Research progress of high-entropy amorphous materials and their additive manufacturing technology
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摘要: 高熵非晶合金具有独特的物理、化学和力学性能以及更好的热稳定性，因而其制备技术成为国内外重要的研究热点之一. 然而利用传统技术制备高熵非晶材料时会产生晶粒粗大及材料浪费等缺点，难以满足工艺生产需要. 而增材制造技术的精准制造和快速冷却等特点可以解决这一问题，制备出各项性能优越的高熵非晶合金. 简要介绍了高熵非晶材料的研究体系和常用制造方法，着重阐述了高熵非晶材料的断裂强度、耐腐蚀性和热稳定性的研究，对增材制造技术的工艺特征和优势，以及利用增材制造技术制备高熵非晶合金的科学难点作出了总结. 结果表明，利用增材制造技术有利于获得致密均匀的高熵非晶材料，但对于非晶相形成的解释仅限于高熵合金4大效应.最后阐述了近年来利用常用的两种增材制造手段制造高熵非晶合金的研究，并对增材制造技术制备高熵非晶材料的发展趋势提出了展望.Abstract: High-entropy amorphous alloys (HEAAs) exhibit unique physical, chemical and mechanical properties as well as better thermal stability. Thus, its fabrication technology has become one of the important research hotspots at home and abroad. However, high-entropy amorphous materials manufactured by traditional technology had defects such as coarse crystal grains and material waste, which was difficult to meet the needs of processing production. The precise manufacturing and rapid cooling of additive manufacturing technology could solve the problems, and produce high entropy amorphous alloys with superior properties. This review research briefly introduced the research system and common preparation methods of high-entropy amorphous materials. It mainly focused on the research about fracture strength, corrosion resistance and thermal stability of high-entropy amorphous materials. The process features and advantages of additive manufacturing technology, and the scientific difficulties for applying this technology to fabricate high-entropy amorphous alloys were summarized. The results showed that additive manufacturing technology contributed to high-entropy amorphous materials with dense and uniform microstructures, while the explanation for the formation of amorphous phases was limited to the four effects of high-entropy alloys, Finally, a discussion with two additive manufacturing methods commonly used in the fabrication of high-entropy amorphous materials in recent years was made. Furthermore, the prospects for the development trend of fabricating high-entropy amorphous materials by additive manufacturing technology were put forward.
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Keywords:
- high-entropy alloy /
- amorphous phase /
- additive manufacturing /
- grain refinement
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0. 序言
2219铝合金作为重要的轻量化结构材料广泛应用于运载火箭贮箱等关键构件. 焊接是铝合金航空航天构件成形制造的必要工序，焊缝质量直接关系到铝合金构件的服役可靠性. 变极性钨极氩弧焊(variable polarity tungsten inert gas welding, VPTIG)因其工艺适应性好等优点，目前是2219铝合金焊接生产的主流工艺. 随着焊接电源技术的不断发展，有研究人员在常规VPTIG基础上引入高频(≥20 kHz)脉冲电流，创新性地提出了双频复合脉冲变极性氩弧焊接工艺(double-pulsed variable polarity tungsten inert gas welding, DP-VPTIG)[1]. 研究表明，20 kHz以上高频脉冲电流的引入可增强电弧力和挺度，增大焊缝熔深、增强熔池流动，促进焊缝组织细化，加速熔池气体逸出，进一步提升接头性能[2-3].
