技术领域technical field
本发明属于增材制造及粉末冶金技术领域，更具体地，涉及一种高性能7050 铝合金3D打印选区激光熔化成形件及其应用。The invention belongs to the technical field of additive manufacturing and powder metallurgy, and more particularly relates to a high-performance 7050 aluminum alloy 3D printing selective laser melting forming part and its application.
背景技术Background technique
3D打印技术，也被称为增材制造技术，被誉为“第三次工业革命”的核心技术。主要包含四种成型方式，选择性激光烧结(SLS)、电子束熔融(EBM)、选区激光熔化(SLM)、和激光近净成形(LENS)，其中研究的重点是选区激光熔化 (SLM)。3D printing technology, also known as additive manufacturing technology, is hailed as the core technology of the "third industrial revolution". It mainly includes four forming methods, Selective Laser Sintering (SLS), Electron Beam Melting (EBM), Selective Laser Melting (SLM), and Laser Near Net Shaping (LENS), among which the research focuses on Selective Laser Melting (SLM).
2011年，德国埃朗根-纽伦堡弗里德里希·亚历山大大学进行了7系了合金 3D打印SLM单道成形报道，证明了其可行性；In 2011, Friedrich Alexander University Erlangen-Nuremberg, Germany conducted a report on the single-pass forming of alloy 3D printing SLM in 7 series, which proved its feasibility;
随后，德国汉堡工业大学Kaufmann N,Imran M,Wischeropp T M等就SLM 工艺参数对7075铝合金成形质量的影响展开了研究，通过优化参数，如调整激光功率、扫描方式、扫描速度、粉末厚度等最终获得了致密度达99％以上的试样[7]。然而热裂纹是一个仍待解决的问题。虽然通过增加层厚、提高预热温度、激光重熔及增大光斑直径等手段可以减少SLM成形时的热裂倾向，却无法消除。受其影响，在拉伸试验时会在热裂纹处造成应力集中，形成裂纹源，产生脆性断裂，试样近乎无延伸率。同时在Z轴方向上，受未熔合缺陷影响，室温拉伸强度不及XOY方向的四分之一。Subsequently, Kaufmann N, Imran M, Wischeropp TM, etc. of the Technical University of Hamburg, Germany, conducted research on the influence of SLM process parameters on the forming quality of 7075 aluminum alloy. By optimizing parameters, such as adjusting laser power, scanning mode, scanning speed, powder thickness, etc. A sample with a density of more than 99% was obtained[7] . However, thermal cracking is an unsolved problem. Although the tendency of hot cracking during SLM forming can be reduced by increasing the layer thickness, increasing the preheating temperature, laser remelting and increasing the spot diameter, it cannot be eliminated. Affected by it, stress concentration will be caused at the hot crack during the tensile test, forming a crack source, resulting in brittle fracture, and the sample has almost no elongation. At the same time, in the Z-axis direction, the tensile strength at room temperature is less than a quarter of that in the XOY direction due to unfused defects.
2014年，比利时鲁汶大学的Kruth团队在探究如何减少裂纹的方向上取得了进展。虽然最终成型件的致密度只有98.9％，但实现了7xxx系高强铝合金的无裂纹成形。原理是添加4wt％的粒径小于10μm的Si，与基体粉末21铝合金粉体混合后成形，通过细化晶粒，减小7075铝合金SLM成形时的热裂倾向，来达到消除其热裂纹的目的。In 2014, Kruth's team at the University of Leuven in Belgium made progress in the direction of how to reduce cracks. Although the density of the final formed part is only 98.9%, crack-free forming of 7xxx series high-strength aluminum alloys is achieved. The principle is to add 4wt% of Si with a particle size of less than 10μm, mix it with the matrix powder 21 aluminum alloy powder, and then form it. By refining the grains, the hot cracking tendency of the 7075 aluminum alloy SLM during forming is reduced, so as to eliminate its hot cracking. the goal of.
