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金属学报, 2023, 59(1): 75-86 DOI: 10.11900/0412.1961.2022.00431

综述

基于高通量制备的增材制造材料成分设计

张百成,1,2, 张文龙1,2, 曲选辉1,2

1.北京科技大学 新材料技术研究院 北京材料基因工程高精尖创新中心 北京 100083

2.北京科技大学 现代交通金属材料与加工技术北京实验室 北京 100083

Composition Design of Additive Manufacturing Materials Based on High Throughput Preparation

ZHANG Baicheng,1,2, ZHANG Wenlong1,2, QU Xuanhui1,2

1.Beijing Advanced Innovation Center for Materials Genome Engineering, Advanced Material & Technology Institute, University of Science and Technology Beijing, Beijing 100083, China

2.Beijing Laboratory of Metallic Materials and Processing for Modern Transportation, University of Science and Technology Beijing, Beijing 100083, China

通讯作者: 张百成，zhangbc@ustb.edu.cn，主要从事增材制造研究

责任编辑: 毕淑娟

收稿日期: 2022-08-31   修回日期: 2022-10-20  

基金资助: 国家重点研发计划项目(2021YFB3802300)
国家自然科学基金项目(51901020)
国家自然科学基金项目(52171026)

Corresponding authors: ZHANG Baicheng, associate professor, Tel:(010)82663610, E-mail:zhangbc@ustb.edu.cn

Received: 2022-08-31   Revised: 2022-10-20  

Fund supported: National Key Research and Development Program of China(2021YFB3802300)
National Natural Science Foundation of China(51901020)
National Natural Science Foundation of China(52171026)

作者简介 About authors

张百成，男，1984年生，副教授，博士

摘要

增材制造作为一种新型制造技术，为航空航天、交通运输和生物医学等领域带来了革命性变化。但目前增材制造用金属材料仍基于传统合金，部分材料并不适用于高能束加工，性能仍有提高空间。目前的增材制造专用材料开发未脱离传统试错法，效率低下，是制约增材制造材料性能提高的瓶颈问题。本文就增材制造钢、钛合金、铝合金材料现状和问题进行了讨论，并列举增材制造高通量制备和表征技术在材料开发和设计上的应用，结合增材制造高通量制备的原理和特点，最后阐述了增材制造高通量制备和表征技术在材料开发上的机遇和挑战，并对增材制造关键材料开发与成分优化未来的发展方向做出展望。

关键词： 增材制造; 高通量材料制备与表征; 材料开发; 力学性能

Abstract

As a new manufacturing technology, additive manufacturing has brought about revolutionary changes in the aerospace, transportation, and biomedicine fields. However, since the metal materials used in additive manufacturing are still mainly traditional alloys, some of them are unsuitable for high-energy beam processing, indicating room for performance improvements. Besides, the development of additive manufacturing materials still follows the traditional trial-and-error model, seriously restricting the development of high-performance materials. Therefore, this paper discusses this situation and the existing additive manufacturing technology problems of steel, titanium alloys, and aluminum alloys, after which the application of high-throughput preparation and characterization technologies in material development and design were expounded. Combined with the principle and characteristics of high-throughput additive manufacturing preparations, the prospects and challenges of the high-throughput preparation and characterization technology of additive manufacturing in material development were expounded. Then, futuristic developmental directions of key materials for additive manufacturing development and composition optimization were proposed.

Keywords： additive manufacturing; high-throughput preparation and characterization; materials development; mechanical property

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本文引用格式

张百成, 张文龙, 曲选辉. 基于高通量制备的增材制造材料成分设计[J]. 金属学报, 2023, 59(1): 75-86 DOI:10.11900/0412.1961.2022.00431

ZHANG Baicheng, ZHANG Wenlong, QU Xuanhui. Composition Design of Additive Manufacturing Materials Based on High Throughput Preparation[J]. Acta Metallurgica Sinica, 2023, 59(1): 75-86 DOI:10.11900/0412.1961.2022.00431

增材制造(additive manufacturing，AM)技术(也称为三维(3D)打印技术)发展于20世纪80年代后期，是一种集制造技术、信息技术和新材料技术多学科融合发展的新型制造技术[1~3]，因其具有材料设计制造自由度高的特点，给航空航天、交通运输和生物医学等领域带来了革命性变化，更是被美国麦肯锡咨询公司列入决定未来经济的十二大颠覆技术之一[2]。有别于传统减材或等材制造技术，金属增材制造通过高能束激光、电弧或电子束等热源使材料之间有效熔合，逐层累加材料构建出三维实体的制造技术，随着增材制造技术的不断发展和完善，针对金属材料逐渐形成了一系列比较成熟的高能束增材制造技术，例如选区激光熔化(SLM)、定向能量沉积(DED)以及电子束熔融(EBM)等。近年来，高能束增材制造合金材料因其独特的微观结构和优异的力学性能引起了学者们的广泛关注，其快速凝固和冷却的工艺特点更容易获得精细的组织结构以提高材料的力学性能，在金属材料开发应用领域具有极大潜力。

