tensile strength of a titanium alloy rolled bar To solve the technical problem of reducing the tensile strength of the material and increasing the dispersion of the tensile properties, especially the high temperature tensile strength, obtained by the process in the prior art.
本发明提供了一种提高钛合金轧棒高温拉伸强度的热加工方法,包括如下步骤:The invention provides a hot working method for improving the high temperature tensile strength of a titanium alloy rolled bar, comprising the following steps:
1)将经开坯和中间坯锻造获得的棒材在β单相区加热变形获得终轧棒坯,在β单相区加热变形获得终轧棒坯的过程中,加热温度设定为相变点以上30~50℃,保温时间按1min/mm计算,然后径锻或轧制成型,变形量为40%~70%,变形后空冷;1) The final rolled billet is obtained by heating and deforming the bar obtained by the billet and intermediate billet forging in the β single-phase region. During the process of heating and deforming the final rolled billet in the β single-phase region, the heating temperature is set to phase transformation. The temperature is 30~50℃ above the point, the holding time is calculated as 1min/mm, and then forging or rolling is formed, the deformation is 40%~70%, and the air cooling after deformation;
2)将步骤1)获得的棒坯经修磨去除表面缺陷后在α+β两相区低温段加热轧制,在α+β两相区低温段加热轧制的过程中,将终轧棒坯加热温度设定为相变点以下60~100℃,保温时间按1min/mm计算,然后轧制成型,轧制变形量为60%~90%,变形后空冷。2) After grinding the bar obtained in step 1) to remove surface defects, it is heated and rolled in the low temperature section of the α+β two-phase region. During the process of heating and rolling in the low temperature section of the α+β two-phase region, the final rolled bar is The heating temperature of the billet is set to be 60-100°C below the transformation point, the holding time is calculated as 1min/mm, and then rolled into a shape with a rolling deformation of 60% to 90%, and air-cooled after deformation.
钛合金棒材的制备流程一般为:铸锭熔炼、开坯、中间坯锻造、径锻/轧制、终轧、热处理,本发明主要针对钛合金终轧棒坯制备工艺及终轧工艺。The preparation process of titanium alloy bar is generally: ingot smelting, billet opening, intermediate billet forging, radial forging/rolling, final rolling, heat treatment.
通过本发明的方法制备后,钛合金轧棒轧态中α相以均匀的、细小的等轴状或蠕虫状存在,尺寸1-3um,不存在大块α。经双重退火热处理后,组织为双态组织,初生α分布均匀,尺寸5-8um,不存在大块α。通过本发明的方法制备后具有该组织的材料的室温拉伸和600℃高温拉伸强度明显提高,且数值稳定。After being prepared by the method of the present invention, the α phase in the rolling state of the titanium alloy rolled bar exists in a uniform and fine equiaxed or worm-like shape, the size is 1-3um, and there is no large α phase. After double annealing and heat treatment, the microstructure is a two-state structure, the primary α distribution is uniform, the size is 5-8um, and there is no large α. After being prepared by the method of the present invention, the room temperature tensile strength and the high temperature tensile strength of 600° C. of the material having the structure are obviously improved, and the numerical value is stable.
本发明中优化高温型钛合金α晶粒尺寸和均匀性的工艺设计原理如下:The process design principle for optimizing the grain size and uniformity of high temperature titanium alloy α in the present invention is as follows:
(1)在传统“α+β两相区制坯”+“α+β两相区轧制”工艺中,坯料为典型的α+β双态组织,含初生α相和β转变组织;在随后的α+β相区(相变点以下30-50℃)加热中,初生α晶粒长大,β转变组织中α片层也发生粗化,轧制过程中,初生α相和β转变组织中α片层都开始发生破碎,但破碎的程度不同。厚度较小的α片层易发生破碎,但粗大的初生α相破碎效果有限,尤其是坯料中存在的大块α。变形的不均匀导致终轧棒材组织不均匀,进而影响拉伸强度。(1) In the traditional "α+β two-phase region billet making" + "α+β two-phase region rolling" process, the billet is a typical α+β two-state structure, including primary α phase and β transformation structure; During the subsequent heating in the α+β phase region (30-50°C below the transformation point), the primary α grains grow, and the α sheet in the β transformation structure also coarsens. During the rolling process, the primary α phase and β transformation The α-sheets in the tissues all began to break up, but the degree of break-up was different. The α lamellae with smaller thickness are prone to crushing, but the crushing effect of the coarse primary α phase is limited, especially the large pieces of α existing in the billet. The non-uniform deformation leads to the non-uniform structure of the final rolled bar, which in turn affects the tensile strength.
