材料研究学报, 2022, 36(12): 919-925 DOI: 10.11901/1005.3093.2021.395

研究论文

热处理对Ti-6Mo-5V-3Al-2Fe-2Zr合金拉伸性能的影响

刘知多1, 张浩宇,1, 程军2, 周舸1, 张兴君3, 陈立佳1

1.沈阳工业大学材料科学与工程学院 沈阳 110870

2.西北有色金属研究院 陕西省医用金属材料重点实验室 西安 710016

3.辽宁北方精密设备有限公司沈阳分公司 沈阳 110020

Effect of Heat Treatment on Tensile Property of Ti-6Mo-5V-3Al-2Fe-2Zr Alloy

LIU Zhiduo1, ZHANG Haoyu,1, CHENG Jun2, ZHOU Ge1, ZHANG Xingjun3, CHEN Lijia1

1.School of Materials Science and Engineering, Shenyang University of Technology, Shenyang 110870, China

2.Northwest Institute for Non-ferrous Metal Research, Shaanxi Key Laboratory of Biomedical Metal Materials, Xi'an 710016, China

3.Liaoning North Precision Equipment Co. Ltd., Shenyang Branch, Shenyang 110020, China

通讯作者: 张浩宇,副教授,zhanghaoyu@sut.edu.cn,研究方向为高强韧钛合金成分设计及变形工艺

收稿日期: 2021-07-05   修回日期: 2021-08-28  

基金资助: 辽宁省“揭榜挂帅”科技攻关项目(2021JH1/10400069)
辽宁省教育厅青年科技人才“育苗”项目(LQGD2020012)

Corresponding authors: ZHANG Haoyu, Tel: 18624087566, E-mail:zhanghaoyu@sut.edu.cn

Received: 2021-07-05   Revised: 2021-08-28  

Fund supported: “Jie Bang Gua Shuai” Technological Tacking Project of Liaoning Province(2021JH1/10400069)
Liaoning Provincial Department of Education Youth Science and Technology Talents “Seedling” Project(LQGD2020012)

作者简介 About authors

刘知多,男,1996年生,硕士生

摘要

研究了固溶+单级时效处理、固溶+双级时效处理、固溶+随炉冷却处理对新型亚稳β钛合金Ti-6Mo-5V-3Al-2Fe-2Zr的显微组织和拉伸性能的影响。结果表明:与固溶+单级时效处理相比,固溶+双级时效处理析出的晶内次生α相间距减小和体积分数增大而使合金的强度提高。两种热处理都使合金中生成连续的晶界α相,导致合金的塑性降低;与上述两种热处理相比,固溶+随炉冷却处理使合金中析出的晶内次生α相的间距明显减小且沿晶界生成向晶内生长的αwgb相,使合金的强度和塑性显著提高,其抗拉强度达到1421 MPa,断后伸长率为7.7%;与次生α相的体积分数相比,其间距是影响合金强度的主要因素。随着次生α相间距的减小,合金的强度提高。

关键词: 金属材料; 亚稳β钛合金; 随炉冷却; 次生α; 拉伸性能

Abstract

The effect of three type of heat treatments on the microstructure and tensile properties of a novel metastable β-titanium alloy Ti-6Mo-5V-3Al-2Fe-2Zr was investigated, namely solution and single-stage aging, solution and two-stage aging, as well as solution and furnace cooling. The results show that: compared with the solution and single-stage aging treatment, the strength of the alloy was improved with the decrease of the spacing of secondary α phase precipitated within grains and the increase of its volume fraction by solution and two-stage aging treatment. Continuous α phase formed at grain boundary resulted by the above two heat treatment processes, which leading to poor plasticity of the alloy. Compared with the above two heat treatment processes, the heat treatment of solid solution and furnace cooling could induce obviously the decrease of the spacing of the intracrystalline secondary α phase precipitated, thus increase the amount of αwgb phase formed along the grain boundary and grew into the grain, thereby increase significantly the strength and plasticity of the alloy i.e., the tensile strength of the alloy reaches 1421 MPa, and the fracture elongation is 7.7%. Relative to the volume fraction of the secondary α phase, the spacing is the main factor affecting the strength of the alloy. With the decrease of the spacing of the secondary α phase, the alloy strength increases.

