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材料研究学报, 2026, 40(6): 474-480 DOI: 10.11901/1005.3093.2025.274

研究论文

热处理温度对FeCrVTa0.1W0.1Ti0.1C0.17 多组元合金组织与性能的影响

郭威1,2,3, 张月林1,2, 曹梓恒1,2, 李龙丰1,2, 赵觅,4, 吴树森1,2

1.华中科技大学 材料成形与模具技术全国重点实验室 武汉 430074

2.华中科技大学材料科学与工程学院 武汉 430074

3.深圳华中科技大学研究院 深圳 518057

4.华中科技大学航空航天学院 武汉 430074

Effect of Heat Treatment Temperature on Microstructure and Properties of FeCrVTa0.1W0.1Ti0.1C0.17 Alloy of Multi-components

GUO Wei1,2,3, ZHANG Yuelin1,2, CAO Ziheng1,2, LI Longfeng1,2, ZHAO Mi,4, WU Shusen1,2

1.State Key Laboratory of Materials Processing and Die & Mould Technology, Huazhong University of Science and Technology, Wuhan 430074, China

2.School of Materials Science and Engineering, Huazhong University of Science and Technology, Wuhan 430074, China

3.Shenzhen Huazhong University of Science and Technology Research Institute, Shenzhen 518057, China

4.School of Aerospace Engineering, Huazhong University of Science and Technology, Wuhan 430074, China

通讯作者: 赵觅，副教授，zhaomi2018@hust.edu.cn，研究方向为高温结构材料与金属高温腐蚀防护

收稿日期: 2025-09-11   修回日期: 2025-10-28  

基金资助: 国家自然科学基金(52201075)
湖北省重点研发计划(2025BAB012)
湖北省自然科学基金(2023AFB798)
深圳市科技计划(JCYJ20220530160813032)
深圳市科技计划(JCYJ20240813153421029)

Corresponding authors: ZHAO Mi, Tel: 17508640660, E-mail:zhaomi2018@hust.edu.cn

Received: 2025-09-11   Revised: 2025-10-28  

Fund supported: National Natural Science Foundation of China(52201075)
Key Research and Development Program of Hubei Province(2025BAB012)
Natural Science Foundation of Hubei Province(2023AFB798)
Shenzhen Science and Technology Program(JCYJ20220530160813032)
Shenzhen Science and Technology Program(JCYJ20240813153421029)

作者简介 About authors

郭 威，男，1987年生，副研究员

摘要

研究了不同热处理温度对FeCrVTa0.1W0.1Ti0.1C0.17多组元合金显微组织与力学性能的影响。结果表明，在800 ℃、900 ℃热处理的合金中析出的晶内细密Laves相产生强化作用使其强度显著提高(屈服强度达1501 MPa)，但是晶界上的富Fe相随着热处理温度的提高由孤立枝晶演变为连续网状结构，成为裂纹扩展优先路径而使合金的塑性下降。在1000 ℃热处理的合金中Laves相的粗化严重弱化其强化作用，而富Fe相则转变为孤立的团块状缓解了晶界脆性使塑性恢复到28.9%、而强度回复到铸态水平。富Fe相的形貌(连通性)是调控FeCrV基多组元合金塑性的关键因素，而Laves相的尺寸影响强度的演变。

关键词： 金属材料; 多主元合金; 热处理; 微观组织; 力学性能; 析出强化

Abstract

FeCrV-based alloy FeCrVTa0.1W0.1Ti0.1C0.17 was prepared by vacuum arc melting technique, and subjected to vacuum heat treatment. Then the effect of heat treatment temperatures (800 oC, 900 oC, 1000 oC) on its microstructure and mechanical properties were investigated viacompression tester, hardness tester, scanning electron microscopy, electron probe microanalyzer and X-ray diffractometer. It reveals that heat treatments at 800 and 900 oC may significantly enhance the alloy strength (yield strength up to 1501 MPa) through precipitation strengthening by fine intragranular Laves phases. However, as temperature increases, the Fe-rich phase at grain boundaries evolves from isolated dendrites into a continuous network structure, acting as a preferential path for crack propagation and leading to reduced ductility. At 1000 oC, coarsening of Laves phases severely weakens their strengthening effect, while the Fe-rich phase transforms into isolated blocky particles, alleviating grain boundary embrittlement and restoring ductility to 28.9%, with strength returning to the as-cast level. The results demonstrate that the morphology (connectivity) of the Fe-rich phase is the key factor governing ductility, while the size of Laves phases dominates the evolution of strength. This finding provides a reference for balancing the strength-ductility of FeCrV-based alloys of multi-components.

