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通过慢拉伸、恒位移等加载方法, 评估了含氢Ti-2.5A1-2Zr-1Fe合金的力学性能衰减行为及氢脆敏感性的变化. 利用扫描电子显微镜对断口微观形貌特征进行了分析, 并采用二次离子质谱仪对氢的宏观分布进行了表征, 揭示了断口脆性区域与氢宏观分布之间的内在联系. 此外, 结合位错载氢运动模型及扩散方程, 探讨了氢的扩散机制以及慢应变速率对氢扩散过程产生的影响. 为了进一步探索氢化物的存在性, 利用透射电子显微镜对表面高氢浓度层和裂纹尖端及其附近物相进行了表征分析, 最终未发现氢化物相的析出, 综合上述实验数据和微观物相结构分析, 对Ti-2.5Al-2Zr-1Fe合金的氢脆机制进行了探讨, 认为该合金的氢脆机制由HEDE机制主导.The Ti-2.5Al-2Zr-1Fe used as hull structural material, is susceptible to hydrogen embrittlement induced by corrosion and hydrogen evolution in marine environments. Considering the long-term service of ships, the hydrogen embrittlement behavior under slow strain rate is crucial for evaluating the alloy’s service performance and ensuring long-term ship structural safety. In order to investigate the hydrogen embrittlement mechanism of Ti-2.5Al-2Zr-1Fe alloy under slow strain rate conditions, this study combines slow tension and constant displacement loading techniques to systematically evaluate the attenuation of mechanical properties and the dynamic changes in hydrogen embrittlement sensitivity of hydrogen-containing Ti-2.5Al-2Zr-1Fe alloy. Employing scanning electron microscopy (SEM), we thoroughly analyze the microstructural features of fracture surfaces. Meanwhile, the close correlation between the brittle zone at the fracture site and the macroscopic distribution of hydrogen atoms is elucidated by using secondary ion mass spectrometry (SIMS). Additionally, theoretical analysis based on diffusion equations reveals a notable increase in hydrogen diffusion distance within the Ti-2.5Al-2Zr-1Fe alloy as hydrogen charging time increases. Further, using the dislocation-hydrogen interaction model, we derive a critical strain rate threshold $ {\varepsilon _0} = {{\left( {30RT} \right)} {/ } {\left( {\rho DE} \right)}} $ for dislocation-mediated hydrogen transport in titanium alloys. When the externally applied strain rate ε falls below this threshold, dislocations efficiently capture and transport hydrogen atoms, enhancing hydrogen diffusion depth and significantly augmenting the alloy’s hydrogen embrittlement sensitivity, thereby accelerating material embrittlement. The Vickers-hardness (HV) test further elucidates the dual nature of hydrogen’s influence on titanium alloy properties: although moderate hydrogen content slightly enhances surface hardness, exceeding a specific threshold leads to a major negative influence on plasticity, far exceeding the benefits of surface hardening, resulting in a substantial decline in overall mechanical performance. To comprehensively decipher the hydrogen embrittlement mechanism of Ti-2.5Al-2Zr-1Fe alloy, transmission electron microscopy (TEM) is employed to analyze the phase composition in regions of high hydrogen concentration, crack tips, and their vicinities. The analysis results indicate that no direct precipitation of hydrides is observed; instead, hydrogen atoms preferentially accumulate in the β-phase, prompting microcrack propagation along β-phase boundaries. According to the aforementioned experimental data and microstructural analysis, we propose that the hydrogen embrittlement mechanism in Ti-2.5Al-2Zr-1Fe alloy is primarily governed by the HEDE mechanism. Furthermore, when the strain rate falls below ε0, it synergizes with the dislocation-mediated hydrogen transport mechanism, vastly expanding the influence scope of the HEDE mechanism and exacerbating the alloy’s hydrogen embrittlement sensitivity.
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Keywords:
- titanium alloy /
- hydrogen embrittlement /
- slow strain rate /
- hydride
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图 1 Ti-2.5Al-2Zr-1Fe微观组织图
Fig. 1. Microstructures of the Ti-2.5Al-2Zr-1Fe plate used in this work.
图 2 圆棒拉伸试样尺寸（单位为 mm）
Fig. 2. Dimensions of tensile specimen used in this work (unit: mm).
图 4 聚焦离子束(FIB)制取TEM试样过程示意图
Fig. 4. Process of preparing TEM samples by focused ion beam (FIB) used in this work.
