稀土Ce掺杂对循环载荷下Ti-22Nb合金力学性能的影响

冀卫国; 孟晓凯; 朱金才; 邓厚伟

doi:10.12404/j.issn.1671-1815.2507703

科学技术与工程 ›› 2026, Vol. 26 ›› Issue (28) :12137-12143 DOI: 10.12404/j.issn.1671-1815.2507703

矿冶工程

稀土Ce掺杂对循环载荷下Ti-22Nb合金力学性能的影响

冀卫国 ¹ ,
孟晓凯 ¹^,^* ,
朱金才 ²^,³ ,
邓厚伟 ¹

作者信息 +

Effect of Rare Earth Ce Doping on Mechanical Properties of Ti-22Nb Alloys under Cyclic Loading

JI Wei-guo ¹ ,
MENG Xiao-kai ¹^,^* ,
ZHU Jin-cai ²^,³ ,
DENG Hou-wei ¹

Author information +

文章历史 +

摘要

为明确稀土元素Ce作为合金化元素对Ti-Nb二元合金力学性能的影响规律,采用真空电弧熔炼技术制备了不同成分的Ti-22Nb-xCe[x=0, 0.06, 0.1, 0.5(原子分数/%)]合金,系统研究了稀土Ce掺杂对循环载荷下Ti-22Nb合金力学性能的影响。结果表明,所有合金的滞回曲线均呈现先下移后稳定的滞后稳定化现象。稀土Ce可以显著提高Ti-22Nb合金的循环稳定性,适量Ce掺杂可以有效调控合金的弹性模量、弹性变形能以及等效阻尼比,其中Ti-22Nb-0.1Ce合金具有最大的弹性模量、最大的弹性变形能以及较小的等效阻尼比。另外,稀土Ce掺杂与循环加载均显著提高Ti-Nb-Ce合金的显微硬度。

Abstract

To clarify the effect of rare earth element Ce as alloying element on the mechanical properties of Ti-Nb binary alloy, Ti-22Nb-xCe[x=0, 0.06, 0.1, 0.5(atomic fraction/%)]alloys with different Ce content were fabricated by vacuum arc melting technology. The effect of rare earth Ce doping on mechanical properties of Ti-22Nb alloys under cyclic loading was systematically studied. The results show that the hysteresis curves of all alloys first move down and then become stable. Rare earth Ce can significantly improve the cyclic stability of Ti-22Nb alloys. Appropriate amount of Ce doping can effectively control the elastic modulus, elastic deformation energy and equivalent damping ratio of the alloys. Among them, Ti-22Nb-0.1Ce alloy has the largest elastic modulus, the largest elastic deformation property and a smaller equivalent damping ratio. In addition, rare earth Ce doping and cyclic loading significantly improve the microhardness of Ti-Nb-Ce alloys.

Graphical abstract

关键词

Ti-Nb基合金 / 稀土元素Ce / 循环加载 / 弹性模量 / 显微硬度

Key words

Ti-Nb-based alloys / rare earth element Ce / cyclic loading / elastic modulus / microhardness

引用本文

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冀卫国, 孟晓凯, 朱金才, 邓厚伟. 稀土Ce掺杂对循环载荷下Ti-22Nb合金力学性能的影响[J]. 科学技术与工程, 2026, 26(28): 12137-12143 DOI:10.12404/j.issn.1671-1815.2507703

JI Wei-guo, MENG Xiao-kai, ZHU Jin-cai, DENG Hou-wei. Effect of Rare Earth Ce Doping on Mechanical Properties of Ti-22Nb Alloys under Cyclic Loading[J]. Science Technology and Engineering, 2026, 26(28): 12137-12143 DOI:10.12404/j.issn.1671-1815.2507703

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钛合金作为20世纪重要的结构材料之一,凭借其高比强度、优异的耐腐蚀性和良好的高温性能,成为现代航空航天领域不可或缺的关键材料^[1-4]。尤其在航空发动机中,钛合金被广泛应用于压气机叶片和盘件等核心部件,这些部件需承受数万次“起飞-巡航-降落”循环带来的复杂载荷,对其服役性能提出较高要求^[5-9]。为克服传统钛合金性能上的局限,满足新一代航空航天装备的发展需求,近年来添加β稳定元素Nb的Ti-Nb合金受到广泛关注,在服役性能和损伤容限方面展现出显著优势^[10]。

