技术领域technical field
本发明属于激光增材制造技术领域，更具体地，涉及一种基于激光增材制造的合金材料构件及其制备方法。The invention belongs to the technical field of laser additive manufacturing, and more specifically relates to an alloy material component based on laser additive manufacturing and a preparation method thereof.
背景技术Background technique
激光选区熔化技术(Selective Laser Melting，SLM)通过将三维模型转换为二维截面，采用激光束熔化特定区域的粉末，使其凝固为二维平面，最终层层堆积出整个零件。采用SLM技术无需刀具、模具、夹具即可成形任意复杂构件，可以实现复杂与精细零件的制备。然而，目前SLM制备金属材料存在着氧含量难控制问题，容易发生元素挥发及与氧结合形成冶金缺陷现象，导致成形件性能差。Selective Laser Melting (SLM) converts a three-dimensional model into a two-dimensional section, uses a laser beam to melt powder in a specific area, solidifies it into a two-dimensional plane, and finally accumulates the entire part layer by layer. SLM technology can be used to form any complex components without tools, molds, and fixtures, and can realize the preparation of complex and fine parts. However, the current SLM preparation of metal materials has the problem of difficult control of oxygen content, which is prone to element volatilization and combination with oxygen to form metallurgical defects, resulting in poor performance of formed parts.
为此，针对SLM成形技术，利用稀土元素亲氧的特点，通过在粉末材料中加入稀土颗粒，使其吸收成形腔和粉末中残余的氧气，减少夹杂物数量及含量。同时，成形的氧化物可以打断材料晶粒的生长，降低晶粒尺寸，提升材料的强度、硬度等性能。在成形过程中，稀土元素与氧元素易结合生成氧化物，由于激光选区熔化逐层成形，每一层在高能激光束下熔化然后快速凝固，在每一个小熔池内部稀土易与氧原位结合成氧化物，可以有效夺取合金中氧生成稀土氧化物，以氧化物的形式弥散分布在每一层的表面，经过增材制造逐层成形，导致氧化物在顶部表面堆积，减少合金氧化烧损率及有效脱气去夹杂，同时发生细晶强化作用，起到细化均匀显微组织，改善合金材料均匀性，有利于提高热稳定性，提升合金材料强度及延伸率。因此，利用SLM技术制备一种面向激光增材制造的专用合金材料，对实际生产及应用拥有十分重要的作用。For this reason, aiming at the SLM forming technology, using the oxophilic characteristics of rare earth elements, by adding rare earth particles into the powder material, it can absorb the residual oxygen in the forming cavity and powder, and reduce the number and content of inclusions. At the same time, the formed oxide can interrupt the growth of material grains, reduce the grain size, and improve the strength, hardness and other properties of the material. During the forming process, rare earth elements and oxygen elements are easily combined to form oxides. Due to laser selective melting, each layer is melted and then rapidly solidified under the high-energy laser beam. In each small molten pool, rare earth elements are easily combined with oxygen in situ. Combined into oxides, it can effectively capture the oxygen in the alloy to form rare earth oxides, which are dispersed in the form of oxides on the surface of each layer, and are formed layer by layer through additive manufacturing, resulting in the accumulation of oxides on the top surface, reducing the oxidation and burning of the alloy. Loss rate and effective degassing to remove inclusions, and at the same time, fine-grain strengthening occurs, which can refine and uniform microstructure, improve the uniformity of alloy materials, and help improve thermal stability, strength and elongation of alloy materials. Therefore, using SLM technology to prepare a special alloy material for laser additive manufacturing plays a very important role in actual production and application.
专利CN113564437A公开了一种非晶增强金属基复合材料的制备与成形方法，通过混合非晶合金粉末和金属粉末进行SLM成形，但该方法没有提及成形过程中抗氧化控制氧含量问题。专利CN113215441A公开了一种基于SLM成型的纳米颗粒增强钛基复合材料及其制备方法，通过多个增强相制备复合材料，但该方法无法准确控制成形过程中氧化物问题，出现熔池中金属氧化物与稀土氧化物过多问题。Patent CN113564437A discloses a preparation and forming method of an amorphous reinforced metal matrix composite material, by mixing amorphous alloy powder and metal powder for SLM forming, but this method does not mention the problem of anti-oxidation and control of oxygen content during the forming process. Patent CN113215441A discloses a nanoparticle-reinforced titanium-based composite material based on SLM and its preparation method. The composite material is prepared through multiple reinforcement phases, but this method cannot accurately control the oxide problem during the forming process, and metal oxidation in the molten pool occurs. The problem of too many compounds and rare earth oxides.
发明内容Contents of the invention
针对现有技术的以上缺陷或改进需求，本发明提供了一种基于激光增材制造的合金材料构件及其制备方法，其目的在于，有效控制SLM成形过程中制件容易氧化，夹杂物数目及含量增加的问题，从而调控制件的微观组织并提高结构性能。In view of the above defects or improvement needs of the prior art, the present invention provides an alloy material component based on laser additive manufacturing and its preparation method. The purpose is to effectively control the easy oxidation of the workpiece during the SLM forming process, the number of inclusions and content increase, thereby adjusting the microstructure of the component and improving the structural performance.