(2)在本发明提出的“β相区制坯”+“α+β两相区轧制”工艺中,充分利用了前后热加工环节的耦合作用和组织演变。坯料在β区加热和变形制备中间坯,通过控制加热温度和变形量,可以形成片层厚度均匀的魏氏组织。β加热温度不易太高,时间不易太长,且要有一定的变形量,否则β晶粒长大且变形后空冷过程易形成平直、连续的晶界α相量,不利于后续破碎。研究和实践表明,β区加热温度选择相变点以上30~50℃,保温时间按1min/mm计算,变形量为40%~70%,获得的魏氏组织片层均匀,不存在平直、连续的晶界α。在随后的α+β相区加热中,片层出现了一定的长大,通过控制加热温度和时间,可以避免过渡长大。这种均匀的片层在变形过程中,不同位置处片层α相均匀破碎,可形成均匀的、细小的等轴状或蠕虫状α,整个观察范围不存在大块α。研究和实践表明,α+β两相区轧制加热温度选择相变点以下60~100℃,保温时间按1min/mm计算,轧制变形量为60%~90%,获得的组织中α片层充分破碎。两相区加热温度太低,轧制开裂;太高α相回溶,参与变形破碎片层α相有限。变形量太小α片层不能破碎,太大则存在温升过大风险。(2) In the "β-phase region billet making" + "α+β two-phase region rolling" process proposed by the present invention, the coupling effect and microstructure evolution of the front and rear hot working links are fully utilized. The billet is heated and deformed in the beta zone to prepare the intermediate billet. By controlling the heating temperature and the amount of deformation, a Widmandelstein microstructure with uniform lamella thickness can be formed. The β heating temperature is not easy to be too high, the time is not too long, and there must be a certain amount of deformation, otherwise the β grains grow and the air cooling process after deformation is easy to form a straight and continuous grain boundary α phase, which is not conducive to subsequent crushing. Research and practice show that the heating temperature in the beta zone is 30-50°C above the phase transition point, the holding time is calculated as 1min/mm, and the deformation is 40%-70%. Continuous grain boundary α. During the subsequent heating in the α+β phase region, the lamellae grow to a certain extent, and the excessive growth can be avoided by controlling the heating temperature and time. During the deformation process of this uniform lamella, the α phase of the lamella is uniformly broken at different positions, and can form a uniform and fine equiaxed or worm-like α, and there is no large α in the entire observation range. Research and practice show that the rolling heating temperature in the α+β two-phase region is 60-100°C below the transformation point, the holding time is calculated as 1min/mm, and the rolling deformation is 60%-90%. The layers are sufficiently broken. If the heating temperature in the two-phase region is too low, the rolling cracks; if the α phase is too high, the α phase will dissolve back, and the α phase participating in the deformation and crushing of the lamellae is limited. If the deformation is too small, the α sheet cannot be broken, and if it is too large, there is a risk of excessive temperature rise.
在后续的双重退火热处理时,部分α发生粗化形成初生α,其它部分形成β转变组织。由于不存在大块α,且初生α尺寸、分布均匀,因此材料的室温拉伸强度和高温拉伸强度出现了明显的提升,且多次测量结果波动不大。During the subsequent double annealing heat treatment, part of α is coarsened to form primary α, and other parts form β-transformed structure. Due to the absence of bulk α and the uniform size and distribution of primary α, the room temperature tensile strength and high temperature tensile strength of the material have been significantly improved, and the results of multiple measurements have little fluctuation.