同年，国内华中科技大学武汉光电国家实验室开始了7xxx系铝合金SLM成形的研究，发现了熔池模式与热裂纹地形成与分布地关系。SLM成形的铝合金可根据工艺参数的设置，如激光能量大小、扫描方式、扫描速度、粉末厚度等和离焦量即激光焦点离作用物质的距离的设定来调整，激光交点处光斑中心的功率密度过高，容易蒸发金属液成孔，而离开激光焦点的各平面上的功率密度分布较均匀。而根据工艺参数及离焦量可大致可以分为三种熔池模式：稳定的热传导、稳定的深熔焊及过度模式。在稳定的热传导和过度模式下，热裂纹分别与沉积方向平行，几乎垂直生长及呈混乱状。这些裂纹只有通过添加微量元素才能达到消除的目的，仅仅调整优化工艺参数是无法消除的。In the same year, the Wuhan National Laboratory of Optoelectronics of Huazhong University of Science and Technology in China started the research on SLM forming of 7xxx series aluminum alloys, and found the relationship between the molten pool mode and the formation and distribution of thermal cracks. The aluminum alloy formed by SLM can be adjusted according to the setting of process parameters, such as laser energy, scanning mode, scanning speed, powder thickness, etc. and the setting of defocusing amount, that is, the distance between the laser focus and the action substance. If the power density is too high, it is easy to evaporate the molten metal to form holes, and the power density distribution on each plane leaving the laser focus is relatively uniform. According to the process parameters and the amount of defocusing, it can be roughly divided into three molten pool modes: stable heat conduction, stable deep penetration welding and transition mode. In stable thermal conduction and transition modes, thermal cracks grow parallel to the deposition direction, grow almost vertically and are chaotic, respectively. These cracks can only be eliminated by adding trace elements, which cannot be eliminated only by adjusting and optimizing process parameters.
2017年下半年，美国加州大学巴拉巴拉分校的Martin J H,Yahata B D, HundleyJ M等人通过静电组装技术，获得了均匀的混合物。粉体中的纳米ZrH2颗粒作为异质形核质点，在7050粉体表面分布均匀，起到了细化晶粒的作用。而原本具有方向性，容易导致热裂的柱状晶转化为各方向上尺寸相差较小的等轴晶，增强了抗热裂性能，降低了热裂敏感性，从而使7050高强铝合金无裂纹的 SLM成形得以实现。7系铝合金3D打印SLM成型的主要缺点在于成型时热热裂纹仅依靠优化打印参数无法消除，而添加Si后虽然通过细化晶粒的作用减小了铝合金SLM成形时的热裂纹，实现了无裂纹成形但Si作为铝合金中的杂质元素，其成形件的致密度只有98.9％，极大地影响了成形件地性能。In the second half of 2017, Martin JH, Yahata BD, HundleyJ M and others from the University of California, Barabara, obtained a homogeneous mixture through electrostatic assembly technology. The nano-ZrH2 particles in the powder, as heterogeneous nucleation particles, are evenly distributed on the surface of the 7050 powder, which plays the role of grain refinement. The columnar crystals that are originally directional and easily lead to hot cracking are transformed into equiaxed crystals with small differences in size in all directions, which enhances the resistance to hot cracking and reduces the sensitivity to hot cracking, so that the 7050 high-strength aluminum alloy has no cracks. SLM shaping is achieved. The main disadvantage of 7-series aluminum alloy 3D printing SLM molding is that thermal cracks cannot be eliminated only by optimizing the printing parameters during molding. In order to form without cracks, but as an impurity element in the aluminum alloy, the density of the formed parts is only 98.9%, which greatly affects the performance of the formed parts.
发明内容SUMMARY OF THE INVENTION
为了解决上述现有技术存在的不足和缺点，本发明的目的在于提供了一种高性能7050铝合金3D打印选区激光熔化成形件。In order to solve the above-mentioned deficiencies and shortcomings of the prior art, the purpose of the present invention is to provide a high-performance 7050 aluminum alloy 3D printing selective laser melting forming part.
本发明另一目的在于提供了上述高性能7050铝合金3D打印选区激光熔化成形件的应用。Another object of the present invention is to provide the application of the above-mentioned high-performance 7050 aluminum alloy 3D printing selective laser melting forming parts.
本发明的目的通过下述技术方案来实现：The object of the present invention is achieved through the following technical solutions:
一种高性能7050铝合金3D打印选区激光熔化成形件，所述成形件是先将 Ta粉和过筛的7050铝合金粉末混合；再采用单激光器打印，激光器功率为 450～500W，预热温度为200～250℃，在基板上打印，得到含Ta的7050铝合金件；最后使用切割机将含Ta的7050铝合金件从基板上切下制得。A high-performance 7050 aluminum alloy 3D printing selective laser melting forming part. The forming part is firstly mixed with Ta powder and sieved 7050 aluminum alloy powder; At a temperature of 200-250° C., print on the substrate to obtain a Ta-containing 7050 aluminum alloy part; finally, use a cutting machine to cut the Ta-containing 7050 aluminum alloy part from the substrate to obtain it.