为实现上述目的，按照本发明的一方面，提出了一种基于激光增材制造的合金材料构件的制备方法，包括如下步骤：In order to achieve the above object, according to one aspect of the present invention, a method for preparing an alloy material component based on laser additive manufacturing is proposed, including the following steps:
将粒径为15～45μm的合金粉末和粒径为100nm～500nm稀土粉末混合，使稀土粉末颗粒均匀弥散分布在合金粉末中，且稀土粉末黏附在合金粉末上，形成混合粉末；Mix the alloy powder with a particle size of 15-45 μm and the rare earth powder with a particle size of 100nm-500nm, so that the rare earth powder particles are uniformly dispersed in the alloy powder, and the rare earth powder adheres to the alloy powder to form a mixed powder;
根据构件的三维结构模型，对混合粉末采用激光选区熔化技术进行逐层成形，得到合金材料构件；成形时，稀土夺取合金中的氧生成稀土氧化物，且该稀土氧化物弥散分布在每一层的表面。According to the three-dimensional structure model of the component, the mixed powder is formed layer by layer by laser selective melting technology to obtain the alloy material component; during forming, the rare earth captures the oxygen in the alloy to form a rare earth oxide, and the rare earth oxide is dispersed in each layer s surface.
作为进一步优选的，混合粉末中，稀土粉末所占的质量分数为0.3％～3％。As a further preference, in the mixed powder, the mass fraction of the rare earth powder is 0.3%-3%.
作为进一步优选的，混合粉末中，稀土粉末所占的质量分数为1％～3％。As a further preference, in the mixed powder, the mass fraction of the rare earth powder is 1%-3%.
作为进一步优选的，所述稀土粉末的粒径为100nm～200nm。As a further preference, the particle size of the rare earth powder is 100nm-200nm.
作为进一步优选的，进行激光选区熔化时，激光功率为100W～500W，扫描速率为400mm/s～2000mm/s，扫描间距为0.06mm～0.12mm，层厚为0.03mm～0.06mm。As a further preference, when performing selective laser melting, the laser power is 100W-500W, the scanning speed is 400mm/s-2000mm/s, the scanning distance is 0.06mm-0.12mm, and the layer thickness is 0.03mm-0.06mm.
作为进一步优选的，所述稀土粉末为钇、钪、铌中的一种或组合。As a further preference, the rare earth powder is one or a combination of yttrium, scandium and niobium.
作为进一步优选的，所述合金粉末为铁基合金、铝合金、钛合金中的一种或组合。As a further preference, the alloy powder is one or a combination of iron-based alloys, aluminum alloys, and titanium alloys.
作为进一步优选的，在成形前几层构件时：铺一层粉末，激光束按预设轨迹成形一层后，将扫描方向旋转90°再次扫描，重新熔化已凝固区域，然后再进行下一层成形。As a further preference, when forming the first few layers of components: lay a layer of powder, and after the laser beam forms a layer according to the preset trajectory, rotate the scanning direction by 90° to scan again, re-melt the solidified area, and then proceed to the next layer take shape.
作为进一步优选的，完成前几层成形后：不再重复扫描，仅使层与层之间激光扫描方向旋转67°，直至构件整体成形。As a further preference, after the first few layers are formed: do not repeat scanning, but only rotate the laser scanning direction between layers by 67° until the component is formed as a whole.
按照本发明的另一方面，提供了一种基于激光增材制造的合金材料构件，其采用上述制备方法制备而成。According to another aspect of the present invention, an alloy material component based on laser additive manufacturing is provided, which is prepared by the above-mentioned preparation method.
总体而言，通过本发明所构思的以上技术方案与现有技术相比，主要具备以下的技术优点：Generally speaking, compared with the prior art, the above technical solution conceived by the present invention mainly has the following technical advantages:
1、本发明以微米级的合金粉末与纳米级的稀土单质粉末为原材料，粉末熔化时，纳米级粒径的稀土容易形成稀土氧化物，并在逐层成形过程中稀土氧化物至表面堆积，最终减少构件内部氧化物，能够解决激光制造氧含量难控制难题；可提升合金材料的强度、塑性、耐磨性等力学性能，解决了传统加工方法工时长流程多、加工成本高、整体制造难成形、构件变形难控制及微观组织难调控等问题。1. The present invention uses micron-scale alloy powder and nano-scale rare earth simple substance powder as raw materials. When the powder is melted, the rare earth with nano-scale particle size is easy to form rare earth oxides, and the rare earth oxides accumulate on the surface during the layer-by-layer forming process. Ultimately reducing the internal oxides of components can solve the problem of difficult control of oxygen content in laser manufacturing; it can improve the mechanical properties of alloy materials such as strength, plasticity, wear resistance, etc., and solve the problems of traditional processing methods such as long working hours, high processing costs, and overall manufacturing difficulties. Difficult control of forming, component deformation, and difficult regulation of microstructure.