当Nb原子分数为16%~44%时,Ti-Nb合金在冷却过程中发生非扩散型β→α″热弹性马氏体相变,表现出形状记忆效应,然而,固溶态Ti-Nb合金在5%拉伸应变下的最大可恢复应变仅为3%^[11-15]。Wang等^[16]研究发现,Ti-16Nb(原子分数/%)合金在2%预应变范围内可以实现完全形状恢复,且在3.26%预应变下经20次循环后仍保持40%以上的恢复率,其屈服强度、抗拉强度和延展率分别为461 MPa、613 MPa和19.2%。Guedes等^[17]研究发现,随着Nb含量增加,Ti-Nb合金的弹性模量由68.63 GPa(Ti-23Nb)降至38.85 GPa(Ti-27Nb),其中Ti-25Nb合金在25次循环加载后仍保持最高的可恢复应变(1.58%)。Kim等^[11]研究表明,Ti-26Nb 合金经573 K/1 h时效后具有良好的循环稳定性。Guo等^[18]采用原位同步辐射X射线衍射揭示了Ti-36Nb合金高达2.2%的线性可恢复应变源于低杨氏模量与宽应力范围内β-α″应力诱发马氏体相变的协同作用。Pillmeier等^[19]研究了严重塑性变形对β型Ti-45Nb合金裂纹扩展行为的影响,发现经高压扭转处理后,合金硬度提高约60%,达到(270±4) HV(HV为维氏硬度)。

为突破传统Ti-Nb合金的性能局限,通过Mo、Al、In、Ga、Zr和Sn等合金化元素设计可以改善其综合力学性能。通过调控Nb/Mo含量与热处理工艺,Ti-27Nb、Ti-24Nb-1Mo、Ti-21Nb-2Mo和Ti-18Nb-3Mo合金经973 K热处理后表现出优异的超弹性,随着Mo含量增加超弹性应变最高达2.6%^[20],并发现Ti-20Nb-5Mo显微硬度为400 HV^[21]。Al添加可以显著细化Ti-Nb-Al合金的β相晶粒并减小晶格常数,当Al原子分数为3%时,在6%的拉伸应变下实现了4.7%的应变恢复,恢复率达78%^[22]。Pilz等^[23]研究发现,亚稳β型Ti-40Nb-3.5In与 Ti-36Nb-3.5In 兼具低杨氏模量(58 GPa)与较高抗拉强度(553 MPa)。Alberta等^[24]研究表明,当Ga的质量分数为8%时,Ti-Nb-Ga合金的显微硬度为 232 HV,高于未添加的Ti-45Nb合金(147 HV)。研究表明,Zr添加使Ti-Nb-Zr合金表现出超过 600 MPa 的高周疲劳极限,显著优于传统α-β型钛合金,且Zr元素可以改善Ti-Nb-Zr合金在拉伸变形过程中的超弹性特性^[25-26]。Azevedo等^[27-28]研究发现,Ti-42Nb-2.5Sn合金经冷轧和时效处理后断裂韧性为25 MPa·m^1/2,显著高于Ti-35Nb合金。

铈(Ce)作为典型的稀土元素,对镁基、铝基及镍基合金具有显著的强韧化作用。Gao等^[29]研究表明,当Ce的质量分数为0.6%时,镁合金的屈服强度、抗拉强度和伸长率分别达到281 MPa、295 MPa 和27.9%。Cengiz等^[30]研究发现,在Al-Si合金中添加质量分数为2%的Ce,其极限抗拉强度提高25%~30%,并有效改善了Al-12Si合金的延展性。Chen等^[31]研究发现,掺入原子分数为0.15%Ce的Ni-Mn-Ga-B合金经601次循环加载-卸载后仍保持优异的超弹性稳定性。当前,关于Ce元素对Ti-Nb合金力学性能影响的研究尚鲜见报道。为此,研究稀土Ce掺杂Ti-22Nb合金的循环加载特性,通过拉伸循环加载与显微硬度测试,分析Ce微合金化对合金模量、能量耗散特性及硬度的影响规律。研究成果可为Ti-Nb基合金的成分优化及循环服役性能提升提供理论依据,同时对拓展其在航天工程领域的应用具有重要价值。

1 实验材料与方法

以纯度均为99.99%的钛、铌和铈颗粒为原料,按照名义成分Ti-22Nb-xCe[x =0, 0.06, 0.1, 0.5(原子分数/%)]进行配比。所有原料经无水乙醇清洗后,置于水冷铜坩埚中,在高纯氩气保护气氛下,采用WS-4型非自耗真空电弧熔炼炉进行熔炼。为促进合金成分均匀化,熔炼过程使用磁搅拌对熔融金属液体进行搅拌,搅拌电流5 A,并将铸锭反复熔炼6次,每次熔炼后将铸锭翻转180°,熔炼时长 5 min,最后浇铸至铜模冷却成型,铸锭质量约为 36 g。使用DK7740型电火花线切割机将铸锭加工成所需尺寸试样,并通过机械研磨去除表面氧化层与变形层。采用MP-1型抛光机在2 000 r/min转速下使用Al₂O₃悬浮液(W1.0)进行粗抛,然后使用UNIPOL-802型自动抛光机在250 r/min转速下使用SiO₂悬浮液(80 nm)进行精抛,获得无痕且光滑的镜面试样。