优选地，所述筛的孔径为45～90μm。Preferably, the aperture of the sieve is 45-90 μm.
优选地，所述Ta粉和7050铝合金粉末的质量比为1：(15～49)。Preferably, the mass ratio of the Ta powder and the 7050 aluminum alloy powder is 1:(15-49).
优选地，所述混合的时间为1～2h。Preferably, the mixing time is 1-2 hours.
优选地，所述含Ta的7050铝合金件的孔隙率为5～7％。Preferably, the porosity of the Ta-containing 7050 aluminum alloy part is 5-7%.
所述的高性能7050铝合金3D打印选区激光熔化成形件在粉末冶金及增材制造领域中的应用。The application of the high-performance 7050 aluminum alloy 3D printing selective laser melting forming part in the field of powder metallurgy and additive manufacturing.
本发明高强铝合金因其热裂敏感性高而不易3D打印成形，而相对于柱状晶，细小均匀的等轴晶结构可以容纳更多应变防止热裂。在获取细小等轴晶的方法中，最常用的手段是晶粒细化，而在原有合金体系中引入合金元素使其生成异质形核核心是一种有效的晶粒细化方法。本发明选用Ta元素作为异质形核剂3D打印7050铝合金，并通过光学显微镜、扫描电镜、X射线衍射、显微硬度计等分析测试手段来研究Ta对3D打印7050铝合金组织和性能的影响。结果表明，相对于3D打印7050铝合金，Ta元素的引入可提高合金的致密度，降低热裂敏感性，显著细化晶粒，提高硬度，增强耐腐蚀性。其主要原因是在3D打印过程中，Ta能与Al反应生成300-500nm的Al3Ta作为Al的异质形核核心细化晶粒，使7050-Ta铝合金具有细小均匀的等轴晶结构，这种结构能显著减少热裂纹，并产生细晶强化作用。此外，弥散分布的Al3Ta能减缓合金的浸泡腐蚀速率。The high-strength aluminum alloy of the present invention is not easy to be formed by 3D printing due to its high sensitivity to thermal cracking, and compared with columnar crystals, the fine and uniform equiaxed crystal structure can accommodate more strains to prevent thermal cracking. Among the methods for obtaining fine equiaxed grains, the most commonly used method is grain refinement, and the introduction of alloying elements into the original alloy system to generate heterogeneous nucleation cores is an effective method for grain refinement. In the present invention, Ta element is used as a heterogeneous nucleating agent to 3D print 7050 aluminum alloy, and the effect of Ta on the structure and performance of 3D printed 7050 aluminum alloy is studied by optical microscope, scanning electron microscope, X-ray diffraction, microhardness tester and other analysis and testing methods. influences. The results show that, compared with 3D printing 7050 aluminum alloy, the introduction of Ta element can improve the density of the alloy, reduce the sensitivity to hot cracking, significantly refine the grains, improve the hardness, and enhance the corrosion resistance. The main reason is that in the 3D printing process, Ta can react with Al to form Al3 Ta of 300-500 nm as the heterogeneous nucleation core of Al to refine the grains, so that the 7050-Ta aluminum alloy has a fine and uniform equiaxed crystal structure. , this structure can significantly reduce hot cracks and produce fine-grain strengthening. In addition, the dispersed Al3 Ta can slow down the immersion corrosion rate of the alloy.
与现有技术相比，本发明具有以下有益效果：Compared with the prior art, the present invention has the following beneficial effects:
1.本发明通过添加合金元素Ta作为异质形核剂，来降低7系高强铝合金 SLM成型时的热裂敏感性，消除裂纹，降低孔隙率，提高成形件的性能。Ta作为添加剂运用到铝合金的成形中时，会形成硬质相，作为核心被Al包裹，对铝合金基体起强化作用。1. In the present invention, by adding alloying element Ta as a heterogeneous nucleating agent, the hot crack sensitivity of 7 series high-strength aluminum alloy SLM is reduced, cracks are eliminated, porosity is reduced, and the performance of the formed parts is improved. When Ta is used as an additive in the forming of aluminum alloys, it will form a hard phase, which is wrapped by Al as the core and strengthens the aluminum alloy matrix.