金属材料作为高能束增材制造技术的原料，是保证打印质量的基础，其成分及质量决定了产品性能，也直接影响了金属增材制造技术的应用范围。然而，目前增材制造用合金材料主要基于传统合金，这些传统系列合金材料主要基于铸、锻、焊等传统工艺开发，在高能束加工过程中易产生开裂或者性能退化。因此，优化和开发增材制造技术新型材料体系，拓展材料种类和应用范围显得尤为重要。

按照材料传统设计路线，实现材料的开发到产品的应用，通常遵循顺序迭代试错的研发模式[4]：对目标成分进行反复试错，直至其宏、微观组织结构达到一定的要求，或者性能满足某种产品适用标准，而这往往需要很长的时间周期和高昂的经济成本。而增材制造用粉体材料中的制粉过程更加剧了串联式材料设计的困难和复杂程度，因此极大限制了增材制造专用材料的研发进展。

在材料开发领域，材料基因工程的思想为未来新材料开发带来了新的理念，材料基因工程借鉴生物基因研究方法，将材料牌号、成分、结构、性能相互对应关系组成传统材料独特的“材料基因数据库”，但由于增材制造工艺冷却速率远高于传统工艺，传统数据库并不适用于增材制造合金材料的开发和设计，因此建立独特的增材制造材料数据库至关重要。高通量技术用最少的实验次数获得最多的材料数据，极大地加快了新材料的研发速度，并形成了一套完备的新材料开发方法，例如高通量计算平台的并发式材料计算筛选、离散/梯度变化样品的高通量制备、材料高通量表征与服役评价等技术[5]。其中，高通量制备和表征是加速新材料开发和材料数据库构建的关键步骤。高通量制备通过一次实验可制备得到成分特征连续梯度变化或上百个成分离散变化的样品，高通量表征允许一次实验对上百个不同特征试样进行表征，通过高通量制备和表征可同时获得大量实验数据，以求最少的样品制备、最小的体积消耗的情况下快速智能地对材料成分的数据进行评估和预测[6]。高通量制备和表征成分梯度材料，可以获得新合金材料或新合金成分，构建材料成分-结构-性能内在联系以及完善材料数据库，使得新材料开发简单化、科学化，高通量材料开发流程与传统试错流程对比如图1所示。

图1

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图1   高通量材料开发流程与传统试错材料开发流程对比

Fig.1   Comparison of the high-throughput material development process (a) with traditional trial-and-error material development process (b)


通过材料基因工程思想解决增材制造领域材料研发难题是增材制造研究的重点，利用高通量制备与表征手段建立成分-结构-性能之间的联系，不仅能在最小成本下快速筛选极端成分点，充分发掘材料潜力，加速增材制造专用材料的开发，还可以快速完善增材制造材料数据库，通过大数据技术和高通量手段实现新材料的预测和验证。本文通过回顾增材制造传统系列材料的研究现状引出不同材料体系中的研发前沿方向，并通过材料基因工程思想对不同材料性能提高手段进行分析，最后阐述了高通量技术在增材制造材料开发上的前景和挑战。

1 增材制造材料现状

目前最常见的增材制造合金材料包括钢材、钛合金、镍合金、铝合金和铜合金[7~11]，这些材料在过去几年中已被广泛研究和讨论。该部分通过材料成分角度简要总结了铝合金、钛合金和钢的组织结构的演变规律，引出增材制造合金材料在微观、介观、宏观层面面临的几个关键问题，并论述了高通量增材制造材料设计方法在解决这些问题方面的独特优势，如图2[12~15]所示。通过高通量增材制造制备和表征梯度试样，开发和优化增材制造新合金材料，解决不同尺度下增材制造材料面临的科学难题，有望推动航空航天关键部件性能进一步提升。

图2

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图2   高通量增材制造提升航空航天关键材料性能[12~15]

Fig.2   Improving the performance of key aerospace materials by high-throughput additive manufacturing technology[12-15] (BD—building direction, UTS—ultimate tensile strength, YS—yield strength, wNi—mass fraction of Ni)