尽管VPTIG工艺已获得显著进步，但2219铝合金熔化焊接头强度系数和断后伸长率仍普遍较低，对接头进行强塑化处理具有重要的工程应用价值. 焊后热处理是调控接头显微组织和力学性能的重要手段. 目前针对2219铝合金电弧焊接头热处理优化的研究报道相对较少. 由于含有约6%Cu元素，2219铝合金可通过不同的时效处理在Al基体中引入多种沉淀析出相(GP，θ″，θ′，θ)，进而获得不同程度的析出强化效果[4]. Ding等人[5]研究发现固溶时效处理能对2219铝合金弧焊接头抗拉强度和疲劳强度具有一定的提升作用，较焊态分别提高43%和18%. Zhu等人[6]也报道了相似的研究结果，通过固溶时效处理可使得2219铝合金弧焊接头的抗拉强度提高44%，同时也能提高接头的耐腐蚀性能. Lü等人[7]研究了梯度失配对2219铝合金变极性TIG对接焊接头组织和性能的影响. 随着对接失配程度增加，接头强度逐渐降低. 搅拌摩擦焊接头组织和性能的影响. 随时效时间延长，接头强度能显著提高，但断后伸长率有一定降低. 周政等人[8]研究了不同气氛对2219合金TIG焊接头组织与性能的影响，研究发现采用氮气保护TIG焊可减小热影响区面积，提高断后伸长率和焊缝硬度. 综合上述研究，各种焊后热处理工艺对2219铝合金接头性能都能产生显著影响，但不同热处理工艺对接头性能调控的微观组织层面机理并未详细阐明. 如何通过优化焊后热处理工艺发挥材料本征组织-性能特点，实现焊缝强韧化，对进一步提升焊接质量十分关键.
以4 mm 2219-T6铝合金双频复合脉冲VPTIG焊接接头为研究对象，对比研究两种典型焊后热处理工艺(直接时效处理和固溶时效处理)对接头显微组织演变及力学性能的影响，探究不同热处理状态接头变形行为的微观机制，为2219铝合金电弧焊接接头热处理强化策略的优化设计提供理论参考.
1. 试验方法
焊接试件采用2219-T6铝合金板材，尺寸规格为240 mm × 120 mm × 4 mm. 焊前对试件板材进行表面油渍去除和酸碱洗表面氧化层去除，焊接方向垂直板材轧制方向. 采用1.2 mm ER2319焊丝作为填充金属，不开坡口. 通过北京航空航天大学自主研发的超音频脉冲电弧焊接系统(HPVP550)完成焊接试验，采用双频复合变极性脉冲方波电流(图1). 具体焊接工艺参数如表1所示.
表 1 焊接工艺参数Table 1. Welding parameters基值电流Ib/A 峰值电流IP/A 超音频脉冲
电流IHP/A低频脉冲
周期t2/ms超音频脉冲
周期t3/ms变极性电流
周期t1/ms送丝速度vs/(m·min−1) 焊接速度v/(m·min−1) 氩气流量Q/(L·min−1) 110 220 80 500 0.05 10 1.5 20 20 研究设计了两组热处理对比工艺. 根据相关研究报道，2219铝合金的峰值时效温度为175 ℃，保温12 h可获得较好的析出强化效果[5-6]. 因此，第一组为直接时效处理，即将焊接接头直接在175 ℃保温12 h后空冷至室温. 第二组为固溶时效处理，首先将接头在535 ℃保温1 h后快速水冷至室温，再将接头在175 ℃保温12 h后空冷至室温. 同时，将未经过热处理的焊态接头作为对照组.
采用线切割方法切取并制备金相试样，观察面磨抛后使用Keller试剂对金相试样进行化学侵蚀，使用ZEISS Scope.A1型光学显微镜对接头进行显微组织表征. 微观组织表征样品和力学性能测试取样位置和拉伸试样尺寸如图2所示. 采用截线法对平均晶粒尺寸进行统计测量，每组接头晶粒测量数不少于200个. 采用JEOL JSM 7100F型场发射扫描电镜(scanning electron microscopy, SEM)和FEI Tecnai G2 F20型透射电镜(transmission electron microscopy, TEM)对接头微观组织结构进行细致表征. 通过Image pro plus(IPP)软件对析出相特征尺寸进行定量统计，每组接头所统计的析出相粒子数量不少于100个. 其中，析出相总面积/视域面积百分比即为析出相面积分数. 使用INNOVATEST FALCON500型硬度计对焊接接头进行显微维氏硬度测试，加载载荷1.96 N，加载时间10 s. 在不同热处理状态接头不同区域测试至少10个点，统计硬度平均值作为该区域硬度. 根据GB/T 2651—2008 《焊接接头拉伸试验方法》标准采用INSTRON 5982型万能力学试验机进行室温单轴拉伸试验，拉伸应变速率为0.001 s−1. 测试前，铣掉拉伸试样焊缝处正反面余高.