2.本发明在成形过程中，Ta与Al会形成Al3Ta。这是一种新型的高温结构材料，在7050铝合金SLM成形时会起到细化晶粒及固溶强化的作用，从而减小热烈倾向，提高致密度，降低孔隙率，提升试样性能。2. During the forming process of the present invention, Ta and Al will form Al3 Ta. This is a new type of high-temperature structural material, which will play the role of grain refinement and solid solution strengthening when 7050 aluminum alloy SLM is formed, thereby reducing the thermal tendency, increasing the density, reducing the porosity, and improving the performance of the sample.
附图说明Description of drawings
图1为实施例1中粉末形貌及成分：(a，c)Ta粉，(b，d)7050铝合金粉。Figure 1 shows the powder morphology and composition in Example 1: (a, c) Ta powder, (b, d) 7050 aluminum alloy powder.
图2为对比例1中7050(a)和实施例1中7050-Ta(b,c)试样的金相。Figure 2 shows the metallographic phase of the 7050(a) in Comparative Example 1 and the 7050-Ta(b,c) sample in Example 1.
图3为实施例1中调整阈值后用灰度显示的孔隙率图。FIG. 3 is a porosity graph displayed in grayscale after threshold adjustment in Example 1. FIG.
图4为实施例1中7050-Ta和对比例1中的7050试样的X衍射图谱。4 is the X-ray diffraction pattern of the 7050-Ta in Example 1 and the 7050 sample in Comparative Example 1.
图5为对比例1中7050和实施例1中7050-Ta试样的EBSD图像及晶粒尺寸分布。5 is the EBSD image and grain size distribution of the 7050 in Comparative Example 1 and the 7050-Ta sample in Example 1.
图6为实施例1中3D打印7050-Ta铝合金的微观形貌。FIG. 6 shows the microstructure of the 3D printed 7050-Ta aluminum alloy in Example 1.
图7为实施例1中7050-Ta显微硬度直方图。FIG. 7 is a microhardness histogram of 7050-Ta in Example 1. FIG.
图8为对比例1中7050铝合金试样腐蚀后金相(a、b)和实施例1中7050-Ta 铝合金试样腐蚀后金相(c、d)。Figure 8 shows the metallographic phase (a, b) of the 7050 aluminum alloy sample in Comparative Example 1 after corrosion and the metallographic phase (c, d) of the 7050-Ta aluminum alloy sample in Example 1 after corrosion.
图9为实施例1中的7050-Ta和对比例1中7050试样腐蚀后的截面形貌。9 is the cross-sectional morphology of the 7050-Ta in Example 1 and the 7050 sample in Comparative Example 1 after corrosion.
具体实施方式Detailed ways
下面结合具体实施例进一步说明本发明的内容，但不应理解为对本发明的限制。若未特别指明，实施例中所用的技术手段为本领域技术人员所熟知的常规手段。除非特别说明，本发明采用的试剂、方法和设备为本技术领域常规试剂、方法和设备。The content of the present invention is further described below in conjunction with specific embodiments, but should not be construed as a limitation of the present invention. Unless otherwise specified, the technical means used in the examples are conventional means well known to those skilled in the art. Unless otherwise specified, the reagents, methods and equipment used in the present invention are conventional reagents, methods and equipment in the technical field.
实施例1Example 1
1.筛粉：使用筛粉机(品牌型号TURBULAT2F,220V，50Hz，0.18kW) 过筛(筛孔尺寸90μm)，可有效地防止了粉末粒度不符的情况出现，并且将部分由于运输等原因造成的粘连团聚的粉末筛分掉，基本上去除了因粉末粒度等因素导致的SLM成形时的不理想情况出现的可能性。1. Sieve powder: Use a sieving machine (brand model TURBULAT2F, 220V, 50Hz, 0.18kW) to sieve (sieve size 90μm), which can effectively prevent the inconsistency of powder particle size, and will be partially caused by transportation and other reasons. The cohesive and agglomerated powder is screened out, which basically removes the possibility of undesired conditions during SLM molding caused by factors such as powder particle size.
2.混粉：按照2wt％Ta粉和98wt％7050铝合金粉末，使用三维摇摆式粉末混合机混1-2h至混匀。2. Mixing powder: According to 2wt% Ta powder and 98wt% 7050 aluminum alloy powder, use a three-dimensional rocking powder mixer to mix for 1-2h until uniform.