1.1 铝合金成形性优化

铝合金作为航空航天和交通运输领域重要的轻质结构材料，是增材制造技术广泛应用和研究的材料之一。铝合金通常采用锻造等传统方式成形，具有优异的力学性能，其合金体系庞大，元素种类繁多，第二相复杂，但由于Al对氧敏感，能量吸收率低，高凝固收缩和导热的特性，通过高能束增材制造方式成形困难[16]。开裂是增材制造铝合金最常见的失效形式，原因在于熔池内非平衡凝固致使溶质富集，液相平衡线改变导致成分过冷，柱状枝晶交错生长形成晶间通道，冷却过程中液相凝固收缩和热收缩产生空洞和微裂纹，并通过晶粒内或晶间扩展最终引起开裂[17]。共晶元素可以降低凝固范围从而减少热裂倾向，例如Si元素可以降低铝合金熔点和热膨胀，提高熔体流动性，并在晶界以纳米颗粒形式析出增强Al基体[18]，这也是Al-Si系铝合金研究最早且打印工艺最成熟的原因。典型的AlSi10Mg合金在增材制造高冷速条件下，表现出良好的可打印性和精细的微观结构，具有高于铸造接近锻造合金的力学性能。然而由于增材制造有别于传统制造的热过程，沉淀相的形成存在很大差异，导致其他系列传统铝合金仍然较难直接通过增材制造方式制造或难以达到所需结构和性能，例如传统时效Al-Cu合金在基体内形成均匀细小的板状Al2Cu沉淀相，显著增强Al-Cu合金性能[19]，而增材制造Al-Cu系列合金在凝固过程中Cu元素在晶界处偏析，Al2Cu或其他三元共晶相在晶界处形成并随着热循环逐渐粗化和连通，导致了较低的抗裂性[20]，不难发现增材制造铝合金中第二相的析出对成形性以及性能提升十分重要。

近年来，研究[17]表明添加形核剂是一种有效的提高铝合金打印性和力学性能的成分改性方法，例如，ZrH2粉末改性铝合金7075、6061等。高能束增材制造变形铝合金过程中，由于温度梯度的存在，材料内部形成了发达的平行于构建方向的柱状晶(图3a[17]和b[21])，晶间空腔和裂纹在凝固收缩引起的残余应力作用下沿晶间扩展导致开裂。Zr的加入在熔池反应形成Al3Zr，与基体Al相晶格失配度小于0.52%，高冷速下在凝固前沿形成大量低能垒异质形核位点，诱导产生精细无裂纹的异质等轴晶结构(图3c[22])，表现出接近锻造合金的力学性能，实现了难打印材料的高性能增材制造[17]。事实证明了成分改性在诱导铝合金异质形核、促进第二相析出强化方面具有显著作用，而在合金开发、成分优化以及解决增材制造合金成形问题方面，增材制造高通量制备表现出巨大的潜力。据报道[23,24]，2%Zr (质量分数，下文若非特殊说明，元素成分均为质量分数)改性的铝合金无裂纹产生，但过度的Al3Zr硬脆相导致材料延展性降低，而Zr含量降低至0.6%时，材料延展性提高但晶粒细化不充分，结合铝合金改性原理和高通量增材制造优势，通过增材制造高通量制备和表征Zr含量在0.6%~2%梯度渐变铝合金试样，能够获得精细的全等轴晶和高强韧组合铝合金。Jin等[25]在Al-Cu合金中引入0~2%的TiC，诱导均匀的等轴晶形核以及Al2Cu相的均匀析出，高通量制备和表征TiC含量为0~2%梯度变化的Al-Cu合金，能够筛选得到晶粒最细，强韧性最好的Al-Cu合金。Li等[14]通过在Al-Mn-Mg合金中引入0.5%(Sc + Zr + Hf) (原子分数)过渡元素来诱导等轴晶原位形核以及形成层状异质结构产生，Al3(Sc, Zr, Hf)和Al6Mn强化相分别在晶界和晶内的析出使材料强度得到显著提升，通过增材制造高通量制备和表征更能短时间内筛选上百种不同成分比例的(Sc + Zr + Hf)复杂形核剂，快速开发增材制造新型铝合金并获得材料的最佳组织结构特性。Leijon等[26]利用共溅射和电子束重熔方式制备出高成分分辨率的Al-Nb和Al-Zr梯度材料，通过组织形貌以及显微硬度等高通量表征分析发现，Nb含量为1.3%~2.4% (原子分数)时，材料发生柱状晶向等轴晶的转变且晶粒显著细化(图3d[26])，晶粒细化能够有效抑制增材制造铝合金中的热裂倾向，为新型可增材制造Al-Nb合金成分确定范围。

图3

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图3   铝合金凝固曲线及晶粒长大示意图，改性前后增材制造铝合金晶粒结构形貌，及高通量优化铝合金成分范围[17,21,22,26]