2、本发明利用稀土元素亲氧的特点，通过在粉末材料中加入小粒径的稀土颗粒，使其吸收成形腔和粉末中残余的氧气，有效夺取氧生成稀土氧化物，并以氧化物的形式弥散分布在每一层的表面，减少构件内部氧化物，从而减少合金氧化烧损率及有效脱气去夹杂。每一层表面的氧化物可以打断材料晶粒的生长，降低晶粒尺寸，发生细晶强化作用，从而细化显微组织，改善合金材料均匀性，有利于提高热稳定性，提升合金材料强度及延伸率。具体来说，在激光增材制造成形过程中，金属粉末受到热作用熔化形成熔池。由于热梯度的存在，且熔池中液体受到浮力、表面张力、重力和马兰戈尼效应等作用下，发生液体流动，同时温度分布也受到影响。熔池温度变化会引起液体流动，两者互相影响，最终实现动态平衡。混合粉末大多数是卫星粉末状态，即纳米稀土粉末黏附在微米合金粉末上，在混合粉末发生熔化时，稀土粉末极易脱落，在众多力作用下产生非平衡现象，移动至每一层的表面。2. The present invention utilizes the oxygen-loving characteristics of rare earth elements to absorb the residual oxygen in the forming cavity and powder by adding small-sized rare earth particles to the powder material, effectively capturing oxygen to generate rare earth oxides, and using the oxides The form is dispersed and distributed on the surface of each layer, reducing the internal oxides of the components, thereby reducing the oxidation and burning rate of the alloy and effectively degassing and removing inclusions. The oxides on the surface of each layer can interrupt the growth of material grains, reduce the grain size, and produce fine-grain strengthening, thereby refining the microstructure, improving the uniformity of the alloy material, and helping to improve thermal stability and enhance the alloy material. strength and elongation. Specifically, during the forming process of laser additive manufacturing, metal powder is melted by heat to form a molten pool. Due to the existence of thermal gradient, and the liquid in the molten pool is affected by buoyancy, surface tension, gravity and Marangoni effect, the liquid flow occurs, and the temperature distribution is also affected. The temperature change of the molten pool will cause the liquid to flow, and the two will affect each other, and finally achieve a dynamic balance. Most of the mixed powder is in the state of satellite powder, that is, the nano-rare earth powder adheres to the micro-alloy powder. When the mixed powder is melted, the rare earth powder is easy to fall off, and it will move to the surface of each layer under the action of many forces. .
3、基于重力作用预先设计合金与稀土粉末成分，确定稀土单质粉末的质量分数；稀土质量分数过少时，虽然稀土的加入可以使合金中晶粒尺寸更加细小，但容易发生界面偏聚现象，导致合金中的界面结合强度降低，无法体现出细晶强化效果；而稀土过多时，稀土与合金元素产生金属间化合物，减少稀土元素细化晶粒作用，发生组织恶化，合金反而粗化。3. Pre-design the composition of the alloy and rare earth powder based on gravity, and determine the mass fraction of the rare earth elemental powder; The interfacial bonding strength in the alloy is reduced, and the fine-grain strengthening effect cannot be reflected; when there are too many rare earths, the rare earths and alloying elements will produce intermetallic compounds, which will reduce the grain refinement effect of the rare earth elements, and the structure will deteriorate, and the alloy will be coarsened instead.
4、本发明设计了激光选区熔化的成形方式，在成形前几层构件时，对已凝固区域进行垂直方向的重复扫描，从而在基板与成形件之间形成优良的冶金结合效果。4. The present invention designs the forming method of laser selective melting. When forming the first few layers of components, the solidified area is repeatedly scanned in the vertical direction, thereby forming an excellent metallurgical bonding effect between the substrate and the formed part.
附图说明Description of drawings
图1为本发明实施例球磨后混合粉末的扫描电子显微镜图；Fig. 1 is the scanning electron microscope picture of the mixed powder after ball milling of the embodiment of the present invention;
图2为本发明实施例混合粉末增材制造成形构件的扫描电子显微镜图。Fig. 2 is a scanning electron microscope image of a shaped component manufactured by mixed powder additives according to an embodiment of the present invention.
具体实施方式Detailed ways
为了使本发明的目的、技术方案及优点更加清楚明白，以下结合附图及实施例，对本发明进行进一步详细说明。应当理解，此处所描述的具体实施例仅仅用以解释本发明，并不用于限定本发明。此外，下面所描述的本发明各个实施方式中所涉及到的技术特征只要彼此之间未构成冲突就可以相互组合。In order to make the object, technical solution and advantages of the present invention clearer, the present invention will be further described in detail below in conjunction with the accompanying drawings and embodiments. It should be understood that the specific embodiments described here are only used to explain the present invention, not to limit the present invention. In addition, the technical features involved in the various embodiments of the present invention described below can be combined with each other as long as they do not constitute a conflict with each other.