图 6 不同充氢时间下的拉伸曲线 (a) 常规拉伸; (b) 慢应变拉伸
Fig. 6. Tensile stress-strain curves of the differently charged samples: (a) Conventional tensile test; (b) slow strain tensile test
图 7 两种应变速率下性能变化 (a) 断面收缩率; (b) 延伸率; (c) 抗拉强度
Fig. 7. Variation curves of mechanical properties of samples at different strain rates: (a) Reduction of area; (b) percentage elongation; (c) tensile strength.
图 8 两种应变速率下的氢脆敏感性变化
Fig. 8. Variation curves of hydrogen embrittlement sensitivity at different strain rates.
图 9 常规拉伸试样断口的宏观和微观形貌图 (a), (b), (c) 0 h常规拉伸试样; (d), (e), (f) 8 h常规拉伸试样
Fig. 9. Macroscopic and microscopic morphology of fracture surface in the conventional tensile test: (a), (b), (c) The 0 h conventional tensile sample; (d), (e), (f) the 8 h conventional tensile sample.
图 10 慢拉伸试样断口的宏观和微观形貌图 (a), (b), (c) 0 h慢拉伸试样; (d), (e), (f) 8 h慢拉伸试样
Fig. 10. Macroscopic and microscopic morphology of fracture surface in the slow tensile test: (a), (b), (c) The 0 h slow tensile sample; (d), (e), (f) the 8 h slow tensile sample.
图 11 不同充氢时间下试样断口的宏观形貌图 (a)—(d) 24—264 h的常规拉伸试样; (e)—(h) 24—264 h的慢拉伸试样
Fig. 11. Macroscopic morphology of the fracture surface of the differently charged samples: (a)–(d) The conventional tensile samples are 24–264 h; (e)–(h) the slow tensile samples are 24–264 h.
图 12 试样表面硬度随充氢时间的变化
Fig. 12. Variation of surface hardness of specimen with charging time.
图 13 二次离子质谱分析结果 (a)氘的分布; (b)铝的分布
Fig. 13. The SIMS analysis results of Ti-2.5A1-2Zr-1Fe alloy: (a) Distribution of deuterium; (b) distribution of aluminum.
图 15 充氢48 h WOL试样的断口宏观形貌
Fig. 15. Macro-morphology of fracture surface of WOL sample in constant displacement experiment after pre-cracking after 48 hours of charging.
图 16 (a) 充氢48 h WOL试样断口TEM形貌; (b) A区域的SAED图样; (c) B区域的SAED图样
Fig. 16. (a) The TEM morphology of fracture surface of WOL sample charged with hydrogen for 48 h; (b) the SAED pattern in area A; (c) the SAED pattern in area B.
图 17 Ti-2.5Al-2Zr-1Fe合金不同充氢时间下氢扩散深度理论值
Fig. 17. Theoretical values of hydrogen diffusion depth of Ti-2.5A1-2Zr-1Fe alloy at different charging time.
图 18 载氢位错与相界交互行为及其机制示意图
Fig. 18. Schematic Diagram of the interaction behavior and mechanism between hydrogen-loaded dislocations and phase boundaries.
表 1 二次离子质谱测试参数
Table 1. Parameters of SIMS testing.
入射能量/keV 入射角/(°) 电流强度/pA 扫描面积/m2 极性及质量范围/amu 30 45 1.142 500×500 负离子模式 0—227 
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[1] 杨锐, 马英杰, 雷家峰, 胡青苗, 黄森森 2021 金属学报 57 1455
Google Scholar
Yang R, Ma Y J, Lei J F, Hu Q M, Huang S S 2021 Acta Metall. Sin. 57 1455
Google Scholar
[2] 何燕, 周刚, 刘艳侠, 王皞, 徐东生, 杨锐 2018 物理学报 67 050203
Google Scholar
He Y, Zhou G, Liu Y X, Wang H, Xu D S, Yang R 2018 Acta. Phys. Sin. 67 050203
Google Scholar
[3] 吴明宇, 弭光宝, 李培杰 2024 物理学报 73 086103
Google Scholar
Wu M Y, Mi G B, Li P J 2024 Acta. Phys. Sin. 73 086103
Google Scholar
[4] 丁智松, 高巍, 魏敬鹏, 金耀华, 赵晨, 杨巍 2022 物理学报 71 028102
Google Scholar
Ding Z S, Gao W, Wei J P, Jin Y H, Zhao C, Yang W 2022 Acta. Phys. Sin. 71 028102