Fig.3   Solidification curves and crystal growth diagrams (a)[17], grain structures of additive manufacturing aluminum alloy before (b)[21] and after (c)[22] modification, and high-throughput composition optimizations of aluminum alloy (d)[26] (Insets in Fig.3d show microstructure evolution of 1.3% and 2.4%Nb (atomic fraction) modified additive manufacturing aluminum alloy)


1.2 钛合金等轴晶结构控制

由于钛材料弹性模量低、导热系数小，采用传统机加工方式成形困难，周期长且成本高，是公认的传统难加工材料，增材制造已经成为航空航天领域钛合金关键部件的重要制备方式[27,28]。钛合金分为α、α + β以及β型钛合金，随合金元素种类和含量的不同具有不同的平衡相[29]。例如Al、Si元素的加入有利于α相的稳定，形成具有hcp结构的针状α/α'钛合金(图4a[30])，因其优异抗蠕变性和可焊性，广泛用于石油化工、交通运输领域[30]。α + β钛合金用途最广(如Ti6Al4V)，除了含有α稳定元素外，还含有β稳定元素，如V、Cr、Mo、Nb，这些元素的加入有利于降低α→β转变温度，增大α + β相区，通过增材制造可得到精细的α + β双相结构(图4b[31])，这类钛合金具有优异的强度、延展性、疲劳和抗蠕变性等综合力学性能，常用于航空航天等领域[31]。继续增加β稳定元素使得β相能够在室温稳定保留，通过增材制造最终形成蜂窝状β结构钛合金(图4c[32])，如Ti-Ta合金，它们具有低弹性模量、高强度质量比、高韧性和疲劳强度，是一种有前途的生物医学材料[32]。由于增材制造高冷速下显著的温度梯度使生长方向与热梯度方向一致或相近的柱状β晶粒具有更大的生长优势，受此影响，α、α + β以及β钛合金普遍表现出粗大柱状晶以及外延生长的特点，值得注意的是，α、α + β或β结构均来自优先凝固的β晶，其形状和尺寸直接影响钛合金最终的结构和性能。最终形成一定的织构并表现出显著的各向异性[28,33] (图4d[33~37])。增材制造钛合金中粗大柱状晶和织构严重限制了其性能的进一步提升，加速了构件的累积损伤失效[33]。

图4

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图4   增材制造α、α + β、β钛合金微观结构及增材制造钛合金水平、构建方向力学性能范围[30~37]

Fig.4   Microstructures of α (a)[30], α + β (b)[31],and β (c)[32] titanium alloys by additive manufacturing, and mechanical properties distribution in transverse and longitudinal directions of additive manufacturing titanium alloy (d)[33-37] (Z—building direction, αGB—grain boundary of α phase. Inset in Fig.4b shows fine layered Widmanstätten structure, X—xz plane)


为了避免增材制造钛合金中柱状β晶带来的不利影响，一种有效的办法是通过引入新元素提高材料成分过冷能力，抵消高热梯度的负面影响，限制晶粒生长的同时激活更多原子形核，从而形成精细的等轴晶结构[38]。Zhang等[38]利用Ti-Cu合金具有较高的组织过冷能力这一特性，将Cu元素引入钛合金中，确保在组成过冷区触发异质成核，使柱状晶粒完全转变为等轴晶粒，并且使原β晶粒细化了2个数量级(图5a和b[38])。这种精细的完全等轴晶粒和共析薄片组织，使Ti-Cu合金具有出色的力学性能，Ti-8.5Cu和Ti-3.5Cu分别表现出优异的强度和延展性(图5c[38])。Zhang等[39]利用Fe、Cr、Ni等元素偏析过程对钛合金进行微米级浓度调控，通过添加4.5%316L同样实现了钛合金的精细化等轴晶转变，同时形成了具有高度异质性和超精细的调制α' + β双相结构钛合金。结果表明，引入新合金成分提高材料成分过冷能力是增材制造高冷速下实现精细等轴晶转变的有效手段。通过报道[38,39]可以发现8.5%Cu以及4.5%316L等成分配比的选取可能并非准确，这种成分选取的方式仍遵循传统试错模式，难以得到材料的最佳性能组合。增材制造高通量制备具有成分和组织结构特征梯度连续变化的试样，对成分梯度变化的Ti-(3.5%~8.5%)Cu以及(0~6%)316L调制的钛合金进行表征，理清成分-结构-性能演变规律，有望得到更精细的全等轴晶结构并实现钛合金微观结构和力学性能的最佳搭配，使其性能得到进一步提高。Gong等[40]通过增材制造高通量制备和表征技术研究Ti-xMn (x = 1~12，质量分数，%)梯度合金的微观结构和显微硬度关系，建立成分-结构-性能联系发现，随着Mn含量的增加结构明显细化，最终成功发掘得到具有极高的硬度和强度的Ti-Mn合金，这充分证明了增材制造高通量制备和表征手段在快速探索材料成分区间，控制钛合金微观结构方面的独特优势。引入新元素调控成分过冷，结合增材制造高通量制备技术对钛合金成分大范围探索，有望解决钛合金难以获得精细的等轴晶结构问题。