3.打印：打印所用设备型号为(铂力特metal additive manufacture machineS200。单激光器，激光器功率：500W；基板尺寸：105mm×105mm；预热温度： 250℃)、打印参数为激光功率210W，扫描速度165mm/s，其他打印参数如表表2所示，试样编号(对应编号1～6实例1～6)如表3所示。3. Printing: The model of the equipment used for printing is (BLT metal additive manufacture machineS200. Single laser, laser power: 500W; substrate size: 105mm×105mm; preheating temperature: 250℃), the printing parameters are laser power 210W, scanning speed 165mm/s, other printing parameters are shown in Table 2, and the sample numbers (corresponding to numbers 1 to 6, examples 1 to 6) are shown in Table 3.
4.打印完后使用电火花切割机从基板上切下，测试相应的性能。4. After printing, use an EDM cutting machine to cut it from the substrate to test the corresponding performance.
实施例2Example 2
与实施例1不同的在于：所述Ta粉和7050铝合金粉末的质量比为1：49，打印参数为激光功率310W，扫描速度165mm/s。The difference from Example 1 is that the mass ratio of the Ta powder and the 7050 aluminum alloy powder is 1:49, the printing parameters are the laser power 310W, and the scanning speed 165mm/s.
实施例3Example 3
与实施例1不同的在于：所述Ta粉和7050铝合金粉末的质量比为1：24，打印参数为激光功率210W，扫描速度115mm/s。The difference from Example 1 is that the mass ratio of the Ta powder and the 7050 aluminum alloy powder is 1:24, the printing parameters are the laser power 210W, and the scanning speed 115mm/s.
实施例4Example 4
与实施例1不同的在于：所述Ta粉和7050铝合金粉末的质量比为1：24，打印参数为激光功率210W，扫描速度165mm/s。The difference from Example 1 is that the mass ratio of the Ta powder and the 7050 aluminum alloy powder is 1:24, the printing parameters are the laser power 210W, and the scanning speed 165mm/s.
实施例5Example 5
与实施例1不同的在于：所述Ta粉和7050铝合金粉末的质量比为1：10，打印参数为激光功率260W，扫描速度115mm/s。The difference from Example 1 is that the mass ratio of the Ta powder and the 7050 aluminum alloy powder is 1:10, the printing parameters are the laser power 260W, and the scanning speed 115mm/s.
实施例6Example 6
与实施例1不同的在于：所述Ta粉和7050铝合金粉末的质量比为3：47，打印参数为激光功率260W，扫描速度165mm/s。The difference from Example 1 is that the mass ratio of the Ta powder and the 7050 aluminum alloy powder is 3:47, the printing parameters are the laser power 260W, and the scanning speed 165mm/s.
对比例1Comparative Example 1
1.筛粉：使用筛粉机(品牌型号TURBULAT2F,220V，50Hz，0.18kW) 过筛(筛孔尺寸90μm)，可有效地防止了粉末粒度不符的情况出现，并且将部分由于运输等原因造成的粘连团聚的粉末筛分掉，基本上去除了因粉末粒度等因素导致的SLM成形时的不理想情况出现的可能性。1. Sieve powder: Use a sieving machine (brand model TURBULAT2F, 220V, 50Hz, 0.18kW) to sieve (sieve size 90μm), which can effectively prevent the inconsistency of powder particle size, and will be partially caused by transportation and other reasons. The cohesive and agglomerated powder is screened out, which basically removes the possibility of undesired conditions during SLM molding caused by factors such as powder particle size.
2.打印：将7050铝合金粉末，使用三维摇摆式粉末1-2h至混匀。打印所用设备型号为(铂力特metal additive manufacture machine S200。单激光器，激光器功率：500W；基板尺寸：105mm×105mm；预热温度：250℃)，打印参数为激光功率210W，扫描速度165mm/s，其他打印参数如表2所示。2. Printing: Mix 7050 aluminum alloy powder with three-dimensional rocking powder for 1-2 hours. The model of the equipment used for printing is (BLT metal additive manufacture machine S200. Single laser, laser power: 500W; substrate size: 105mm×105mm; preheating temperature: 250℃), the printing parameters are laser power 210W, scanning speed 165mm/s , and other printing parameters are shown in Table 2.
3.打印完后使用电火花切割机从基板上切下，测试相应的性能。3. After printing, use an EDM cutting machine to cut it from the substrate to test the corresponding performance.