本发明实施例提供的一种基于激光增材制造的合金材料构件的制备方法，包括如下步骤：A method for preparing an alloy material component based on laser additive manufacturing provided by an embodiment of the present invention includes the following steps:
(1)选取粒径范围15～45μm的合金粉末及粒径范围100～500nm的稀土单质粉末作为原材料，将两者在惰性气体氛围下球磨，通过球磨混合均匀，使稀土颗粒细小均匀弥散分布在合金粉末中，得到混合粉末，将球磨后的粉末干燥。(1) Select the alloy powder with a particle size range of 15-45 μm and the rare earth elemental powder with a particle size range of 100-500 nm as raw materials, ball mill the two in an inert gas atmosphere, and mix them uniformly through ball milling to make the rare earth particles fine and evenly dispersed in the In the alloy powder, a mixed powder is obtained, and the ball-milled powder is dried.
具体的，球磨过程中，罐内温度升高易发生合金粉末氧化，所以需要在球磨之前对球磨罐抽真空，并通入氩气避免粉末氧化。为减少空气水分与氧对粉末造成影响，保证原料洁净还需在真空环境下进行干燥处理。Specifically, during the ball milling process, the alloy powder oxidation is likely to occur when the temperature in the tank rises, so it is necessary to evacuate the ball mill tank before ball milling, and pass in argon gas to avoid powder oxidation. In order to reduce the impact of air moisture and oxygen on the powder and ensure the cleanliness of the raw materials, it is necessary to dry them in a vacuum environment.
(2)依据设计成形产品的三维结构模型，对获得的混合粉末采用激光选区熔化技术进行成形，无需机械加工及后切削处理就能获得完整的设计成形产品。且成形时，稀土夺取合金中的氧生成稀土氧化物，且该稀土氧化物弥散分布在每一层的表面。(2) According to the three-dimensional structural model of the designed and formed product, the obtained mixed powder is formed by laser selective melting technology, and a complete designed and formed product can be obtained without machining and post-cutting. And during forming, the rare earths take oxygen from the alloy to form rare earth oxides, and the rare earth oxides are dispersed on the surface of each layer.
具体的，先采用三维造型软件设计出金属基复合材料构件的三维模型并切片分层，转成STL文件，以备进行激光选区熔化加工。然后将洁净干燥的基板放在成形设备工作台上，预先通入一定量的高纯氩气(≥99.99％)，控制腔内氧含量；在基板表面铺一层粉末，高能激光束按照预先设计轨迹成形第一层，随后将扫描方向旋转90°再次扫描，重新熔化已凝固区域；然后基板下降一个高度，将下一层粉末铺在基板上；重复上述操作成形1-5层，在基板与成形件之间形成优良的冶金结合效果，在5层以后，不再重复扫描，仅仅改变层与层之间激光扫描方向旋转67°，直至成形件整体成形。等零件自然冷却后，切割分离零件和基板，得到最终金属基复合材料。Specifically, the three-dimensional model of the metal matrix composite component is first designed by using three-dimensional modeling software, sliced and layered, and converted into an STL file for laser selective melting processing. Then put the clean and dry substrate on the working table of the forming equipment, and pre-introduce a certain amount of high-purity argon gas (≥99.99%) to control the oxygen content in the cavity; spread a layer of powder on the surface of the substrate, and the high-energy laser beam is designed according to the pre-designed The trajectory forms the first layer, and then rotates the scanning direction by 90° to scan again to re-melt the solidified area; then the substrate is lowered to a height, and the next layer of powder is spread on the substrate; repeat the above operation to form 1-5 layers, between the substrate and An excellent metallurgical bonding effect is formed between the formed parts. After the 5th layer, the scanning is no longer repeated, and the laser scanning direction is only changed between layers and rotated by 67° until the formed part is formed as a whole. After the parts are cooled naturally, the parts and the substrate are cut and separated to obtain the final metal matrix composite.
优选的，稀土单质粉末在混合粉末中的质量分数为0.3％～3％，进一步优选为1％～3％，更进一步优选为1.5％；合金粉末与稀土单质粉末之间不发生化学反应。Preferably, the mass fraction of the rare earth elemental powder in the mixed powder is 0.3% to 3%, more preferably 1% to 3%, and even more preferably 1.5%; no chemical reaction occurs between the alloy powder and the rare earth elemental powder.
优选的，稀土粉末粒径100～500nm，进一步优选为100nm～200nm；这一设计还可以避免粒径过小时产生的稀土化合物比表面积过大，流动性变差容易发生相互粘连团聚；或粒径过大时稀土化合物分布不够均匀易出现成分偏析现象。Preferably, the particle size of the rare earth powder is 100-500nm, more preferably 100nm-200nm; this design can also avoid the excessive specific surface area of the rare earth compound produced when the particle size is too small, and the fluidity becomes poor, which is prone to mutual adhesion and agglomeration; or the particle size When it is too large, the distribution of rare earth compounds is not uniform enough, and the phenomenon of component segregation may easily occur.