图5

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图5   增材制造Ti6Al4V合金和Ti-8.5Cu合金的微观组织形貌、晶粒长大机理示意图以及增材制造Ti-Cu合金拉伸性能曲线[38]

Fig.5   Microstructure morphologies of Ti6Al4V (a) and Ti-8.5Cu (b) alloys, and grain growth mechanism of additive manufactured Ti6Al4V alloy and Ti-8.5Cu alloy, and tensile property curves of additive manufactured Ti-Cu alloy (c)[38] (Inset in Fig.5b shows the high magnified image of equiaxed grain structure. Inset in Fig.5c shows Ti-8.5Cu alloy has higher constitutional supercooling ability. CS—constitutional supercooling, TA—melt temperature, TE—equilibrium liquidus temperature, ΔTCS—amount of constitutional supercooling in front of the growing solid that provides the nucleation undercooling, ΔTn—critical undercooling for nucleation. ΔTCS(= TE- TA) and the value of ΔTn is qualitatively represented by the length bar, and the gray shape represents the grain morphology of the alloy)


1.3 钢材的异质结构设计

钢材作为最古老应用的金属材料，也是最早通过增材制造实现打印的金属材料，具有高强度和良好的延展性，以及出色的耐磨性和耐腐蚀性[41]。钢材中不同的基体组织(奥氏体、铁素体、马氏体)和各种沉淀相(金属间沉淀物、碳化物)决定这类合金的微观组织和性能，增材制造通过改变热过程来控制材料组织结构演变，而高冷却速率的增材制造钢形成了与传统加工显著不同的微观结构和性能[42]。目前，增材制造钢材主要有奥氏体不锈钢、工具钢、铁素体不锈钢和双相钢等，从成分角度来讲它们随着铁素体稳定元素Cr和奥氏体稳定元素Ni含量的不同，主要形成4种结构，如图6[43~46]所示。铁素体和奥氏体不锈钢中具有高Cr元素含量以保证其耐腐蚀性，不含奥氏体稳定元素的铁素体不锈钢，室温下通常为铁素体或铁素体/马氏体结构，而奥氏体不锈钢中高Ni含量使其奥氏体结构得以稳定保留。铁素体不锈钢在增材制造过程中形成细小的晶粒尺寸，同时伴有均匀分布的纳米颗粒或氧化物沉淀[42,47] (图6a[43])，而增材制造奥氏体不锈钢具有精细的异质结构、高位错密度、特殊亚结构、大角度晶界以及显著的元素偏析的综合结构[48~51] (图6b[44])。马氏体钢通常具有少量的Cr元素，如马氏体时效钢和含碳工具钢，它们最终使用的显微组织均为带有沉淀物的马氏体相[52]。高Ni含量的马氏体时效钢形成大量的残余奥氏体，具有优异的延展性，而高C含量的工具钢中由于碳化物的析出表现为硬脆的马氏体显微组织，在热应力作用下更容易产生开裂。马氏体时效钢和含碳工具钢在凝固过程中均通过微观偏析使合金元素富集在枝晶间，形成与传统加工方式截然不同的蜂窝状/树枝状凝固微观结构[45,53] (图6c[45]和d[46])，成分对最终结构的影响为材料的设计提供了更多的可能。

图6

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图6   增材制造钢中主要组成元素和微观结构的变化[43~46]

Fig.6   Changes of element composition (mass fraction, %) and microstructure of additive manufactured steel

(a) ferritic stainless steel[43] (b) austenitic stainless steel[44]

(c) maraging steel[45] (d) carbon-containing tool steel H13[46]