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图 2 取样位置及样品尺寸示意图Figure 2. Schematic of sampling position and sizes of tensile samples. (a) schematic of sampling position; (b) illustration of tensile sample dimension2. 试验结果与分析
2.1 焊后热处理对晶粒形貌的影响
图3为不同热处理状态接头不同区域的光学金相组织. 从图3a~图3c可以发现，不同热处理状态2219铝合金接头热影响区内的α-Al晶粒皆以等轴晶形态为主. 焊态α-Al等轴晶平均直径为41.7 μm，直接时效态平均晶粒尺寸未发生明显增大，达到60.2 μm. 与前两者相比，固溶时效态热影响区等轴晶更加粗大，平均晶粒尺寸增大至96.4 μm. 受熔池凝固界面前沿元素偏聚促进异质形核的影响，氩弧焊可导致具有细晶特征的带状熔合区形成，位于热影响区和焊缝区之间，如图3d~图3f所示. 直接时效处理对熔合区附近的α-Al晶粒形态未造成显著影响，即热影响区为粗等轴晶，熔合区为细等轴晶，焊接区为粗大等轴枝晶且熔合区细晶尺寸未发生明显变化. 但从图3f可观察到，固溶时效态接头熔合区附近各区域内的α-Al晶粒都发生了一定程度的粗化，熔合区细晶组织特征未能得到保留. 如图3g所示，2219铝合金氩弧焊接头焊缝区主要以粗大的α-Al等轴枝晶为主，大量的α + θ共晶组织(图中黑色相)分布于初生α-Al枝晶臂之间. 直接时效处理未改变焊缝区的枝晶形貌特征(图3h)，但固溶时效处理导致焊缝区共晶组织显著减少，枝晶形态转变为粗大柱状晶特征(图3i). 由于焊前母材经过轧制 + T6(固溶 + 人工时效)热处理，因此，母材α-Al晶粒由大量沿轧制方向排列的拉长变形晶粒 + 少量细小等轴晶构成(图3j)，平均晶粒尺寸为13.4 μm. 经过直接时效处理后，拉长晶粒形貌特征基本保留，晶粒尺寸未发生显著变化，平均晶粒尺寸为22.6 μm. 但经过固溶时效处理后，母材区α-Al晶粒全部转变为粗大等轴晶，平均晶粒尺寸增大至70.1 μm. 从晶粒形态的演变可以推断，较低的时效温度(175 ℃)只能使母材变形晶粒发生轻微的粗化，而较高的固溶处理温度(535 ℃)，可显著促进母材晶粒发生再结晶和粗化，使得变形晶粒转变为粗大的等轴晶.
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图 3 不同热处理状态接头不同区域金相组织Figure 3. Metallography of different regions of the joints under different heat treatment conditions. (a) as-welded HAZ; (b) directly aging-treated HAZ; (c) solution and aging treated HAZ; (d) FZ line of the as-welded joint; (e) FZ line of the directly aging-treated joint; (f) FZ line of the solution and aging treated joint; (g) WS of the as-welded joint; (h) WS of the directly aging-treated joint; (i) WS of the solution and aging treated joint; (j) BM of the as-welded joint; (k) BM of the directly aging-treated joint; (l) BM of the solution and aging treated joint2.2 焊后热处理对第二相的影响
2219铝合金主要有两类常见第二相：一种是在凝固过程中产生的微米尺度共晶组织，由次生α-Al和θ-Al2Cu相构成[9]，主要呈长条状沿初生α-Al晶界分布，少量分布于初生α-Al晶粒内部；第二种为时效处理导致的纳米尺度富Cu析出相，如GP，θ″和θ′等亚稳时效析出相，主要分布于α-Al基体中. 通过SEM可表征不同热处理状态2219铝合金接头焊缝区共晶组织形貌，如图4所示. 从图4a可以看出，焊态焊缝区内存在大量共晶组织，由次生α-Al(暗色)和θ-Al2Cu相(亮色)层状交替构成. 直接时效态焊缝区内的共晶组织相对焊态更加分散，单个共晶组织平均尺寸略微降低，如图4b所示. 经过固溶时效处理后，焊缝区内共晶组织进一步分散，长条状共晶组织消失，且共晶组织内的θ-Al2Cu相由层状转变为更细小的短棒状或球状，如图4c所示.