对比例2Comparative Example 2
与对比例1不同的在于：打印参数为激光功率310W，扫描速度165mm/s。The difference from Comparative Example 1 is that the printing parameters are the laser power of 310W and the scanning speed of 165mm/s.
对比例3Comparative Example 3
与对比例1不同的在于：打印参数为激光功率210W，扫描速度115mm/s。The difference from Comparative Example 1 is that the printing parameters are the laser power of 210W and the scanning speed of 115mm/s.
对比例4Comparative Example 4
与对比例1不同的在于：打印参数为激光功率210W，扫描速度165mm/s。The difference from Comparative Example 1 is that the printing parameters are the laser power of 210W and the scanning speed of 165mm/s.
对比例5Comparative Example 5
与对比例1不同的在于：打印参数为激光功率260W，扫描速度115mm/s。The difference from Comparative Example 1 is that the printing parameters are the laser power of 260W and the scanning speed of 115mm/s.
对比例6Comparative Example 6
与对比例1不同的在于：打印参数为激光功率260W，扫描速度165mm/s。The difference from Comparative Example 1 is that the printing parameters are the laser power of 260W and the scanning speed of 165mm/s.
打印所使用的粉末为45μm的椭球形Ta粉和粒度为90μm的球形7050铝合金粉末，相应的粉末形貌图及元素含量如表1和图1所示：The powders used for printing are 45μm ellipsoidal Ta powder and 90μm spherical 7050 aluminum alloy powder. The corresponding powder morphology and element content are shown in Table 1 and Figure 1:
表1粉体材料元素组成及含量Table 1 Elemental composition and content of powder materials
表2打印参数Table 2 Printing Parameters
表3实施例1-6试样标号Table 3 Examples 1-6 Sample Nos.
表47050-Ta试样的孔隙率Table 47050-Ta Sample Porosity
图2为对比例1中7050(a)及实施例1中7050-Ta(b,c)试样的金相。在同样的打印参数下，未添加Ta的7050铝合金粉末选区激光熔化成形件的致密度仅为88.6±6％，孔隙尺寸较大，裂纹扩展严重，如图2中(a)所示。受力时容易在孔隙及裂纹处造成应力集中，将其作为裂纹源扩展，降低铝合金件的抗拉强度、延伸率等力学性能。如果作为机械零件，其力学性能及可靠性基本不可能达标。同时孔隙增加了铝合金件与外界接触的表面积，并且孔隙中的氧化皮难以去除，容易形成点腐蚀的孔洞，并在腐蚀时作为均匀分布的质点，和试样表面形成一定电位差，加快试样表面的面腐蚀，加快腐蚀速率。提高了工件对制造、储存及使用过程中对工况及维护的要求，增加生产及维护成本，降低可靠性及使用寿命。从图2中(b、c)可知，7050-Ta试样的热裂纹较少，说明添加Ta可降低 7050铝合金SLM成形件的热裂倾向，提高致密度。Figure 2 shows the metallographic phase of the 7050(a) in Comparative Example 1 and the 7050-Ta(b,c) sample in Example 1. Under the same printing parameters, the density of 7050 aluminum alloy powder selective laser melting forming parts without Ta addition is only 88.6±6%, the pore size is large, and the crack propagation is serious, as shown in Fig. 2(a). When stressed, it is easy to cause stress concentration at pores and cracks, which are used as crack sources to expand, reducing the mechanical properties of aluminum alloy parts such as tensile strength and elongation. If it is used as a mechanical part, its mechanical properties and reliability are basically impossible to meet the standards. At the same time, the pores increase the surface area of the aluminum alloy parts in contact with the outside world, and the oxide scale in the pores is difficult to remove, which is easy to form pitting holes, and acts as uniformly distributed particles during corrosion, forming a certain potential difference with the surface of the sample, speeding up the test. The surface corrosion of the sample surface accelerates the corrosion rate. It improves the working conditions and maintenance requirements of workpieces in the process of manufacturing, storage and use, increases production and maintenance costs, and reduces reliability and service life. It can be seen from Figure 2 (b, c) that the 7050-Ta sample has less hot cracks, indicating that adding Ta can reduce the hot cracking tendency of 7050 aluminum alloy SLM forming parts and improve the density.