优选的，进行激光选区熔化时，高能激光束源为Yb光纤激光，激光功率为100W～500W，扫描速率为400mm/s～2000mm/s，扫描间距为0.06mm～0.12mm，层厚为0.03mm～0.06mm。Preferably, when performing selective laser melting, the high-energy laser beam source is Yb fiber laser, the laser power is 100W-500W, the scanning rate is 400mm/s-2000mm/s, the scanning distance is 0.06mm-0.12mm, and the layer thickness is 0.03 mm ~ 0.06mm.
优选的，球磨时间为1h～5h，转速为150rpm～300rpm。Preferably, the ball milling time is 1h-5h, and the rotation speed is 150rpm-300rpm.
优选的，合金粉末为铁基合金(如钢)、铝合金或钛合金中的一种或组合。Preferably, the alloy powder is one or a combination of iron-based alloys (such as steel), aluminum alloys or titanium alloys.
优选的，稀土单质粉末为钇、钪或铌中的一种或组合。Preferably, the rare earth elemental powder is one or a combination of yttrium, scandium or niobium.
本发明通过加入一定粒径的稀土元素粉末发生反应改性，稀土元素亲氧性较好，在成形过程中会与成形腔和粉末中残余的氧元素结合，在熔池边缘生成氧化物，沿着熔池分布，当下一层熔化时，氧化物上升到表面，经过增材制造逐层成形，使氧化物在表面堆积，实现去氧提纯，同时发生细晶强化，从而起到细化均匀显微组织，改善合金材料均匀性的作用，有利于提高热稳定性，大幅度提升合金材料强度及延伸率。通过本发明方法，能够降低激光选区熔化中氧含量对成形件质量的影响，同时大幅细化晶粒尺寸，改善缺陷问题，可以获得综合力学性能优异且形状复杂精密的金属基复合材料制件。In the present invention, reaction modification occurs by adding rare earth element powder with a certain particle size. The rare earth element has good oxophilicity, and will combine with the residual oxygen element in the forming cavity and powder during the forming process to form oxides at the edge of the molten pool. According to the distribution of the molten pool, when the next layer melts, the oxide rises to the surface, and is formed layer by layer through additive manufacturing, so that the oxide accumulates on the surface to achieve deoxidation and purification, and fine-grain strengthening occurs at the same time, so as to achieve a uniform and uniform appearance. The microstructure improves the uniformity of the alloy material, which is conducive to improving the thermal stability and greatly improving the strength and elongation of the alloy material. The method of the present invention can reduce the influence of oxygen content on the quality of formed parts in laser selective melting, greatly refine the grain size, improve defect problems, and obtain metal matrix composite parts with excellent comprehensive mechanical properties and complex and precise shapes.
以下为具体实施例：The following are specific examples:
实施例1Example 1
以激光选区熔化技术制备与成形钪/铝合金材料，具体步骤如下：Preparation and shaping of scandium/aluminum alloy materials by laser selective melting technology, the specific steps are as follows:
(1)采用三维造型软件设计出铝合金材料构件的三维模型并切片分层，转成STL文件，以备进行激光选区熔化加工；(1) Use 3D modeling software to design a 3D model of aluminum alloy material components, slice and layer them, and convert them into STL files for laser selective melting processing;
(2)原料准备：选用粒径范围在15～45微米球形铝合金粉末及粒径范围在100～500nm高纯Sc粉末，经干燥后在真空环境下存储；(2) Raw material preparation: select spherical aluminum alloy powder with a particle size range of 15-45 microns and high-purity Sc powder with a particle size range of 100-500 nm, and store them in a vacuum environment after drying;
(3)球磨法制备复合粉末：将铝合金粉末与合计3wt.％的高纯Sc粉末在惰性气体氛围下球磨，通过低能球磨混合均匀；球磨条件：球磨时间4h，转速270rpm。在球磨之前对球磨罐抽真空，并通入氩气避免粉末氧化。为减少空气水分与氧对粉末造成影响，保证原料洁净还需在真空环境下进行干燥处理。混合粉末如图1所示，可看出合金粉末上附着有小的稀土粉末。(3) Preparation of composite powder by ball milling method: ball mill the aluminum alloy powder and a total of 3wt.% high-purity Sc powder in an inert gas atmosphere, and mix uniformly through low-energy ball milling; ball milling conditions: ball milling time 4h, speed 270rpm. Before the ball milling, vacuumize the ball mill jar and pass in argon gas to avoid powder oxidation. In order to reduce the impact of air moisture and oxygen on the powder and ensure the cleanliness of the raw materials, it is necessary to dry them in a vacuum environment. The mixed powder is shown in Figure 1, and it can be seen that there are small rare earth powders attached to the alloy powder.