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图 4 不同热处理状态2219铝合金接头焊缝区扫描电镜表征结果Figure 4. SEM characterization of welding seam of the 2219 aluminum alloy joints under different heat treatment conditions. (a) as welded; (b) directly aging treated; (c) solution and aging treated通过TEM对直接时效态和固溶时效态焊缝区内纳米尺度的析出相进行观察，表征结果如图5所示. 从图5a可以发现，直接时效态焊缝基体中存在低密度粗大θ′-Al2Cu析出相，并且析出相颗粒分布不均匀. 而固溶时效处理态焊缝区内存在大量弥散分布的细小θ″-Al3Cu析出相，如图5b所示. 对两种不同热处理接头焊缝区内共晶组织和时效析出相颗粒的特征尺寸进行定量统计，结果如表2所示. 从定量结果可以发现，固溶时效热处理可导致共晶组织减少和细化，同时导致基体内析出相尺寸减小且密度增大.
表 2 不同热处理焊缝区第二相特征尺寸定量统计结果Table 2. Characteristic sizes of second phases in the welding seams under different heat treatment conditions热处理状态 α + θ共晶组织 析出相 面积分数f(%) 周长l/μm 直径D/nm 厚度δ/nm 数量密度dn/nm−3 焊态 5.1 12.3 — — — 直接时效 4.7 11.2 106 5.4 11.7 固溶时效 2.5 1.8 22 0.6 68.5 ![]()
图 5 不同热处理状态焊缝区透射电镜表征结果Figure 5. TEM characterization results of welding seams under different heat treatment conditions. (a) directly aging treated; (b) solution and aging treated不同热处理工艺导致的焊缝区第二相组织演变差异与合金元素扩散行为有密切关系. 由于焊缝金属经历了非平衡快速凝固过程，合金元素未得到充分扩散，不仅导致基体存在一定程度的合金元素过饱和，同时也易造成局部元素偏聚和偏析. 在一定高温下，伴随着合金元素重新溶于基体，焊缝共晶组织会发生回溶；而在较低的温度下保温，α-Al基体中过饱和合金元素将以第二相的形式析出，以上两个过程皆需要通过原子的长程扩散来实现. 在175 ℃直接时效过程中，较低的保温温度使得原子扩散能力有限，富Cu共晶组织相对稳定，经过长时间时效后共晶组织回溶程度较低，焊缝基体元素过饱和程度未得到显著提升. 在时效过程中，较低的元素过饱和度使得析出形核率和形核密度较低，同时元素偏聚和偏析相可为析出提供异质形核点，导致不均匀析出产生，即处于优势能态的第二相晶核将优先吸收周围过饱和原子，进而持续长大熟化. 另外，由于碟盘状θ′/θ″第二相颗粒可引入各向异性的共格应力场，由于析出相粒子之间的共格应力场交互作用，易造成析出相偏聚长大行为[10-11]，如图5a中左侧粗大θ′-Al2Cu析出相偏聚形貌. 综合以上因素，直接时效处理最终易造成低密度且分布不均匀的粗大析出相形貌.
与之不同的是，固溶处理温度(535 ℃)已达到完全α-Al单相区，较高的保温温度使得原子扩散能力显著增强，共晶组织中的合金元素回溶于基体中，α-Al晶内基体中合金元素过饱和度显著增加. 固溶处理不仅减少了α-Al晶界附近共晶组织，同时能有效消除基体中的元素偏聚和偏析结构，有助于成分均匀化. 在相同的时效条件下，基体中较高的元素过饱和度和较均匀的元素分布导致较大的析出均匀形核率和形核密度，最终获得较细小和均匀的第二相析出形貌.