图3为实施例1中调整阈值后用灰度显示的孔隙率图。添加Ta的打印件孔隙率有了较大的改善(表4)。从图3中可知，7050-Ta试样平均孔隙率在5～8％之间，最低可达到2.59％。说明添加Ta可降低7050铝合金SLM成形件的孔隙率。FIG. 3 is a porosity graph displayed in grayscale after threshold adjustment in Example 1. FIG. The porosity of the prints with the addition of Ta showed a larger improvement (Table 4). It can be seen from Figure 3 that the average porosity of the 7050-Ta sample is between 5 and 8%, and the minimum can reach 2.59%. It shows that adding Ta can reduce the porosity of 7050 aluminum alloy SLM parts.
图5为对比例1中7050及实施例1中7050-Ta试样的EBSD图像及晶粒尺寸分布图。由图5中(a)可以看出，3D打印7050铝合金的晶粒不规则且粗大，并具有柱状晶结构，热裂纹沿晶界分布，平均晶粒尺寸为74.9μm。图5中(b) 的3D打印7050-Ta铝合金则具有细小均匀的等轴晶结构，平均晶粒尺寸仅为 4.5μm，表明Ta的异质形核晶粒细化效果显著。5 is an EBSD image and a grain size distribution diagram of the 7050 in Comparative Example 1 and the 7050-Ta sample in Example 1. It can be seen from (a) in Figure 5 that the grains of the 3D printed 7050 aluminum alloy are irregular and coarse, and have a columnar grain structure. The thermal cracks are distributed along the grain boundaries, and the average grain size is 74.9 μm. The 3D printed 7050-Ta aluminum alloy in Figure 5(b) has a fine and uniform equiaxed grain structure with an average grain size of only 4.5 μm, indicating that the heterogeneous nucleation grain refinement effect of Ta is remarkable.
图4为对比例1中7050和实施例1中7050-Ta试样的X射线衍射图，通过对材料进行X射线衍射，得出的衍射图谱中，7050-Ta的试样比7050试样多出了一个峰，如图4中的白点所示，按照前期的分析及预测情况，推测为Al3Ta。图6为3D打印7050-Ta铝合金的微观形貌照片，由图可知，7050-Ta具有细小均匀的等轴晶，且第二相沿晶界分布。其中，有些尺寸为300nm-500nm的颗粒存在于晶粒中心位置，经过EDX分析可知，这种颗粒的元素原子百分比是75.1％Al 和24.9％Ta，因此，这种颗粒是Al3Ta。Figure 4 is the X-ray diffraction pattern of the 7050 in Comparative Example 1 and the 7050-Ta sample in Example 1. By performing X-ray diffraction on the material, in the obtained diffraction pattern, the 7050-Ta sample is more than the 7050 sample A peak appears, as shown by the white point in Fig. 4. According to the previous analysis and prediction, it is presumed to be Al3 Ta. Figure 6 is a photo of the microscopic morphology of the 3D printed 7050-Ta aluminum alloy. It can be seen from the figure that 7050-Ta has fine and uniform equiaxed grains, and the second phase is distributed along the grain boundaries. Among them, some particles with a size of 300nm-500nm exist in the center of the grains. After EDX analysis, it can be seen that the atomic percentages of such particles are 75.1% Al and 24.9% Ta. Therefore, this particle is Al3 Ta.
选区激光熔化成形7050铝合金件在不添加Ta的情况下，平均硬度值在 76.6～80HV。而7050-Ta试样在6种打印参数条件下平均硬度值上均有小幅度的提升(图7)。这主要因为，Ta元素使7050铝合金的微观组织变为细小均匀的等轴晶结构，降低了合金的热裂敏感性，减少了成形件的裂纹，此外，在基体中弥散分布的细小均匀的Al3Ta相是硬质相，可强化合金。In the case of selective laser melting and forming of 7050 aluminum alloy parts without adding Ta, the average hardness value is 76.6-80HV. However, the average hardness of the 7050-Ta sample under the six printing parameters was slightly improved (Fig. 7). This is mainly because the Ta element changes the microstructure of the 7050 aluminum alloy into a fine and uniform equiaxed crystal structure, which reduces the hot cracking sensitivity of the alloy and reduces the cracks of the formed parts. The Al3 Ta phase is a hard phase that strengthens the alloy.