Google Scholar
[5] Robertson I M, Sofronis P, Nagao A 2015 Metall. Mater. Trans. A 46 2323
Google Scholar
[6] Venezuela J, Zhou Q J, Liu Q L 2018 Mater. Today Commun. 17 1
Google Scholar
[7] Olden V, Thaulow C, Johnsen R 2008 Mater. Des. 29 1934
Google Scholar
[8] Lynch S P 2007 NACE International Corrosion Conference Nashville, Tennessee, March, 2007 p07493
[9] Wang X, Zhu R T, Li C Y, Wang X, Huang P F 2020 Rare Met. Mater. Eng. 49 3769
[10] Zhang S Q, Wan J F, Zhao Q Y 2020 Corros. Sci 164 108345
Google Scholar
[11] Xu Y L, Li L T 2021 Mater. Res. Express 8 046531
Google Scholar
[12] 汪洋, 吴冰, 宿彦京, 邢焰, 王向轲, 高鸿, 李岩 2020 有色金属工程 10 33
Google Scholar
Wang Y, Wu B, Su Y J, Xing Y, Wang X K, Gao H, Li Y 2020 Nonferrous Met. Eng. 10 33
Google Scholar
[13] Sun Z G, Hou H L 2008 J. Alloys Compd. 476 550
Google Scholar
[14] Liu X Y, Wang J, Gao L Q 2021 J. Alloys Compd. 862 158669
Google Scholar
[15] Tien J, Thompson A W, Bernstein I M 1976 Metall. Trans. A 7 821
Google Scholar
[16] 吴明宇, 弭光宝, 李培杰, 黄旭 2023 物理学报 72 166102
Google Scholar
Wu M Y, Mi G B, Li P J, Huang X 2023 Acta Phys. Sin. 72 166102
Google Scholar
[17] 周伟, 姚泽坤, 谭立军, 郭鸿镇, 张建伟, 梁晓波 2011 稀有金属材料与工程 40 1230
Zhou W, Yao Z K, Tan L J, Guo H Z, Zhang J W, Liang X B 2011 Rare Met. Mater. Eng. 40 1230
[18] 赵晓丽, 张永健, 邵成伟, 惠卫军, 董瀚 2018 金属学报 54 1031
Google Scholar
Zhao X L, Zhang Y J, Shao C W, Hui W J, Dong H 2018 Acta Metall. Sin. 54 1031
Google Scholar
[19] 张滨, 郑华, 刘实, 王隆保 2005 原子能科学技术 39 522
Google Scholar
Zhang B, Zheng H, Liu S, Wang L B 2005 At. Energy Sci. Technol. 39 522
Google Scholar
[20] Chen C Q, Li S X, Lu K 2003 Acta Mater. 51 931
Google Scholar
[21] 王艳飞, 巩建鸣, 蒋文春, 姜勇, 唐建群 2011 金属学报 47 594
Wang Y F, Gong J M, Jiang W C, Jiang Y, Tang J Q 2011 Acta Metall. Sin. 47 594
[22] 刘战伟 2009 桂林电子科技大学学报 29 108
Google Scholar
Liu Z W 2009 J. Guilin Univ. Electron. Technol. 29 108
Google Scholar
[23] 孙志杰, 王洋 2020 材料开发与应用 35 94
Sun Z J, Wang Y 2020 Dev. Appl. Mater. 35 94
[24] 刘晓镇, 韩恩厚, 宋影伟 2023 中国有色金属学报 33 307
Google Scholar
Liu X Z, Han E H, Song Y W 2023 Chin. J. Nonferrous Met. 33 307
Google Scholar
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Wang X Y, Sun L L, Liu R P, Yao Y S, Zhang J, Wang W K 2004 Acta Phys. Sin. 53 3845
Google Scholar
[26] 孙永伟, 陈继志, 刘军 2015 金属学报 51 1315
Sun Y W, Chen J Z, Liu J 2015 Acta Metall. Sin. 51 1315
[27] 李洪佳, 孙光爱, 龚建, 陈波, 王虹, 李建, 庞蓓蓓, 张莹, 彭述明 2014 物理学报 63 236101
Google Scholar
Li H J, Sun G A, Gong J, Chen B, Wang H, Li J, Pang B B, Zhang Y, Peng S M 2014 Acta Phys. Sin. 63 236101
Google Scholar
[28] Kan B, Wu W J, Yang Z X, Li J X 2020 Mater. Sci. Eng. A 775 138963
Google Scholar
[29] Wang M Q, Akiyama E, Tsuzaki K 2007 Corros. Sci. 49 4081
Google Scholar
[30] 王贞, 刘静, 张施琦, 黄峰 2022 中国腐蚀与防护学报 42 106
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Wang Z, Liu J, Zhang S Q, Huang F 2022 J. Chin. Soc. Corros. Prot. 42 106
Google Scholar
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