异质结构(HS)材料是一种由结构不均匀或物理性质显著差异的区域构成的材料，例如具有第二相颗粒和多相的钢和合金，通过异质区域间的协调配合，具有显著的异质变形诱导强化作用[54]。异质结构通常导致各区域力学性能的显著差异，传统工艺通常不允许这种非均质结构的产生，而在增材制造材料中它被认为是一种有效的强化手段，在受控结构的协调配合作用下显现出惊人的力学性能[54]。双相不锈钢(duplex stainless steel，DSS)由近等比例的α铁素体相和γ奥氏体相组成，同时兼具优异的强韧性和耐腐蚀特性[55]。增材制造双相不锈钢通常要先在常温获得完全铁素体结构，经过高温热处理(1100℃)和快速冷却来获得所需的双相结构[56,57]，而这种方式获得的双相钢两相组成和结构难以有效控制，无法通过异质结构进一步发掘材料性能潜力。研究[58]发现，作为奥氏体稳定元素，Ni的添加有望解决双相钢受控异质结构问题，Li等[58]将22Cr双相钢粉与6%Ni混合，在新的成分下通过激光粉末床融合(LPBF)技术获得受控双相结构，成功构建出近等比双相钢(new duplex steel) (图7a[58])。Li等[58]还在报道中表明，在触发bcc相向fcc相过渡的临界Ni含量下定制打印参数能够有效控制相组成，而这为双相钢甚至其他多相材料个性化异质结构的增材制造提供了一个新的思路，在相变影响元素的临界成分点，仅通过不同层打印参数的控制就能够实现材料的层间结构异质。在传统的锻造状态下，马氏体时效钢基体中形成均匀分布的精细沉淀相，但打印工艺下沉淀析出效果却不尽人意，尽管本征热处理诱导沉淀析出，但存在大量残余奥氏体，致使强度不能满足人们的需求。Kürnsteiner等[15]通过添加5%Ti优化马氏体时效钢Fe20Ni合金成分，并结合定向能量沉积(DED)工艺特点制备出具有分层析出结构的新型大马士革钢(new Damascus steel) (图7b[15])，分层结构由无纳米沉淀物软化区和含有大量NiTi纳米沉淀物的硬化区组成，软硬区域交替的层状异质结构使其性能显著提升，拉伸强度高达1.3 GPa。Li等[58]和Kürnsteiner等[15]利用增材制造技术精确的微观调控能力，实现了独特的结构和优异的力学性能，不难发现无论是临界Ni含量又或是Ti成分的选择对于层状异质结构的形成都十分关键，如影响双相钢相变的(10.0%~10.3%)临界Ni含量和马氏体时效钢Fe20Ni中5%的Ti含量，通过传统试错模式获得影响结构演变的关键成分点，对于材料设计而言不仅消耗大量的成本，也难以获得准确的关键成分。利用材料基因工程思想，通过增材制造高通量制备和表征技术快速筛选成分区间，例如高通量制备和表征Fe20Ni(0~5)Ti，可以更快更准确地得到影响结构演变的关键成分，这种方法推广到其他具有复杂相组成的材料中，有望实现增材制造多相材料宏观异质结构个性化控制，使材料性能得到进一步提升，如图7c[46,48~50,56,58~73]中未来双相钢性能的发展趋势所示。Nie等[74]利用高通量增材制造制备出具有成分连续变化的SS316L-SS431不锈钢，通过高通量表征发现相结构伴随着材料成分梯度变化而连续变化，并筛选出所需的组织结构及最佳性能的不锈钢材料(图7d~g[74])。

图7

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图7   新型双相钢及新型大马士革钢微观结构，增材制造钢性能范围和未来双相钢性能趋势，以及增材制造梯度不锈钢高通量表征和分析[15,46,48~50,56,58~74]

Fig.7   Microstructures of new duplex steel (a)[58] and new Damascus steel (b)[15], performance range of additive manufacturing steel and future performance trend of dual-phase steel (c)[46,48~50,56,58~73], and high-throughput characterization and analysis of additive manufactured gradient stainless steel: microstructures (d), XRD spectra (e), phase composition ratio (f), and hardness curve (g) of SS431-SS316L composition gradient stainless steel (All show a continuous change trend with the change of composition gradient)[74]


2 高通量增材制造制备与表征

目前材料高通量制备技术包括扩散多元结、气相沉积、等离子喷涂、螺旋梯度连铸以及增材制造等，目的是为了获得成分连续变化或离散的组合材料，增材制造因其制备速度快、能耗低、材料利用率高和自下而上逐层制造的特点而被广泛用于制备成分梯度材料(梯度功能材料)。目前用于制备成分梯度材料的2种方法是DED和SLM技术[75]，工艺原理如图8a~c[12,76,77]所示。在DED中，控制不同粉末流速就能实现块状材料成分纵向梯度变化[12]，而在SLM中，通过层间换粉[76]和斜料斗混料[77]的方法同样能够实现块状材料成分梯度变化，不同的是层间换粉SLM梯度试样成分沿纵向阶梯变化，而斜料斗混料SLM梯度试样成分沿水平方向连续变化，水平梯度试样具有更大的成形空间，其构件成分变化平缓，有利于缓解温度梯度在不同位置带来的影响，改善内应力，使零件成分更加稳定，结构更加致密[13]，梯度试样比较如图8d~f[12,13,76]所示。高通量表征技术包括高通量X射线衍射(XRD)、高通量硬度测试、高通量扫描电镜(SEM)和背散射衍射(EBSD)等等，可以迅速获取大量成分特征离散变化试样或梯度连续变化试样的材料及性能信息(图8g[78]和h[13])。目前高通量表征手段仍基于离散的成分特征区域进行表征，开发适用于梯度成分连续表征的技术，对提高增材制造材料开发效率十分重要。