2.3 焊后热处理对力学性能的影响
对不同焊后热处理2219铝合金接头各区域的显微硬度进行测定，结果如表3所示. 结果表明，焊后接头较母材(base metal, BM)发生了显著软化，熔合区为接头强度最大区域，而热影响区(heat affected zone, HAZ)和焊缝区(weld metal, WM)硬度分别仅为母材硬度的78%和56%. 经过直接时效处理后，接头和母材硬度较焊态对应区域硬度略微升高，尤其是熔合区硬度升高显著，与母材硬度相当. 但是，热影响区和焊缝区硬度仍然较低，仅能达到母材硬度的83%和64%，接头软化现象依旧突出. 相比焊态和直接时效态，固溶时效处理使得接头各区域硬度得到了显著提升. 焊缝区硬度能达到母材硬度的93%，热影响区为接头强度最弱区域. 同时，接头各区域硬度分布更加均衡，接头软化现象得到明显改善，接头达到近似等强匹配. 但需要注意的是，固溶时效处理同时也导致母材硬度较焊态升高了16%.
表 3 不同热处理状态2219铝合金接头显微硬度(HV0.2)Table 3. Microhardness of 2219 aluminum alloy joints under different heat treatment conditions热处理状态 热影响区 熔合区 焊缝 母材 焊态 104 112 76 134 直接时效处理 117 141 89 140 固溶时效处理 144 155 148 156 不同热处理状态2219铝合金接头拉伸性能如表4所示. 焊态接头强度和断后伸长率相比母材发生了显著降低，分别仅为母材的57%和45%. 焊态接头强塑性显著恶化与接头软化密切相关. 由于接头焊缝区强度较母材区显著降低，在拉伸过程中，焊缝区首先发生屈服，导致后续塑性变形局限在焊缝区内发生，而母材区几乎不发生塑性变形，即发生显著的应变局域化，最终导致试样整体强度和断后伸长率降低. 经过直接时效处理后，接头整体强度较焊态略微升高，强度系数达到0.60，但断后伸长率却进一步降低至2.0%. 经过固溶时效处理后，接头强度较焊态接头发生显著升高，强度系数达到0.84，并且接头断后伸长率升高至7.0%，达到母材断后伸长率的56%.
表 4 不同热处理状态2219铝合金接头拉伸性能Table 4. Tensile properties of 2219 aluminum alloy joints under different heat treatment conditions热处理状态 抗拉强度
Rm/MPa断后伸长率
A(%)强度系数
φ2219-T6母材 439 12.5 — 焊态 253 5.5 0.57 直接时效处理 264 2.0 0.60 固溶时效处理 371 7.0 0.84 直接时效处理后，焊缝区为低密度不均匀分布的粗大θ′-Al2Cu析出相，其与基体保持半共格关系，只能引入较弱的共格应力场，且与位错的交互方式主要为绕过机制. 此种析出相组织析出强化效果较弱，对焊缝强化效果有限[12]. 焊态和直接时效态接头各区域的强度差异较大，导致拉伸过程中塑性应变主要集中在显著软化的焊缝区内，进而导致接头整体拉伸性能显著变差. 相比而言，固溶时效处理虽然导致α-Al晶粒发生粗化，但焊缝区高密度纳米θ″-Al3Cu析出相可引入较强的共格应力场. 同时，其与位错交互方式主要为切过机制，可产生更显著的析出强化效应[13-14]. 另外，接头各区域强度匹配更加均衡，促进接头整体塑性均匀变形，可获得较大的均匀断后伸长率，伴随显著的应变硬化可获得较高的抗拉强度.
2.4 断裂行为
为研究焊后热处理对拉伸断裂行为的影响，对拉伸样品断口附近区域进行截面金相组织观察，结果如图6所示. 焊态和直接时效态接头拉伸断裂位置位于熔合区附近1 ~ 2 mm距离范围的焊缝区内，且断裂裂纹与拉伸方向呈约45°. 通过高倍数金相照片(图6中插图)可以观察到，焊态和直接时效态接头断裂裂纹倾向于沿长条状共晶组织扩展.