Keywords: metallic materials; metastable β titanium alloy; furnace cooling; secondary α phase; tensile property

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本文引用格式

刘知多, 张浩宇, 程军, 周舸, 张兴君, 陈立佳. 热处理对Ti-6Mo-5V-3Al-2Fe-2Zr合金拉伸性能的影响[J]. 材料研究学报, 2022, 36(12): 919-925 DOI:10.11901/1005.3093.2021.395

LIU Zhiduo, ZHANG Haoyu, CHENG Jun, ZHOU Ge, ZHANG Xingjun, CHEN Lijia. Effect of Heat Treatment on Tensile Property of Ti-6Mo-5V-3Al-2Fe-2Zr Alloy[J]. Chinese Journal of Materials Research, 2022, 36(12): 919-925 DOI:10.11901/1005.3093.2021.395

亚稳β钛合金有比强度高、深淬透性好和冷热成型性能优良等特点,在航空航天、海洋工程、轨道交通等领域有广阔的应用前景[1~5]。这类合金常可用于制造负载的结构件,因此对其强度和塑性等力学性能的要求很高。亚稳β钛合金的组织对热处理十分敏感,热处理对β基体内析出次生α相的形貌、尺寸、分布和体积分数有显著的影响,使其强度和塑性不同[6]。因此,热处理可在较大区间内调整这类合金的强度和塑性[7~9]

关于热处理后亚稳β钛合金的组织、强度和塑性,已经有大量的研究工作[10]。Li等[11]发现,经过850℃/1 h固溶处理和500℃/2 h单级时效处理的Ti-2Al-9.2Mo-2Fe合金强度最高,其抗拉强度为1543 MPa,达到了超高强钛合金标准。Zheng等[12]的研究发现,固溶+双级时效处理也能大幅度提高亚稳β钛合金的强度。在预时效阶段析出的ω相在二次时效阶段促进次生α相形核,进而生成更加细小弥散且分布均匀的次生α相,从而使合金的强度提高。马权等[13]对TB8合金进行固溶+双级时效处理后发现,次生α相明显细化使合金抗拉强度的提高超过了17%。Zhou等[14]则发现,与其他热处理工艺相对,固溶+随炉冷却处理也能显著提高合金的力学性能,生成枝晶状生长的α相实现了强度与塑性的良好匹配。这些结果表明,固溶+单级时效处理、固溶+双级时效处理、固溶+随炉冷却处理等不同的热处理工艺,对亚稳β钛合金析出的次生α相及强度和塑性产生不同的影响。

Ti-6Mo-5V-3Al-2Fe-2Zr (%,质量分数)合金是一种新型的亚稳β钛合金,基于Mo当量准则和d-电子成分设计方法设计,其Mo当量为12.15,Bo、Md值分别为2.7823、2.3765。作为一种新型亚稳β钛合金,热处理工艺对其组织、强度和塑性的影响尚不十分清楚。鉴于此,本文对该合金分别进行固溶+单级时效处理、固溶+双级时效处理以及固溶+随炉冷却处理,研究热处理工艺对Ti-6Mo-5V-3Al-2Fe-2Zr合金的次生α相以及强度和塑性的影响。

1 实验方法

实验用材料为亚稳β钛合金Ti-6Mo-5V-3Al-2Fe-2Zr (%,质量分数)。将高纯海绵钛、Al-Mo中间合金、Al-V中间合金、纯铁和海绵锆经过两次真空自耗熔炼,得到直径为12 mm的亚稳β钛合金Ti-6Mo-5V-3Al-2Fe-2Zr (%,质量分数)铸锭,对其在β相区锻造得到合金板材。用电火花线切割在板材上切取实验用试样。