本发明和已有技术相比,其技术进步是显著的。采用本发明提出的“β相区制坯”+“α+β两相区轧制”工艺技术制备的高温钛合金轧棒,轧态中α相以均匀、细小的等轴状或蠕虫状存在,尺寸1-3um,不存在大块α。经双重退火热处理后,组织为双态组织,初生α尺寸5-8um,不存在大块α。具有该组织的材料的室温拉伸和600℃高温拉伸强度高,且数值稳定。本发明的方法通过优化α相尺寸和均匀性,进而提高其强度并减少强度的分散性,尤其是高温拉伸强度。Compared with the prior art, the present invention has significant technical progress. For the high-temperature titanium alloy rolled bar prepared by the process technology of "β-phase region billeting" + "α+β two-phase region rolling" proposed by the present invention, the α-phase exists in a uniform and fine equiaxed or vermicular shape in the rolling state , the size is 1-3um, and there is no large block α. After double annealing and heat treatment, the microstructure is a two-state microstructure, the primary α size is 5-8um, and there is no bulk α. The material with this structure has high tensile strength at room temperature and high temperature at 600°C, and is numerically stable. The method of the present invention improves the strength and reduces the dispersion of the strength, especially the high temperature tensile strength, by optimizing the size and uniformity of the alpha phase.
附图说明:Description of drawings:
图1为传统“α+β两相区制坯”+“α+β两相区轧制”工艺路线示意图。Figure 1 is a schematic diagram of the traditional "α+β two-phase region billet making" + "α+β two-phase region rolling" process route.
图2为本发明提出的“β相区制坯”+“α+β两相区轧制”工艺路线示意图。Fig. 2 is a schematic diagram of the process route of "β-phase region billet making" + "α+β two-phase region rolling" proposed by the present invention.
图3为对比例中利用传统工艺路线下获得的显微组织形貌。Figure 3 shows the microstructure morphology obtained under the traditional process route in the comparative example.
图4为实施例1中利用本发明提出的制备工艺获得的显微组织形貌。FIG. 4 is the microstructure morphology obtained by using the preparation process proposed by the present invention in Example 1. FIG.
图5为实施例2中利用本发明提出的制备工艺获得的显微组织形貌。FIG. 5 is the microstructure morphology obtained by using the preparation process proposed by the present invention in Example 2. FIG.
具体实施方式:Detailed ways:
对比例和实施例中高温钛合金为Ti-Αl-Sn-Zr-Mo-Nb系,含少量的Si和Ce。对其它近α高温钛合金,本发明提出的制备工艺也可达到同样的效果。The high-temperature titanium alloys in the comparative examples and examples are Ti-Al-Sn-Zr-Mo-Nb systems, containing a small amount of Si and Ce. For other near-α high temperature titanium alloys, the preparation process proposed by the present invention can also achieve the same effect.
对比例:Comparative ratio:
采用三次真空自耗熔炼得到φ760mm铸锭,相变点1020℃。采用快锻机将铸锭开坯成φ220mm,锻造温度1050~1150℃;然后锻造成φ80mm棒材,锻造温度950~970℃。棒材经修磨后装入电炉,温度990℃,保温80分钟,然后径锻成坯料,变形量60%。坯料经修磨去除表面缺陷后装入电炉,温度980℃,保温40分钟,轧制成棒材,变形量75%。轧棒经双重退火,具体为960℃/1h,空冷+570℃/2h,空冷。The φ760mm ingot was obtained by three vacuum consumable smelting, and the phase transition point was 1020°C. Use a quick forging machine to open the ingot to φ220mm, the forging temperature is 1050~1150℃; then it is forged into a φ80mm bar, the forging temperature is 950~970℃. After grinding, the bar is loaded into an electric furnace, the temperature is 990 ° C, and the temperature is kept for 80 minutes, and then it is forged into a billet with a deformation amount of 60%. After the billet is ground to remove surface defects, it is loaded into an electric furnace, the temperature is 980 ° C, the heat preservation is 40 minutes, and it is rolled into a bar with a deformation amount of 75%. The rolled bar is double annealed, specifically 960°C/1h, air-cooled +570°C/2h, air-cooled.