Keywords： metallic materials; multi-principal element alloy; heat treatment; microstructure; mechanical properties; precipitation strengthening

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本文引用格式

郭威, 张月林, 曹梓恒, 李龙丰, 赵觅, 吴树森. 热处理温度对FeCrVTa0.1W0.1Ti0.1C0.17 多组元合金组织与性能的影响[J]. 材料研究学报, 2026, 40(6): 474-480 DOI:10.11901/1005.3093.2025.274

GUO Wei, ZHANG Yuelin, CAO Ziheng, LI Longfeng, ZHAO Mi, WU Shusen. Effect of Heat Treatment Temperature on Microstructure and Properties of FeCrVTa0.1W0.1Ti0.1C0.17 Alloy of Multi-components[J]. Chinese Journal of Materials Research, 2026, 40(6): 474-480 DOI:10.11901/1005.3093.2025.274

对航空航天和能源等领域使用的装备性能要求越来越高和服役条件(高温、高压、强腐蚀、强辐照)越来越苛刻，因此对制造这些装备所用的金属材料的综合性能的要求也随之提高[1~5]。多主元合金独特的多主元效应、显著的晶格畸变效应以及缓慢扩散效应，具有比传统合金高的强度、耐腐蚀性以及高温组织稳定性[6~14]。富含高熔点元素的FeCrVTa系多主元合金具有优异的高温性能，其复杂成分和多主元特征使其具有优异的抗辐照性能，受到了极大的关注[15~18]。但是，FeCrVTa系多主元合金在凝固过程中出现成分偏析和脆性金属间化合物相(如Laves相)局部聚集，影响其性能。因此，应该调控其微观组织以使其强度与塑韧性平衡[19~23]。

热处理可提高多主元合金的微观结构和综合性能[24~36]。FeCoCrNiMo系多主元合金中析出相的形态、尺寸和分布，与退火温度有密切的关系[24]。在850 ℃热处理的合金中析出相细小呈现弥散分布，其硬度(峰值)约为601HV；在1050 ℃热处理后，析出相粗化使其硬度大幅度降低(约375HV)。将FeCoNiCrAl多主元合金涂层在500 ℃长时间保温，其中Al和Cr元素扩散产生的致密氧化物填充涂层孔隙，基体FeCoNiCr的相变使涂层界面结合强度和硬度显著提高[25]。将CoCrFeMnNi合金在不同温度热处理，其微观组织截然不同[26]。在900 ℃热处理后，合金仍保持面心立方(FCC)结构；在较低的温度热处理开始析出第二相，在700 ℃热处理在晶界和晶粒内部析出富含Cr元素的σ相；在500 ℃热处理，析出相的类型更加复杂。何峰[27]研究发现，NiCoCrFe合金在900 ℃具有稳定的单相FCC结构，但是在750 ℃长时间时效合金发生相分离而生成了与基体同为FCC结构但晶格常数不同的条带状组织，表明合金进入了亚稳态。因此，有望通过热处理调控FeCrVTa系多主元合金的微观结构[28~36]。本文研究退火温度对FeCrVTa0.1W0.1Ti0.1C0.17多主元合金微观结构和力学性能的影响。

1 实验方法

1.1 Fe-Cr-V-Ta-W-Ti-C合金试样的制备

实验用原料是纯度为99.95%的金属块(用纯度为99.95%的FeC引入C元素)，用真空电弧熔炼炉分步熔炼制备Fe-Cr-V-Ta-W-Ti-C低活化多主元合金。先将熔炼炉抽真空使其真空度为3 × 10-3~5 × 10-3 Pa，充入99.99%高纯氩气作为保护气体。先熔炼高纯Ti片去除残余氧气，再熔炼W和Ta得到W-Ta预合金，将其与V一起熔炼得到W-Ta-V预合金，最后加入Fe、FeC、Cr、Ti制备出目标成分合金。反复熔炼4次以上，以使合金成分均匀。将制备出的合金进行真空退火，退火温度分别为800 ℃、900 ℃、1000 ℃，升温速率为5 ℃/min，保温24 h后水淬冷却。将铸态试样记为RT，将退火温度为800 ℃、900 ℃、1000 ℃的试样分别记为HT800、HT900、HT1000。