采用MTS Tytron 651型疲劳实验机对Ti-Nb-Ce合金试样进行室温循环加卸载实验,试样尺寸如图1所示。实验在应力控制模式下进行,应变速率设定为0.002 s^-1,应变幅值为2.5%,每个试样进行50次循环,以10 Hz频率进行数据采集,并实时记录应力-应变滞回曲线。采用AHVD-1000XY型显微维氏硬度计对循环加载前后合金试样进行显微硬度测试。实验设定载荷为1.96 N,保载时间10 s。每个样品均选取10个不同区域进行测试,去掉最大值和最小值后取平均值作为最终硬度值,并计算标准差,以确保数据的可靠性与一致性。

2 计算原理

基于循环加载数据,以动应力为纵坐标,动应变为横坐标,绘制并分析不同试样的动应力与动应变滞回环,如图2所示。利用每个滞回环曲线可计算动弹性模量(E_d)和等效阻尼比(λ_d)^[32-34],计算公式分别为

(1)${E}_{\mathrm{d}}=\frac{{\sigma }_{\mathrm{d}}}{{ε }_{\mathrm{d}}}$

(2)${\lambda }_{\mathrm{d}}=\frac{1}{4\mathrm{\pi }}\mathrm{ }\frac{{A}_{\mathrm{h}}}{{A}_{\mathrm{s}}}$

式中:σ_d为动应力;ε_d为动应变;A_h为滞回环ABCDA面积;A_s为△OAE面积。

弹性模量是弹性固体应力-应变关系的重要参数,由于峰值前后容易受到载荷变化与变形状态的影响,故选取滞回曲线峰值的30%和70%作为循环加载的主要过程,并分别进行线性拟合,即从每个滞回环加载段截取峰值应力30%~70%的两点之间斜率为加载段弹性模量,卸载段同理^[35-36]。弹性体受外力作用发生弹性变形,卸载后形状完全恢复,即弹性体受外加载荷做功,能量存储于弹性变形区域,卸载后能量释放,形状恢复。黏弹性材料的力学性能处于弹性材料和黏性材料之间,材料受外加载荷变化时既发生弹性变形又发生蠕变变形,因此,黏弹性材料应力和应变并不对应,还受时间、受载历史等因素影响。形状记忆合金受外加载荷时,实际发生弹性变形、塑性变形和蠕变变形,与黏弹性材料相似。图3^[37]为能量密度参数计算示意图。ABCF的面积为输入总能量,即加载段与坐标轴围成的面积;CDEF的面积为弹性变形能,即卸载段与坐标轴围成的面积;ABCDE的面积为滞回环面积,即耗散能。利用每个滞回环曲线可以计算弹性变形能(W_y),其计算公式为

(3)W_y=$\frac{1}{2}$σε=$\frac{{\sigma }^{2}}{2E}$

式(3)中:σ为最大循环应力;ε为对应的弹性应变;E为材料弹性模量。

3 结果与分析

图4为Ti-22Nb-xCe[x =0, 0.06, 0.1, 0.5(原子分数/%)]合金的循环加卸载应力-应变曲线。由图可见,随着循环加载次数增加,所有试样的滞回曲线均先整体下移而后逐渐趋于稳定。Ti-23Nb(原子分数/%)基合金中也观察到类似现象^[17]。在循环初期(少于10次),滞回曲线整体向右下方偏移。在10~30次循环期间,滞回曲线面积迅速减小。30次循环后,形成稳定的细长梭形,面积波动小于5%。Ti-22Nb-0.1Ce合金的稳定速度较高,经20次循环即达到稳定状态,循环稳定性较好。

图5(a)为Ti-Nb-Ce合金循环加卸载过程动弹性模量随加载次数的变化关系。可以看出,Ti-22Nb二元合金表现出典型的模量退化行为,初始模量急剧下降约40%,最终稳定在约60 GPa。Guedes等^[17]研究发现,Ti-23Nb合金在第一个拉伸加载循环的弹性模量约为68.63 GPa。Ti-22Nb-0.06Ce合金的动弹性模量与Ti-22Nb合金稳定后的接近。当Ce的原子分数增加至0.1%时,合金的动弹性模量大幅增加,整个循环过程中模量均高于100 GPa,且模量退化率低于5%,表现出良好的稳定性。随着Ce含量进一步增加,Ti-22Nb-0.5Ce合金的弹性模量也表现出较好的稳定性,稳定模量约为80 GPa。