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图 6 不同热处理状态2219铝合金接头拉伸断口裂纹扩展路径Figure 6. Cracking path of tensile sample fracture of the 2219 aluminum alloy joints under different heat treatment conditions. (a) as welded; (b) directly aging treated; (c) solution and aging treated造成以上现象主要是由于焊缝区显著软化，拉伸过程中主要的塑性应变将被局限在焊缝区，即发生显著的应变局域化现象. 沿晶界分布的长条共晶组织与基体之间的相界面易存在应力集中，可以为拉伸裂纹提供低能扩展通道. 而经过固溶时效处理后，接头拉伸断裂位于紧挨着熔合区的热影响区内，且裂纹扩展方向与拉伸方向几乎呈90°. 从硬度测试结果(表3)可知，固溶时效态接头热影响区为硬度最低的区域，拉伸过程中应变易集中于此区域，造成断裂在此区域萌生和扩展.
3. 结论
(1) 与2219铝合金双频复合脉冲TIG焊态组织相比，直接时效处理(175 ℃/12 h-空冷)对α-Al晶粒和共晶组织形貌影响较小，并导致焊缝区形成低密度不均匀分布的粗大θ′-Al2Cu析出相；固溶时效处理(535 ℃/1 h-水淬 + 175 ℃/12 h-空冷)使得α-Al晶粒发生粗化，同时共晶组织减少且细化，在焊缝区引入高密度均匀细小的θ″-Al3Cu相析出相.
(2) 直接时效处理对2219铝合金双频复合脉冲TIG焊接头强化作用有限，焊缝区硬度仅为89 HV0.2 (母材硬度64%)，强度系数仅达到0.60，断后伸长率降低至2.0%；固溶时效处理可显著改善接头软化问题，接头各区域硬度接近母材硬度，强度系数升高至0.84，断后伸长率达到7.0%.
(3) 直接时效态接头拉伸断裂于焊缝区，显著的接头软化和不均衡的强度匹配导致接头均匀塑性变形减小和整体强度显著降低；固溶时效处理可获得显著的接头析出强化效应，接头均匀塑性变形能力得到提升，拉伸断裂于热影响区.
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图 1 不同溶液中Fe80B20和(Fe,Co,Ni,Cr)80B20的极化曲线
Figure 1. Polarization curves of the as-spun Fe80B20 and (Fe,Co,Ni,Cr)80B20 alloy ribbons in different solutions. (a) 3.5% NaCl; (b) 0.1 mol/L H2SO4; (c) 0.1 mol/L HCl
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图 2 Fe25Co25Ni25(B, Si)25金属玻璃磁滞回线
Figure 2. Hysteresis loops of Fe25Co25Ni25(B, Si)25 metallic glasses
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图 3 Cr，Mn，Fe，Co和Ni在不同基体中的扩散系数与温度的关系
Figure 3. Temperature dependence of the diffusion coefficients for Cr, Mn, Fe, Co and Ni in different matrices
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图 4 原粉的X射线图和DSC曲线
Figure 4. Corresponding X-ray patterns and DSC curves compared with the original powder. (a) X-ray diffraction pattern; (b) DSC curves；(c) local amplification of DSC curves
表 1 典型高熵非晶合金系
Table 1 Typical high-entropy amorphous alloy system
高熵非晶合金系 制备方法 临界尺寸d/mm Zr41.2Ti13.8Cu12.5Ni10Be22.5[24] 浇铸法 >50 Ti20Zr20Hf20Cu20Ni20[23] 铜模铸造法 1.5 Sr20Ca20Yb20Mg20Zn20[25] 铜模铸造法 4 Er20Tb20Dy20Ni20Al20[25] 铜模铸造法 2 Pd20Pt20Cu20Ni20P20[26] 熔渣包覆水淬法 10 Fe20Si20B20Al20Ni20[27] 球磨法 — Ti20Zr20Cu20Ni20Be20[28] 铜模铸造法 3 CoCrCuFeNiZr0.6[4] 熔体快淬法 — Fe25Co25Ni25(B，Si)25[29] 铜模铸造法 1.5 Er18Gd18Y20Al24Co20[30] 铜模铸造法 5 Fe25Co25Ni25Mo5P10B10[31] 熔体快淬法 1.2 (Fe1/3Co1/3Ni1/3)80(P1/2B1/2)20[32] 熔体快淬法 2 Fe46.8Mo22.7Cr13.6Co7.6C4.8B2.3Y1.2Si1.0[33] 激光熔覆 — 
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