1.2 性能表征

使用X射线衍射仪分析合金试样的物相，扫描角度为30°~100°，扫描速度为3 (°)/min。用扫描电子显微镜(SEM)观察试样的微观组织，用电子探针显微分析仪(EPMA)的波谱(WDS)功能分析试样表面微区成分和测定元素的分布。使用维氏硬度计测量硬度，加载载荷为200 g，保压时间为10 s。每个试样测试12次，去除最大值和最小值后取其结果的平均值。使用直径为3 mm长度为6 mm的圆柱试样测试压缩强度，应变速率为1 × 10-3 s-1，每个试样测试 12 次，去除最大值和最小值后取其平均值作为最终压缩强度值。

2 结果和讨论

2.1 热处理态FeCrVTa0.1W0.1Ti0.1C0.17 合金的微观组织

图1给出了在不同温度热处理的FeCrVTa0.1-W0.1Ti0.1C0.17合金的XRD谱。可以看出，谱中出现了BCC相、碳化物以及Laves相的衍射峰，其中HT1000合金的Laves相衍射峰强度最高。

图1

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图1   在不同温度热处理后FeCrVTa0.1W0.1Ti0.1C0.17合金的XRD谱

Fig.1   XRD patterns of FeCrVTa0.1W0.1Ti0.1C0.17 alloy after heat treatment at different temperatures


如图2a所示，在800 ℃热处理的合金组织中主要有BCC基底、白色碳化物相和黑色碳化物颗粒。值得注意的是，在图2b中红色线条标记区域，在合金的晶界出现了与基体的衬度明显不同的灰色析出相。对图2b A区域中元素的分析结果(表1)表明，上述灰色相为富Fe相，其在晶界的析出面积分数较小，呈不规则的枝晶状形态。根据元素组成推测，该相与基体同为BCC结构，其XRD衍射峰重合，因此在图1中无法分辨。图2c给出了图2b中黑框处组织的放大，可见晶间析出的细小白色Laves相，尺寸仅为几十纳米。

图2

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图2   HT800不同倍率的SEM照片

Fig.2   SEM images of HT800 at different magnifications (a) low-power microstructure, (b) high-power microscopic structure, (c) Laves phase microstructure


表1   在不同温度热处理后FeCrVTa0.1W0.1Ti0.1C0.17 合金晶界处富Fe 相的元素

Table 1  Elements in iron-rich phase at the grain boundaries of the FeCrVTa0.1W0.1Ti0.1C0.17 alloy after heat treatment at different temperature (atomic fraction, %)

AlloyFeCrVTiTaWC
HT80041.0821.2529.090.710.853.757.70
HT90040.0120.9128.440.190.631.308.52
HT100040.6623.9329.770.620.861.912.26

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如图3a所示，在900 ℃热处理的试样，其组织演变与在800 ℃热处理的显著不同。图3b中红色线条标记区域中晶界上富Fe的析出相析出显著加剧，元素分析结果(表1)确认其Fe含量(原子分数)为40.01%。在900 ℃退火的试样中枝晶状富Fe相遍布晶界并相互连通，构成了连续网状结构，极易成为裂纹扩展的通道而使合金的塑性劣化。图3c中的白色纳米Laves相从颗粒状转变为长度约200 nm的短棒状，在晶粒内密集分布。对HT900合金试样的EDS面扫结果(见图4)表明，红色标记区域内的晶界析出相显著富集Fe元素，而Cr、W、Ta元素较为贫化，Ti和Ta元素主要富集在碳化物中。

图3

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图3   HT900的SEM照片

Fig.3   SEM image of HT900 (a) low-magnification microstructure, (b) high magnification microstructure, area B is the gray precipitated phase, (c) microstructure of Laves phase