Ti-Nb-Ce合金在加载与卸载过程的弹性模量演变规律如图5(b)、图5(c)所示。与动弹性模量类似,Ti-22Nb合金的加卸载弹性模量仍呈现出先下降后稳定的特征,且稳定后的模量与 Ti-22Nb-0.06Ce 合金的接近。值得注意的是,当Ce的原子分数达到0.1%时,弹性模量显著提高。然而,当Ce的原子分数进一步增加至0.5%时,弹性模量介于Ti-22Nb-0.1Ce合金与Ti-22Nb合金之间。可见稀土元素Ce对Ti-22Nb合金的刚度具有显著调控作用,适量Ce掺杂可显著增强材料抵抗变形的能力,较多Ce添加会一定程度降低材料的刚度。

图6(a)为Ti-Nb-Ce合金的等效阻尼比随循环次数的变化关系。可以看出,等效阻尼比与循环次数和Ce含量密切相关。在初始循环阶段(循环次数n<10),Ti-22Nb合金的等效阻尼比急剧下降30%~50%,在10~30次循环期间逐渐趋于平衡,当循环次数n>30时,波动幅度始终保持在5%以内,表现出明显的滞后稳定化效应。另外,稀土元素Ce的掺杂使合金的等效阻尼比整体降低,并且随着Ce含量的增加,合金等效阻尼比的稳定性逐渐增强。这一稳定性现象符合Granato-Lücke位错阻尼理论^[38]和KP模型^[39]。值得注意的是,Ti-22Nb-0.5Ce合金的等效阻尼比一直稳定在0.043附近,高于 Ti-22Nb-2Hf 形状记忆合金的0.032^[40]。

图6(b)为弹性变形能随循环次数的变化情况。可以看出,Ti-22Nb二元合金的弹性变形能随循环次数增加先降低后逐渐稳定。当掺杂原子分数为0.06%稀土元素Ce时,合金的弹性变形能减小。当Ce的原子分数增加至0.1%时,Ti-22Nb-0.1Ce合金的弹性变形能显著增加,且平均弹性变形能(-4.0×10⁶ J/m³)高于Ti-22Nb-0.5Ce合金(-5.0×10⁶ J/m³),表现出较好的弹性恢复能力。高Ce含量下弹性变形能储存能力下降可能与脆性金属间化合物的形成有关。值得注意的是,Ti-Nb-Ce三元合金在循环加载后均表现出相对稳定的弹性性能,且波动幅度控制在5%以内,没有出现能量耗散集中点,表明Ce掺杂使Ti-Nb合金具有均匀的变形能力和较好的抵抗损伤能力,并提升材料在服役过程的安全性与可靠性。

图7为Ti-Nb-Ce合金在循环加载前后的显微硬度变化。可以看出,稀土Ce的掺杂使Ti-Nb合金的显微硬度增大。研究发现,Mo添加也会提高 Ti-Nb 合金的显微硬度,Ti-20Nb-5Mo合金的硬度约400 HV^[21,41]。此外,所有合金试样的显微硬度经循环加载后均增大,表现出显著的循环硬化效应。事实上,循环硬化可以增强材料对后续变形的抵抗力,有助于提高服役寿命^[42]。

4 结论

采用真空熔炼工艺制备了不同Ce含量的 Ti-22Nb-xCe[x=0,0.06,0.1,0.5(原子分数/%)]合金,系统研究了合金在循环加载过程的滞回行为、弹性模量、弹性变形能、阻尼性能及显微硬度的变化规律,得到如下结论。

(1) Ti-Nb-Ce合金的滞回曲线均呈典型的滞后稳定化特征,随循环次数增加,先整体下移,随后面积迅速减小并最终稳定为细长的梭形。

(2)稀土Ce可以显著提高Ti-Nb合金的循环稳定性,并降低合金的等效阻尼比。适量Ce掺杂可以有效调控合金的弹性模量、弹性变形能及等效阻尼比,其中Ti-22Nb-0.1Ce合金具有最大的弹性模量与弹性变形能,具有最优的刚度稳定性和弹性恢复能力。

(3)稀土Ce掺杂与循环加载均显著提高合金的显微硬度。Ti-Nb-Ce三元合金的显微硬度均高于Ti-22Nb二元合金,且经过循环加卸载后,所有试样均表现出显著的循环硬化现象。

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