图3为对比例中利用传统两相区轧制工艺路线下获得的显微组织形貌。可见,终轧前坯料内初生α相粗大,尺寸10-20um,局部位置初生α相相连,形成大块α。经终轧后,初生α相破碎程度不同,一些成为细小的等轴状,尺寸2-10um;一些形成尺寸略有减小,尺寸8-15um;还有一些原有的大块α没有充分破碎,遗传下来。在后续的双重退火热处理时,细小的等轴α回溶消失,大块α依然存在。表1给出了轧棒的室温和600℃高温拉伸性能,由于轧制后α相尺寸分布不均且存在大块α,导致轧棒高温性能存在明显的波动,且大部分数值不满足相关的材料规范(屈服强度要求≥550MPa,抗拉强度要求≥650MPa)。Figure 3 shows the microstructure obtained under the traditional two-phase rolling process route in the comparative example. It can be seen that the primary α phase in the billet before the final rolling is coarse, the size is 10-20um, and the primary α phase is connected at local positions to form a large block of α. After the final rolling, the primary α phase is broken to different degrees, some become small equiaxed, with a size of 2-10um; some are slightly reduced in size, with a size of 8-15um; and some original large pieces of α are not sufficiently broken. , inherited. During the subsequent double annealing heat treatment, the small equiaxed α re-dissolved and disappeared, and the large α remained. Table 1 shows the tensile properties of the rolled bars at room temperature and 600 °C. Due to the uneven size distribution of the α phase and the existence of large α blocks after rolling, the high temperature properties of the rolled bars have obvious fluctuations, and most of the values do not meet the relevant requirements. The material specification (yield strength requirement ≥ 550MPa, tensile strength requirement ≥ 650MPa).
实施例1:Example 1:
采用对比例中开坯+锻造后φ80mm棒材。棒材经修磨后装入电炉,温度1070℃,保温80分钟,然后径锻成坯料,变形量60%。轧制坯料经修磨去除表面缺陷后装入电炉,温度920℃,保温40分钟,轧制成棒材,变形量70%。The φ80mm bar after billeting + forging in the comparative example is used. After grinding, the bar is put into an electric furnace, the temperature is 1070 ° C, and the temperature is kept for 80 minutes, and then it is forged into a billet with a deformation amount of 60%. The rolled billet was ground to remove surface defects and then loaded into an electric furnace at a temperature of 920° C., kept for 40 minutes, and rolled into a bar with a deformation of 70%.
图4为实施例1中利用本发明提出的制备工艺获得的棒材的显微组织形貌。可见,终轧前棒坯为网篮组织,α片层厚度均匀,尺寸为1-3um。终轧后片层α相充分破碎,形成均匀的、细小的等轴状或蠕虫状α,短边尺寸1-3um,整个观察范围不存在大块α。经双重退火热处理后,部分α发生粗化形成初生α,尺寸5-8um,其他部分回溶后再析出形成β转变组织。由于不存在大块α,且初生α尺寸均匀,因此材料的室温和600℃高温拉伸强度出现了明显的提升,详见表1。FIG. 4 is the microstructure morphology of the bar obtained by using the preparation process proposed by the present invention in Example 1. FIG. It can be seen that the billet before the final rolling is a basket structure, the thickness of the α lamella is uniform, and the size is 1-3um. After the final rolling, the α-phase of the lamella is sufficiently broken to form a uniform and fine equiaxed or worm-like α with a short side size of 1-3um, and there is no large α in the entire observation range. After double annealing and heat treatment, part of α is coarsened to form primary α, with a size of 5-8um, and other parts are redissolved and then precipitated to form a β-transformed structure. Due to the absence of bulk α and the uniform size of the primary α, the tensile strength of the material at room temperature and high temperature at 600 °C is significantly improved, as shown in Table 1.