采用公式法和金相法测定该合金的相变点。根据加入不同合金元素后合金相转变温度的变化估算合金的相变点 [15]

Tβi=882+fi(xi)

式中的882℃为纯钛的相转变温度,fi (xi )为合金中各元素对相变点的影响值。使用 式(1)计算出该合金相变点的理论值为856.24℃。在该值附近选取不同温度,用金相法测量相变点,最终确定该合金β相转变温度为855℃±5℃。

本文的研究对象为次生α相,因此选择β相转变点(870℃)以上的温度进行固溶处理,一生成单一β相组织,从而避免初生α相对实验结果的影响。根据文献[16,17],以典型的600℃/8 h时效处理作为本实验的单级时效处理制度,以典型的400℃/2 h预时效处理作为本实验双级时效的预时效处理制度。为了便于对比,以600℃作为随炉冷却的初始温度。

将切取的试样分别进行固溶+单级时效处理(HT1)、固溶+双级时效处理(HT2)和固溶+随炉冷却处理(HT3),热处理工艺在图1中给出。

图1

图1   合金的热处理工艺

Fig.1   Heat treatment process (a) solution and single-stage aging; (b) solution and two-stage aging; (c) solution and furnace cooling


是用Nordlys Nano型EBSD探测器观察和分析电解抛光后试样的晶粒尺寸和析出相 (抛光液为6%高氯酸+35%正丁醇+59%甲醇),步长为0.04 μm。使用腐蚀液(氢氟酸∶硝酸∶水=1∶3∶7)腐蚀经过金相砂纸打磨、机械抛光后的合金试样表面,用S-3400N型扫描电子显微镜观察试样的显微组织。使用WDW-100型电子万能试验机分别对三种热处理后的试样进行室温拉伸实验,以测定其拉伸性能,计算其抗拉强度、屈服强度以及断后伸长率。使用S-3400N型扫描电子显微镜观察断口形貌,分析其断裂形式。

2 实验结果

2.1 显微组织

图2给出了热处理前Ti-6Mo-5V-3Al-2Fe-2Zr合金的EBSD图像,可见其组织全部为β相。

图2

图2   热处理前合金的EBSD图像

Fig.2   EBSD image of the alloy before heat treatment


图3给出了经过不同工艺的热处理后Ti-6Mo-5V-3Al-2Fe-2Zr合金的显微组织。由图3a和3b可见,经过HT1处理后在β晶界处生成了连续的晶界α相(αgb);在β晶粒内析出了短棒状次生α相(αi)。由图3c和3d可见,经过HT2处理后在β晶界处也生成了连续的αgb相,但是在β晶粒内析出的αi相数量更多且大部分尺寸较小。其原因是,在预时效阶段生成的ω相在后续高温时效阶段促进αi相的形核从而生成了细小弥散的αi[18~21]。但是,由图3d可见,一些优先形核的αi相在后续高温时效阶段充分的生长而使部分αi相长大而粗化。由图3e和3f可见,经过HT3处理后在β晶界处生成了由αgb相形核并向晶内平行生长的αwgb相,在β晶粒内析出的αi相由短棒状变为针状,宽度明显减小且间距变窄。

图3

图3   不同热处理后合金的显微组织

Fig.3   Microstructure of the alloy after different heat treatment (a) HT1, grain boundary; (b) HT1, intragranular; (c) HT2, grain boundary; (d) HT2, intragranular; (e) HT3, grain boundary; (f) HT3, intragranular


图4给出了经过不同热处理的合金的EBSD图像。图4a、b、c的解析率分别为96.23%、96.12%和95.56%,三者的解析率较高且差异较小。用EBSD进一步分析了次生α相。结果表明,经过HT1、HT2、HT3处理后合金的β晶粒内析出的αi相尺寸逐渐减小,且在β晶界处均生成了连续的αgb相;与HT1和HT2相比,经过HT3处理后合金的晶界处生成了αwgb相,与图3中合金的显微组织相同。用EBSD统计次生α相(αs)的体积分数φ(αs)并结合图3统计αi相的平均间距λ,结果列于表1。可以看出,不同的热处理使αs相体积分数变化的趋势为,HT2>HT3>HT1;αi相平均间距的变化趋势为,HT1>HT2>HT3。