(4)将洁净干燥的铝合金基板放在成形设备工作台上，预先通入一定量的高纯氩气(≥99.99％)，使腔内氧含量小于0.01％。其中高能激光束源为Yb光纤激光，铝合金粉末激光吸收率低，同时Sc元素烧损率与激光能量密度有关，为了保证成形效果良好，激光功率选择400W，扫描速度720mm/s，间距0.12mm，层厚0.03mm。在基板表面铺一层粉末，高能激光束按照预先设计轨迹成形第一层，随后将扫描方向旋转90°再次扫描，重新熔化已凝固区域。然后基板下降一个高度，将下一层粉末铺在基板上。重复上述操作成形1-5层，在基板与成形件之间形成优良的冶金结合效果，在5层以后，不再重复扫描，仅仅改变层与层之间激光扫描方向旋转67°，直至成形件整体成形。等零件自然冷却后，切割分离零件和基板，得到最终铝合金材料，如图2所示。经过上述工艺参数调整，铝合金致密度能够稳定在99.5％以上。(4) Put the clean and dry aluminum alloy substrate on the working table of the forming equipment, and pre-flow a certain amount of high-purity argon gas (≥99.99%) to make the oxygen content in the cavity less than 0.01%. The high-energy laser beam source is Yb fiber laser, the laser absorption rate of aluminum alloy powder is low, and the burning rate of Sc element is related to the laser energy density. In order to ensure a good forming effect, the laser power is 400W, the scanning speed is 720mm/s, and the spacing is 0.12mm. , layer thickness 0.03mm. Spread a layer of powder on the surface of the substrate, and the high-energy laser beam forms the first layer according to the pre-designed trajectory, and then rotates the scanning direction by 90° to scan again to re-melt the solidified area. Then the substrate is lowered to a height, and the next layer of powder is spread on the substrate. Repeat the above operations to form 1-5 layers, forming an excellent metallurgical bonding effect between the substrate and the formed part. After the 5th layer, no repeat scanning, just change the laser scanning direction between layers and rotate 67° until the formed part Overall shape. After the parts are cooled naturally, the parts and the substrate are cut and separated to obtain the final aluminum alloy material, as shown in Figure 2. After the adjustment of the above process parameters, the density of the aluminum alloy can be stabilized above 99.5%.
实施例2Example 2
以激光选区熔化技术制备与成形钪/铝合金材料，具体步骤如下：Preparation and shaping of scandium/aluminum alloy materials by laser selective melting technology, the specific steps are as follows:
(1)采用三维造型软件设计出铝合金材料构件的三维模型并切片分层，转成STL文件，以备进行激光选区熔化加工；(1) Use 3D modeling software to design a 3D model of aluminum alloy material components, slice and layer them, and convert them into STL files for laser selective melting processing;
(2)原料准备：选用粒径范围在15～45微米球形铝合金粉末及粒径范围在100～500nm高纯Sc粉末，经干燥后在真空环境下存储；(2) Raw material preparation: select spherical aluminum alloy powder with a particle size range of 15-45 microns and high-purity Sc powder with a particle size range of 100-500 nm, and store them in a vacuum environment after drying;
(3)球磨法制备复合粉末：将铝合金粉末与合计1.5wt.％的高纯Sc粉末在惰性气体氛围下球磨，通过低能球磨混合均匀；球磨条件：球磨时间4h，转速270rpm。在球磨之前对球磨罐抽真空，并通入氩气避免粉末氧化。为减少空气水分与氧对粉末造成影响，保证原料洁净还需在真空环境下进行干燥处理。(3) Preparation of composite powder by ball milling method: ball mill the aluminum alloy powder and a total of 1.5wt.% high-purity Sc powder in an inert gas atmosphere, and mix uniformly through low-energy ball milling; ball milling conditions: ball milling time 4h, speed 270rpm. Before the ball milling, vacuumize the ball mill jar and pass in argon gas to avoid powder oxidation. In order to reduce the impact of air moisture and oxygen on the powder and ensure the cleanliness of the raw materials, it is necessary to dry them in a vacuum environment.
(4)将洁净干燥的铝合金基板放在成形设备工作台上，预先通入一定量的高纯氩气(≥99.99％)，使腔内氧含量小于0.01％。其中高能激光束源为Yb光纤激光，铝合金粉末激光吸收率低，同时Sc元素烧损率与激光能量密度有关，为了保证成形效果良好，激光功率选择400W，扫描速度720mm/s，间距0.12mm，层厚0.03mm。在基板表面铺一层粉末，高能激光束按照预先设计轨迹成形第一层，随后将扫描方向旋转90°再次扫描，重新熔化已凝固区域。然后基板下降一个高度，将下一层粉末铺在基板上。重复上述操作成形1-5层，在基板与成形件之间形成优良的冶金结合效果，在5层以后，不再重复扫描，仅仅改变层与层之间激光扫描方向旋转67°，直至成形件整体成形。等零件自然冷却后，切割分离零件和基板，得到最终铝合金材料。经过上述工艺参数调整，铝合金致密度能够稳定在99.7％以上。(4) Put the clean and dry aluminum alloy substrate on the working table of the forming equipment, and pre-flow a certain amount of high-purity argon gas (≥99.99%) to make the oxygen content in the cavity less than 0.01%. The high-energy laser beam source is Yb fiber laser, the laser absorption rate of aluminum alloy powder is low, and the burning rate of Sc element is related to the laser energy density. In order to ensure a good forming effect, the laser power is 400W, the scanning speed is 720mm/s, and the spacing is 0.12mm. , layer thickness 0.03mm. Spread a layer of powder on the surface of the substrate, and the high-energy laser beam forms the first layer according to the pre-designed trajectory, and then rotates the scanning direction by 90° to scan again to re-melt the solidified area. Then the substrate is lowered to a height, and the next layer of powder is spread on the substrate. Repeat the above operations to form 1-5 layers, forming an excellent metallurgical bonding effect between the substrate and the formed part. After the 5th layer, no repeat scanning, just change the laser scanning direction between layers and rotate 67° until the formed part Overall shape. After the parts are cooled naturally, the parts and the substrate are cut and separated to obtain the final aluminum alloy material. After the adjustment of the above process parameters, the density of the aluminum alloy can be stabilized above 99.7%.