实施例2:Example 2:
采用对比例中开坯+锻造后φ80mm棒材。棒材经修磨后装入电炉,温度1070℃,保温80分钟,然后轧制成坯料,变形量60%。轧制坯料经修磨去除表面缺陷后装入电炉,温度920℃,保温40分钟,轧制成棒材,变形量70%。与实施例1相比,实施例2采用轧制工艺制备轧制坯料,而实施例1采用径锻工艺制备轧制坯料。The φ80mm bar after billeting + forging in the comparative example is used. After grinding, the bar is loaded into an electric furnace, the temperature is 1070 ° C, and the temperature is kept for 80 minutes, and then it is rolled into a billet with a deformation amount of 60%. The rolled billet was ground to remove surface defects and then loaded into an electric furnace at a temperature of 920° C., kept for 40 minutes, and rolled into a bar with a deformation of 70%. Compared with Example 1, Example 2 adopts a rolling process to prepare rolled billets, while Example 1 adopts a radial forging process to prepare rolled billets.
图5为实施例2中利用本发明提出的制备工艺获得的棒材的显微组织形貌。可见,由于轧坯棒材变形过程也在相变点以上,且变形量和终轧温度、终轧变形量与实施例1相同,因此获得的轧坯棒材组织、终轧棒材轧态组织及终轧棒材热处理态组织与实施例1相近。相比于对比例,材料的室温和600℃高温拉伸强度出现了明显的提升,详见表1。FIG. 5 is the microstructure morphology of the bar obtained by the preparation process proposed by the present invention in Example 2. FIG. It can be seen that since the deformation process of the rolled bar is also above the phase transition point, and the deformation amount, the final rolling temperature, and the final rolling deformation are the same as those in Example 1, the obtained rolled bar structure and the final rolled bar structure as-rolled And the heat-treated structure of the final-rolled bar is similar to that of Example 1. Compared with the comparative example, the tensile strength of the material at room temperature and high temperature at 600 °C has been significantly improved, as shown in Table 1.
实施例3:Example 3:
采用对比例中开坯+锻造后φ80mm棒材。棒材经修磨后装入电炉,温度1050℃,保温80分钟,然后径锻成坯料,变形量50%。轧制坯料经修磨去除表面缺陷后装入电炉,温度960℃,保温40分钟,轧制成棒材,变形量85%。相比于对比例,材料的室温和600℃高温拉伸强度出现了明显的提升,详见表1。The φ80mm bar after billeting + forging in the comparative example is used. After grinding, the bar is loaded into an electric furnace, the temperature is 1050 ℃, and the temperature is kept for 80 minutes, and then it is forged into a billet with a deformation amount of 50%. The rolled billet was ground to remove surface defects and then loaded into an electric furnace at a temperature of 960° C., kept for 40 minutes, and rolled into a bar with a deformation amount of 85%. Compared with the comparative example, the tensile strength of the material at room temperature and high temperature at 600 °C has been significantly improved, as shown in Table 1.
实施例4:Example 4:
采用对比例中开坯+锻造后φ80mm棒材。棒材经修磨后装入电炉,温度1070℃,保温80分钟,然后轧制成坯料,变形量65%。轧制坯料经修磨去除表面缺陷后装入电炉,温度940℃,保温40分钟,轧制成棒材,变形量65%。相比于对比例,材料的室温和600℃高温拉伸强度出现了明显的提升,详见表1。The φ80mm bar after billeting + forging in the comparative example is used. After grinding, the bar is loaded into an electric furnace, the temperature is 1070 ° C, the temperature is kept for 80 minutes, and then it is rolled into a billet with a deformation amount of 65%. The rolled billet was ground to remove surface defects and then loaded into an electric furnace at a temperature of 940° C., kept for 40 minutes, and rolled into a bar with a deformation of 65%. Compared with the comparative example, the tensile strength of the material at room temperature and high temperature at 600 °C has been significantly improved, as shown in Table 1.
表1实施例、对比例力学性能Table 1 Example, Comparative Example Mechanical Properties
本技术领域中的普通技术人员应当认识到,以上的实施例仅是用来说明本发明,而并非作为对本发明的限定,只要在本发明的实质精神范围内,对以上所述实施例的变化、变型都将落在本发明的权利要求书范围内。Those of ordinary skill in the art should realize that the above embodiments are only used to illustrate the present invention, but not to limit the present invention, as long as the changes to the above embodiments are within the spirit and scope of the present invention , modifications will fall within the scope of the claims of the present invention.
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