图8

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图8   梯度材料制备原理示意图、梯度试样比较以及常见的高通量表征方法[12,13,76~78]

Fig.8   Schematics of gradient material preparation principle of directed energy deposition (DED) (a)[12], selective laser melting (SLM) interlayer powder exchange (b)[76], SLM inclined hopper powder mixing process (c)[77], and their sample comparison (d-f)[12,13,76]; and the common high-throughput analysis methods characterization of the structure of gradient samples (atomic fraction) by high-throughput SEM (g)[78] and characterization of phase composition of gradient samples by high-throughput XRD (h)[13] (Inset in Fig.8e shows the gradient transition of the material. FGM—functionally graded material)


3 总结和展望

增材制造技术发展迅速，传统材料和数据库不适用制约了增材制造材料的开发和应用，增材制造相较于传统高通量制备方式具有快速成型、可制备连续梯度或微米级离散试样的特点，在高通量制备方面表现突出。本文从材料成分角度，总结了增材制造材料的发展现状和关键问题，展示了高通量增材制造技术在材料成分优化、新合金材料制备和开发以及成分组织结构研究等方面的巨大应用潜力，但目前仍面对以下几个急需解决的问题。

(1) 增材制造可控梯度变化提供比离散样品更丰富的信息，而目前高通量表征手段仍采用一些离散区域进行表征，测试区域受限于表征手段的采样区域的大小且成分变化影响性能表征准确性，无法做到完全梯度连续变化性能的准确表征。提高表征手段的精度，建立准确的梯度连续的表征方法仍是一种挑战。

(2) 增材制造材料通常表现出优异的性能，但由于可打印材料种类的限制影响了部分材料在增材制造高通量制备和表征上的应用。实现性质差异较大的材料致密完美地打印出来，并形成连续可靠的梯度过渡仍具有挑战。

(3) 增材制造过程中的气孔等缺陷问题显著影响着材料的性能，不同成分的合金增材制造工艺参数往往并不一致，在一定程度上这也增大了增材制造梯度材料制备的复杂性。建立材料成分-结构-性能的可靠联系仍具有挑战。

尽管增材制造高通量制备和表征在材料设计上还面临着巨大的挑战，但事实已经证明它在材料成分设计方面的巨大前景。材料方面，通过高通量增材制造技术有望解决增材制造新合金材料析出相控制问题、等轴晶结构成形问题以及层间异质结构设计问题，开发新一代增材制造合金材料，通过微观到宏观的整体设计，充分发掘增材制造材料性能潜力，实现航空航天领域关键零部件材料性能的进一步提升。技术方面，发展高通量增材制造新工艺、发掘增材制造新材料，不断完善梯度材料表征手段，实现精确、高效、稳定的高通量表征能力，有望建立起材料成分-结构与性能的可靠联系的增材制造材料基因数据库，实现增材制造新材料的高效发掘。

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[Figure: see text].

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Many traditional approaches for strengthening steels typically come at the expense of useful ductility, a dilemma known as strength-ductility trade-off. New metallurgical processing might offer the possibility of overcoming this. Here we report that austenitic 316L stainless steels additively manufactured via a laser powder-bed-fusion technique exhibit a combination of yield strength and tensile ductility that surpasses that of conventional 316L steels. High strength is attributed to solidification-enabled cellular structures, low-angle grain boundaries, and dislocations formed during manufacturing, while high uniform elongation correlates to a steady and progressive work-hardening mechanism regulated by a hierarchically heterogeneous microstructure, with length scales spanning nearly six orders of magnitude. In addition, solute segregation along cellular walls and low-angle grain boundaries can enhance dislocation pinning and promote twinning. This work demonstrates the potential of additive manufacturing to create alloys with unique microstructures and high performance for structural applications.

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Process parameters (laser power and scanning speed) for H13 steel specimens produced by selective laser melting (SLM) are optimized, and microstructural characteristics and mechanical properties are investigated. The optimum process parameters are a laser power of 170 W and a scanning speed of 400 mm/s according to the maximum relative density of 99.2%. The microstructure consists of cellular grains and columnar crystal, which are composed of lath martensite and retained austenite, and there are no carbides or other second-phase particles present. The size of cellular grains is 1 mu m. Compared with the common processed (forged and heat-treated) H13, SLM H13 has similar microhardness (561 HV) and tensile strength (1909 MPa) values. However, the elongation (12.4%) is a factor of similar to 3 times higher and the impact energy (14.4 J) of the SLM specimen is somewhat lower. The relationship between the microstructure and mechanical properties is discussed. Fine grains and no second-phase precipitation determine the strength and plasticity of SLM samples.