图4

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图4   HT900合金的EDS元素面分布

Fig.4   EDS elemental distribution of HT900 alloy


退火温度提高到1000 ℃，使合金的微观组织发生了显著的变化，如图5a所示。在图5b的红色线条标记区域，晶界富Fe相的析出形态发生了较大的变化。对图中C区域的元素分析结果(表1)表明，Fe的含量为40.66% (原子分数)。与在较低温度退火试样的组织相比，富Fe相由枝晶状演变为团块状且不相互连通。合金中这种孤立的团块状析出相有助于降低晶界脆性而使其塑性提高。在中温区800~900 ℃退火时BCC基体中C元素的溶解度较低，扩散速率不足以使其长距离迁移而偏聚在晶界附近的富Fe相中，可能形成了某种富Fe碳化物(如M23C6型)，使该相的脆性提高。在1000 ℃退火C在基体中的溶解度和扩散速率显著提高，使C原子从晶界富Fe相中扩散回基体或与其他元素生成更稳定的碳化物，导致富Fe相中的C含量降低，其形态也从连续的枝晶/网状转变为孤立的、更接近平衡态的团块状。图5c中白色Laves相的数密度降低，但是尺寸增大到亚微米级且在组织中更为均匀的分布。随着退火温度的提高，原子的扩散增强。根据Ostwald熟化机制，较小的析出相(具有更高的界面能和溶解度)逐渐溶解，较大的析出相进一步长大以降低系统的总界面能。这表明，处于HT1000状态的Laves相其数密度降低但是尺寸显著增大。

图5

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图5   HT1000微观组织SEM照片

Fig.5   SEM image of HT1000 (a) low-magnification microstructure, (b) high-magnification microstructure, the C zone is the gray precipitate phase, (c) Laves phase microstructure diagram


2.2 热处理态FeCrVTa0.1W0.1Ti0.1C0.17 合金的力学性能

图6给出了在不同温度热处理后合金的室温压缩应力-应变曲线，其力学性能列于表2。可以看出，随着热处理温度的提高合金的强度呈先提高后降低的趋势，其演变规律与微观组织中的Laves相和富Fe相的形态、尺寸以及分布密切相关。在800 ℃和900 ℃热处理的合金，其硬度和屈服强度显著提高，HT900屈服强度达到1501 MPa，硬度达到774.2 HV0.2 (峰值)。这一强化效应，可归因于晶内析出的细密Laves相。根据Orowan强化机制，是纳米级析出相阻碍位错运动，其强化贡献可表示为

图6

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图6   在不同温度热处理后FeCrVTa0.1W0.1Ti0.1C0.17合金的力学性能

Fig.6   Mechanical properties of the FeCrVTa0.1W0.1Ti0.1C0.17 alloy after heat treatment at different temperatures (a) compressed stress-strain curve, (b) curve showing the variation of mechanical properties with heat treatment temperature


表2   在不同温度热处理后FeCrVTa0.1W0.1Ti0.1C0.17合金的力学性能

Table 2  Mechanical properties of the FeCrVTa0.1W0.1Ti0.1C0.17 alloy after heat treatment at different temperatures

AlloyHardness (HV0.2)Yield strength / MPaBreaking strength / MPaPlastic strain / %Breaking strain / %
RT637.1 ± 5.21350 ± 162664 ± 1533.8 ± 0.135.8 ± 0.1
HT800741.0 ± 6.81459 ± 122573 ± 1417.0 ± 0.319.0 ± 0.3
HT900774.2 ± 7.91501 ± 152352 ± 158.9 ± 0.110.7 ± 0.1
HT1000707.6 ± 6.21351 ± 122665 ± 1528.9 ± 0.230.8 ± 0.2