在测试硬度的过程中，不含Ta的7050试样常会出现硬度值非常小的情况，这是因为7050铝合金试样在SLM成形时致密度不够，显微硬度的压头小，在压到缺陷处时会出现极低的硬度，这也说明了致密度过低，裂纹过多，材料的性能是难以完全发挥的；与之相反的是，虽然7050-Ta的试样也有出现硬度下降的情况，但相比较而言，出现的次数很少，更多的情况是硬度增加，达到100以上。由两种试样的X射线衍射图谱可分析得出，是弥散分布在试样中的Al3Ta所导致的。当显微硬度机的压头压到硬质相Al3Ta时，其硬度便会有大幅度的上升，同时也通过其细晶强化及弥散强化机制，提高了试样的整体硬度。In the process of testing the hardness, the 7050 samples without Ta often have very small hardness values. This is because the 7050 aluminum alloy samples are not dense enough during SLM forming, and the microhardness indenter is small. There will be extremely low hardness at the defect, which also shows that the density is too low, the cracks are too many, and the performance of the material is difficult to fully exert; on the contrary, although the 7050-Ta sample also has a decrease in hardness However, in comparison, the number of occurrences is very small, and more often the hardness increases, reaching more than 100. The X-ray diffraction patterns of the two samples can be analyzed, which is caused by Al3 Ta dispersed in the samples. When the indenter of the microhardness machine is pressed to the hard phase Al3 Ta, its hardness will increase significantly, and at the same time, the overall hardness of the sample will be improved through its fine-grain strengthening and dispersion strengthening mechanisms.
图8为对比例1中7050铝合金试样腐蚀后金相(a、b)和实施例1中7050-Ta 铝合金试样腐蚀后金相(c、d)。从图8中可以看出，不加Ta的7050试样表面已被完全腐蚀，而7050-Ta试样表面较为光亮，腐蚀主要集中于孔隙附近，呈一块块的斑点分布，并未完全覆盖整个面。由此可见不含Ta的7050试样腐蚀较为严重。而对比两试样腐蚀后的截面形貌(图9)，不难看出3D打印7050铝合金中不仅有点蚀特征，还有大块连续的均匀腐蚀特征，而7050-Ta合金中只有点蚀特征，表明7050-Ta耐蚀性更好。主要原因是合金中固溶的Mg及MgZn2相的 Mg极易吸氢造成晶界上固溶氢的增加，形成氢的偏聚，使得晶界的结合能下降，形成腐蚀裂纹源。Al3Ta具有很强的耐腐蚀性，弥散分布的细小Al3Ta颗粒可阻止腐蚀裂纹的延伸及扩展。Figure 8 shows the metallographic phase (a, b) of the 7050 aluminum alloy sample in Comparative Example 1 after corrosion and the metallographic phase (c, d) of the 7050-Ta aluminum alloy sample in Example 1 after corrosion. It can be seen from Figure 8 that the surface of the 7050 sample without Ta has been completely corroded, while the surface of the 7050-Ta sample is brighter, the corrosion is mainly concentrated near the pores, and it is distributed in pieces, not completely covering the whole noodle. It can be seen that the corrosion of the 7050 sample without Ta is more serious. Comparing the cross-sectional morphologies of the two samples after corrosion (Fig. 9), it is not difficult to see that the 3D printed 7050 aluminum alloy not only has pitting features, but also has large continuous and uniform corrosion features, while the 7050-Ta alloy only has pitting features. , indicating that 7050-Ta has better corrosion resistance. The main reason is that the Mg in the solid solution in the alloy and the Mg in the MgZn2 phase are very easy to absorb hydrogen, resulting in the increase of dissolved hydrogen on the grain boundary, the formation of hydrogen segregation, the decrease of the binding energy of the grain boundary, and the formation of corrosion crack sources. Al3 Ta has strong corrosion resistance, and the dispersed fine Al3 Ta particles can prevent the extension and expansion of corrosion cracks.
上述实施例为本发明较佳的实施方式，但本发明的实施方式并不受上述实施例的限制，其他的任何未背离本发明的精神实质与原理下所作的改变、修饰、替代、组合和简化，均应为等效的置换方式，都包含在本发明的保护范围之内。The above-mentioned embodiments are preferred embodiments of the present invention, but the embodiments of the present invention are not limited by the above-mentioned embodiments, and any other changes, modifications, substitutions, combinations and The simplification should be equivalent replacement manners, which are all included in the protection scope of the present invention.
| Application Number | Priority Date | Filing Date | Title |
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| CN201910596778.6ACN110449578A (en) | 2019-07-02 | 2019-07-02 | A kind of 7050 aluminium alloy 3D printing precinct laser fusion drip molding of high-performance and its application |
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