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In the present review, attempts have been made to analyze the metallurgical, mechanical, and corrosion properties of commercial marine alloy duplex stainless steel AISI 2205 with special reference to its weldability, machinability, and surfacing. In the first part, effects of various fusion and solid-state welding processes on joining DSS 2205 with similar and dissimilar metals are addressed. Microstructural changes during the weld cooling cycle such as austenite reformation, partitioning of alloying elements, HAZ transformations, and the intermetallic precipitations are analyzed and compared with the different welding techniques. In the second part, machinability of DSS 2205 is compared with the commercial ASS grades in order to justify the quality of machining. In the third part, the importance of surface quality in a marine exposure is emphasized and the enhancement of surface properties through peening techniques is highlighted. The research gaps and inferences highlighted in this review will be more useful for the fabrications involved in the marine applications.

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DOI     

This experimental study investigates the combined effect of the three primary Additive Manufacturing (AM) build orientations (0 degrees, 45 degrees, and 90 degrees) and an extensive array of heat treatment plans on the plastic anisotropy of maraging steel 300 (MS1) fabricated on the EOSINT M280 Direct Metal Laser Sintering (DMLS) system. The alloys microstructure, hardness, tensile properties and plastic strain behaviour have been examined for various strengthening heat-treatment plans to assess the influence of the time and temperature combinations on plastic anisotropy and mechanical properties (e.g. strength, ductility). A comprehensive visual representation of the material's overall mechanical properties, for all three AM build orientations, against the various heat treatment plans is offered through time - temperature contour maps. Considerable plastic anisotropy has been confirmed in the as-built condition, which can be reduced by aging heat-treatment, as verified in this study. However, it has identified that a degree of transverse strain anisotropy is likely to remain due to the AM alloys fabrication history, a finding that has not been previously reported in the literature. Moreover, the heat treatment plan (6h at 490 degrees C) recommended by the DMLS system manufacturer has been found not to be the optimal in terms of achieving high strength, hardness, ductility and low anisotropy for the MS1 material. With the use of the comprehensive experimental data collected and analysed in this study, and presented in the constructed contour maps, the alloys heat treatment parameters (time, temperature) can be tailored to meet the desired strength/ductility/anisotropy design requirements, either for research or part production purposes.

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As a key component of active phased array radar, the size and performance of T/R (Transmitter and Receiver) components determine the weight and function of the equipment. Wire bonding is one of the commonly used interconnection technologies in T/R components. With the improvement of component integration, it is necessary to develop corresponding high-density wire bonding technologies, which is essential for the miniaturization of bonding wires. However, ultra-fine leads will reduce the mechanical properties and reliability of the solder joints. Ultrasonic hot-press wedge bonding method is used to realize the connection of ultra-fine gold wire and gold pad, and the process parameters are optimized. The results show that with the increase of bonding pressure, bonding time and ultrasonic power, the wire deformation after bonding gradually increases, while the tension of the gold wire after bonding first increases and then decreases. And the influence of process parameters on the deformation of gold ribbon is less than that of gold wire. The excessive force of the second bonding point causes the lead deformation to be larger and the maximum tensile force is less than the first bonding point. Therefore, the number of bonding points needs to be increased. Finally, the best bonding process parameters of the gold wire and gold pad are obtained through the orthogonal experiment method. The bonding of ultra-fine size leads is realized, which is of great significance to the miniaturization of T/R components.

李祺祺, 温耀杰, 张百成 等.

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[J]. 机械工程学报, 2021, 57: 184

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梯度功能材料是由两种或多种材料复合且成分呈连续梯度变化的一种新型复合材料，在当今飞速发展的工程领域受到了广泛的关注。但传统的梯度功能材料制备技术无法满足航空、医疗、军事等工业领域的需要。而增材制造作为一种新兴技术，提供了一种全新的思路来解决梯度功能材料的制备问题。系统总结了增材制造制备梯度功能合金的主要方法，讨论了利用激光熔覆与选区激光熔化技术制备钛基、铁基及金属-陶瓷等梯度合金的研究现状及在相应领域的重要应用，并结合现有工作论述利用选区激光熔化制备连续梯度功能合金的原理与研究进展，最后阐述了利用增材制造技术制备梯度功能合金的挑战和机遇，并展望了本领域的未来发展方向。

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