实施例3Example 3
以激光选区熔化技术制备与成形钪/铝合金材料，具体步骤如下：Preparation and shaping of scandium/aluminum alloy materials by laser selective melting technology, the specific steps are as follows:
(1)采用三维造型软件设计出铝合金材料构件的三维模型并切片分层，转成STL文件，以备进行激光选区熔化加工；(1) Use 3D modeling software to design a 3D model of aluminum alloy material components, slice and layer them, and convert them into STL files for laser selective melting processing;
(2)原料准备：选用粒径范围在15～45微米球形铝合金粉末及粒径范围在100～500nm高纯Sc粉末，经干燥后在真空环境下存储；(2) Raw material preparation: select spherical aluminum alloy powder with a particle size range of 15-45 microns and high-purity Sc powder with a particle size range of 100-500 nm, and store them in a vacuum environment after drying;
(3)球磨法制备复合粉末：将铝合金粉末与合计0.3wt.％的高纯Sc粉末在惰性气体氛围下球磨，通过低能球磨混合均匀；球磨条件：球磨时间4h，转速270rpm。在球磨之前对球磨罐抽真空，并通入氩气避免粉末氧化。为减少空气水分与氧对粉末造成影响，保证原料洁净还需在真空环境下进行干燥处理。(3) Preparation of composite powder by ball milling method: ball mill aluminum alloy powder and 0.3wt.% high-purity Sc powder in an inert gas atmosphere, and mix uniformly by low-energy ball milling; ball milling conditions: ball milling time 4h, speed 270rpm. Before the ball milling, vacuumize the ball mill jar and pass in argon gas to avoid powder oxidation. In order to reduce the impact of air moisture and oxygen on the powder and ensure the cleanliness of the raw materials, it is necessary to dry them in a vacuum environment.
(4)将洁净干燥的铝合金基板放在成形设备工作台上，预先通入一定量的高纯氩气(≥99.99％)，使腔内氧含量小于0.01％。其中高能激光束源为Yb光纤激光，铝合金粉末激光吸收率低，同时Sc元素烧损率与激光能量密度有关，为了保证成形效果良好，激光功率选择400W，扫描速度720mm/s，间距0.12mm，层厚0.03mm。在基板表面铺一层粉末，高能激光束按照预先设计轨迹成形第一层，随后将扫描方向旋转90°再次扫描，重新熔化已凝固区域。然后基板下降一个高度，将下一层粉末铺在基板上。重复上述操作成形1-5层，在基板与成形件之间形成优良的冶金结合效果，在5层以后，不再重复扫描，仅仅改变层与层之间激光扫描方向旋转67°，直至成形件整体成形。等零件自然冷却后，切割分离零件和基板，得到最终铝合金材料。经过上述工艺参数调整，铝合金致密度能够稳定在99.4％以上。(4) Put the clean and dry aluminum alloy substrate on the working table of the forming equipment, and pre-flow a certain amount of high-purity argon gas (≥99.99%) to make the oxygen content in the cavity less than 0.01%. The high-energy laser beam source is Yb fiber laser, the laser absorption rate of aluminum alloy powder is low, and the burning rate of Sc element is related to the laser energy density. In order to ensure a good forming effect, the laser power is 400W, the scanning speed is 720mm/s, and the spacing is 0.12mm. , layer thickness 0.03mm. Spread a layer of powder on the surface of the substrate, and the high-energy laser beam forms the first layer according to the pre-designed trajectory, and then rotates the scanning direction by 90° to scan again to re-melt the solidified area. Then the substrate is lowered to a height, and the next layer of powder is spread on the substrate. Repeat the above operations to form 1-5 layers, forming an excellent metallurgical bonding effect between the substrate and the formed part. After the 5th layer, no repeat scanning, just change the laser scanning direction between layers and rotate 67° until the formed part Overall shape. After the parts are cooled naturally, the parts and the substrate are cut and separated to obtain the final aluminum alloy material. After the adjustment of the above process parameters, the density of the aluminum alloy can be stabilized above 99.4%.