图4

图4   热处理后合金的EBSD图像

Fig.4   EBSD images of the alloy after different heat treatment (a) HT1; (b) HT2; (c) HT3


表1   热处理工艺对αs相体积分数和αi相平均间距的影响

Table 1  Effect of heat treatment on the volume fraction of αs phase and the average spacing of αi phase

Heat treatmentφ(αs)/%λ/nm
HT134.888.75
HT240.364.85
HT337.547.15

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2.2 合金的拉伸性能

合金经过不同工艺的热处理前后的屈服强度(Rp0.2)、抗拉强度(Rm)、断后伸长率(A)和强塑积(Psp),列于表2。可以看出,经过三种工艺的热处理后合金的强度都大幅度提高;与HT1处理相比,HT2热处理使合金的屈服强度和抗拉强度提高,断后伸长率由5.1%降低为4.8%,合金的塑性没有明显的变化;HT3处理后合金的屈服强度和抗拉强度进一步提高,其断后伸长率也明显提高;在三种热处理中,HT3处理后合金的强塑积最高,为10.94 GPa%,其强度与塑性匹配最佳。

表2   热处理对合金拉伸性能的影响

Table 2  Effect of heat treatment on tensile properties of the alloy

Heat treatmentRp0.2/MPaSt.devRm/MPaSt.devA/%St.devPsp/GPa%
Before HT7849891109.10.228.11
HT11099221196265.10.176.10
HT21256191352214.80.215.68
HT31324131421117.70.1310.94

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2.3 合金的断口形貌

图5给出了经过三种工艺热处理后合金的拉伸断口形貌。由图5可见,HT1处理和HT2处理后合金的拉伸断口均呈现出冰糖状特征和较浅的韧窝,其断裂方式为脆性断裂。经过HT3处理后合金的拉伸断口同时呈现出沿晶断裂特征和穿晶断裂特征,韧窝的数量更多且尺寸更大,其断裂方式开始向韧脆混合型断裂转变,表明合金具有较好的塑性。合金拉伸断口的观察结果,与表2中合金塑性的变化趋势相符。

图5

图5   不同热处理后试样的拉伸断口的形貌

Fig.5   Fracture morphology of tensile specimens after different heat treatment (a) HT1; (b) HT2; (c) HT3


3 讨论

亚稳β钛合金的拉伸性能强化机制,包括合金元素于β基体的固溶强化、β晶界强化、初生α相与β基体的界面强化和次生α相析出强化。因此,合金的屈服强度可表示为[22~24]

Rp0.2=Rν+Rss+Rgb+Rpb+Rpcpt

式中Rν为单晶摩擦应力影响项,Rss为合金元素于β基体的固溶强化影响项,Rgbβ晶界强化影响项,Rpb为初生α相与β基体的界面强化影响项,Rpcpt为次生α相析出强化影响项。对显微组织的观察结果表明,在本文的实验中未观察到初生α相,于是 式(2)改为

Rp0.2=Rν+Rss+Rgb+Rpcpt

根据 式(3)计算出次生α相析出强化影响量为

Rpcpt, exp=Rp0.2, exp(Rν+Rss+Rgb)

式中Rpcpt, exp为次生α相析出强化影响量,Rp0.2, exp为合金的屈服强度,Rν+Rss+Rgb的值则等于热处理前合金的屈服强度。由此计算出的Rpcpt, exp数值,列于表3

表3   不同热处理后合金中次生α相的析出强化影响量

Table 3  αs precipitation strength after different heat treatment

Heat

treatment

Rp0.2,exp

/MPa

Rν+Rss+Rgb

/MPa

Rpcpt,exp

/MPa

HT11099784315
HT21256784472
HT31324784540

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表3可见,经过不同工艺的热处理后生成的次生α相的体积分数、相间距等明显不同,进而影响合金强度的变化。文献[25]证实,次生α相的体积分数、相间距是热处理后亚稳β钛合金强度的主要影响因素。