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∆σprecip=0.8Gbλlndb

其中G为剪切模量， b 为Burgers矢量，λ为析出相间距，d为析出相尺寸。HT800中Laves相的尺寸为几十纳米，间距小，强化效果较为显著；HT900中的Laves相虽略有粗化(约200 nm)但是数密度较高，依旧显著的强化作用使合金的硬度和屈服强度都有所提高，但是塑性降低。HT800和HT900的塑性应变分别降至17.0%和8.9%，低于铸态合金的33.8%。塑性劣化的主要原因，是晶界上的富Fe相形态的变化。HT800中晶界上析出的富Fe相数量较少且呈不规则枝晶状，引发局部应力集中促进了裂纹的萌生和扩展，使塑性劣化。与铸态合金相比，HT900的塑性应变下降了74%，表现出严重的脆化。其主要原因是，晶界上大量析出的枝晶状富Fe相相互连接形成了大尺寸网状结构，使裂纹极易沿晶界扩展。此外，虽然HT900的屈服强度最高但其断裂强度却最低，表明其损伤容限极差，其根源在于晶界上连续的富Fe网状结构。一旦屈服后在晶界萌生的微裂纹便沿着脆性的网状通道无阻碍地扩展，使材料在较低的应变下就发生断裂。

与铸态合金相比，在1000 ℃热处理(HT1000)的合金强度基本不变，但其塑性小幅度降低，其硬度为707.6HV0.2，屈服强度为1351 MPa，塑性应变为28.9%。其原因是，细小析出相的数密度显著降低使得析出强化大幅度减弱导致硬度降低。细小Laves析出相的强化和大尺寸富Fe相的弱化，使其屈服强度与铸态合金持平。虽然HT800中的富Fe相未完全连通但其尖锐的枝晶是更严重的应力集中源，更容易萌生微裂纹。而HT1000中的团块状形态则较为圆钝，不会产生严重的应力集中。同时，因Laves相粗化HT1000的基体强度降低，基体中应力的重新分布延缓了裂纹的萌生。这两者共同作用，使HT1000具有比HT800更好的塑性。与HT900相比HT1000的脆性得到一定的缓解，得益于富Fe析出相的扩散充分而不形成相互连接的枝晶结构，而是以团块状分布于各晶界缓解了应力集中并阻碍裂纹的扩展。在HT900的变形过程中，脆性连续晶界网状相使位错在晶内塞积产生的应力集中不能通过晶界滑移或激发晶粒内部滑移系来协调，使应力高度集中在脆性相或其与基体的界面上，极易达到脆性相的断裂强度。同时，连续的网状结构为裂纹扩展提供了贯穿晶粒的“快速通道”，导致沿晶裂纹的早期萌生和高速扩展。反之，HT1000中孤立的团块状相虽然仍是脆性的，但因其不连续使裂纹扩展必须频繁改变路径(如绕过颗粒或撕裂基体)而消耗更多的能量，使其塑性恢复。虽然在不同温度热处理的合金中晶粒内部均析出了细小Laves相，但是晶界上析出的富Fe相使合金的力学性能降低。

权宣通[36]发现，Al0.3CoCrFeNi高熵合金在500~700 ℃退火后晶内弥散析出的L12相使其屈服强度提高，而在700 ℃退火因L12相粗化和分布密度下降强度略有降低；在800 ℃退火后晶界上开始析出弱化晶界的B2相。马铭涛[24]发现，FeCoCrNiMo高熵合金的强度也有相同的演变规律。这种强度的演变规律，与本文的结果相同。但是，本文的独特结果是，FeCrVTa0.1W0.1Ti0.1C0.17合金在1000 ℃热处理使其塑性显著恢复，其原因是脆性晶界相由连续网状向孤立团块状的转变。这个结果，为平衡FeCrVTa系多主元合金的强塑性矛盾提供了依据。

3 结论

(1) FeCrVTa0.1W0.1Ti0.1C0.17多主元合金分别在800 ℃和900 ℃热处理后，晶内析出的细密Laves相(尺寸由几十纳米增长至200 nm)产生了强析出强化效应，使硬度和屈服强度显著提高。

(2) 随着退火温度的提高，晶界富Fe相由孤立枝晶态演变为连续网状结构。这种结构成为裂纹扩展的快速通道，使合金的塑性急剧劣化。热处理温度提高到1000 ℃，合金中晶内Laves相发生明显粗化，使强化效果减弱；晶界上的富Fe相转变为孤立的团块状缓解了应力集中，从而使合金塑性部分恢复。

(3) 热处理温度的改变使析出相的形态、尺寸和分布发生变化，可协同调控合金的强塑性。晶内Laves相与晶界富Fe相的协同演化决定了合金的力学性能。

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