图6给出了经过不同工艺的热处理后合金中次生α相体积分数φ(αs)、αi相平均间距λ与次生α相析出强化影响量Rpcpt,exp之间的关系。由图6a可见,φ(αs)与Rpcpt,exp之间的关系不是线性的,表明次生α相的体积分数并不是该合金强度变化的决定因素。由图6b可见,随着λ的增大Rpcpt,exp逐渐减小,表明αi相平均间距决定了合金强度的变化。

图6

图6   Rpcpt,expφ(αs )和λ的关系

Fig.6   Dependence of Rpcpt,exp on φ(αs ) and λ (a) the dependence of Rpcpt,exp on φ(αs ); (b) the dependence of Rpcpt,exp on λ


位错的运动很难绕过密排六方结构的αi[26~28],因此合金中的大量αi/β界面能有效地阻碍位错的滑移,使其在αi/β界面处大量堆积。因此,可用位错堆积模型解释次生α相的强化。位错堆积前端的局部应力为Nτbαi/β界面阻碍位错运动而产生的排斥力为τ*b,在平衡状态下[29]

Nτb=τ*b

式中τ为位错运动施加的应力;τ*为αi界面产生的应力场,其值与位错源的位置以及界面能量有关,b为伯格斯矢量。

同时,堆积位错的数量可表示为[30]

N=π(1-v)τλ/2Gb

式中v为泊松比;G为剪切模量。设位错源位于两个αi相之间,λ/2为位错的运动距离,则根据 式(5)和 式(6)可得位错滑移穿过αi/β界面的临界应力

τc=2Gbτ*π(1-v)τλ=k0/λ

式中k0为材料常数。 式(7)表明,τcλ-1/2呈线性关系。

图7给出了不同工艺热处理后合金的屈服强度与λ-1/2的关系。可以看出,整体呈现出近似线性相关的关系,与 式(7)给出的结论相符,即随着αi相平均间距的减小合金的强度提高。

图7

图7   Rp0.2λ-1/2的关系

Fig.7   Dependence of Rp0.2 on λ-1/2 after heat treatment


经过HT1和HT2处理的合金,其塑性均较差。其原因是,与被αi相强化的β基体相比,在β晶界处生成的连续αgb相弱化了晶界,使裂纹易于在αgb/β界面处萌生并沿其扩展,对合金的塑性产生了严重的不良影响[31~33]。这也与合金拉伸断口的沿晶断裂特征相符。但是,经过HT3处理后,在合金的β晶界处生成了由αgb相形核并向晶内扩展的αwgb相,不仅为沿晶裂纹扩展提供了更多的路径,而且消耗了沿晶裂纹的能量,减缓了其扩展速率,从而改善了合金塑性。这也与对合金拉伸断口的观察结果相符。

4 结论

(1) 在三种工艺热处理的Ti-6Mo-5V-3Al-2Fe-2Zr合金的晶内析出了αi相,在晶界生成了连续的αgb相;与固溶+单级时效处理与固溶+双级时效处理相比,固溶+随炉冷却处理析出的αi相间距最小,且在晶界处生成了向晶内平行生长的αwgb相。

(2) 与固溶+单级时效处理及固溶+双级时效处理相比,固溶+随炉冷却处理的Ti-6Mo-5V-3Al-2Fe-2Zr合金强度和塑性匹配最佳,其抗拉强度为1421 MPa,屈服强度为1324 MPa,断后伸长率为7.7%。

(3) 经不同工艺的热处理后Ti-6Mo-5V-3Al-2Fe-2Zr合金晶内析出的αi相间距是影响其强度的主要因素,随着αi相间距的减小合金的强度提高;αwgb相的生成,使合金的塑性显著改善。

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