实施例4Example 4
以激光选区熔化技术制备与成形铌/钛合金材料，具体步骤如下：Preparation and forming of niobium/titanium alloy materials by laser selective melting technology, the specific steps are as follows:
(1)采用三维造型软件设计出钛合金材料构件的三维模型并切片分层，转成STL文件，以备进行激光选区熔化加工；(1) Use 3D modeling software to design a 3D model of titanium alloy material components, slice and layer them, and convert them into STL files for laser selective melting processing;
(2)原料准备：选用粒径范围在15～45μm的球形钛合金粉末及粒径范围100～200nm高纯Nb粉末，经干燥后在真空环境下存储；(2) Raw material preparation: select spherical titanium alloy powder with a particle size range of 15-45 μm and high-purity Nb powder with a particle size range of 100-200 nm, store in a vacuum environment after drying;
(3)球磨法制备复合粉末：将钛合金粉末与合计1.5wt.％的高纯Nb粉末在惰性气体氛围下球磨，通过低能球磨混合均匀。球磨条件：球磨时间3h，转速210rpm。(3) Preparation of composite powder by ball milling method: ball mill titanium alloy powder and 1.5 wt.% high-purity Nb powder in an inert gas atmosphere, and mix uniformly by low-energy ball milling. Ball milling conditions: ball milling time 3h, rotation speed 210rpm.
(4)将洁净干燥的钛合金基板放在成形设备工作台上，为了充分熔化Nb元素并降低温度梯度减少残余应力，对基板进行预热至100℃，预先通入一定量的高纯氩气(≥99.99％)，使腔内氧含量小于0.01％。其中高能激光束源为Yb光纤激光，激光功率为350W，扫描速度1500mm/s，间距0.08mm，层厚0.03mm。按实施例1中成形方法进行成形，得到最终钛合金材料。经过上述工艺参数调整，钛合金具有优良的屈服强度和拉伸率。(4) Put the clean and dry titanium alloy substrate on the workbench of the forming equipment. In order to fully melt the Nb element and reduce the temperature gradient to reduce the residual stress, the substrate is preheated to 100 ° C, and a certain amount of high-purity argon is pre-flowed. (≥99.99%), so that the oxygen content in the cavity is less than 0.01%. The high-energy laser beam source is Yb fiber laser, the laser power is 350W, the scanning speed is 1500mm/s, the spacing is 0.08mm, and the layer thickness is 0.03mm. Forming is carried out according to the forming method in Example 1 to obtain the final titanium alloy material. After the adjustment of the above process parameters, the titanium alloy has excellent yield strength and elongation.
实施例5Example 5
以激光选区熔化技术制备与成形钇/不锈钢材料，具体步骤如下：Preparation and shaping of yttrium/stainless steel material by laser selective melting technology, the specific steps are as follows:
(1)采用三维造型软件设计出不锈钢材料构件的三维模型并切片分层，转成STL文件，以备进行激光选区熔化加工；(1) Use 3D modeling software to design a 3D model of stainless steel components, slice and layer them, and convert them into STL files for laser selective melting processing;
(2)原料准备：选用粒径范围在15～45μm的球形不锈钢粉末及粒径范围在100～200nm高纯Y粉末，经干燥后在真空环境下存储；(2) Raw material preparation: select spherical stainless steel powder with a particle size range of 15-45 μm and high-purity Y powder with a particle size range of 100-200 nm, store in a vacuum environment after drying;
(3)球磨法制备复合粉末：将不锈钢粉末与合计1wt.％的高纯Y粉末在惰性气体氛围下球磨，通过低能球磨混合均匀。球磨条件：球磨时间5h，转速180rpm。(3) Preparation of composite powder by ball milling method: stainless steel powder and 1 wt.% high-purity Y powder in total were ball milled in an inert gas atmosphere, and mixed uniformly by low energy ball milling. Ball milling conditions: ball milling time 5h, rotating speed 180rpm.
(4)将洁净干燥的不锈钢基板放在成形设备工作台上，不锈钢材料在高激光功率情况下，部分金属与稀土会发生汽化，元素烧损率升高，为了保证不锈钢材料良好的成形，预先通入一定量的高纯氩气(≥99.99％)，使腔内氧含量小于0.1％。其中高能激光束源为Yb光纤激光，激光功率为150W，扫描速度500mm/s，间距0.09mm，层厚0.03mm。按实施例1中成形方法进行成形，最终得到不锈钢材料。(4) Put the clean and dry stainless steel substrate on the working table of the forming equipment. When the stainless steel material is under high laser power, some metals and rare earths will be vaporized, and the burning rate of elements will increase. In order to ensure good forming of the stainless steel material, pre- A certain amount of high-purity argon gas (≥99.99%) is injected to make the oxygen content in the chamber less than 0.1%. The high-energy laser beam source is Yb fiber laser, the laser power is 150W, the scanning speed is 500mm/s, the spacing is 0.09mm, and the layer thickness is 0.03mm. Carry out shaping according to the shaping method in embodiment 1, finally obtain stainless steel material.
对比例1Comparative example 1
以激光选区熔化技术制备与成形铝合金材料，具体步骤如下：The specific steps of preparing and forming aluminum alloy materials by laser selective melting technology are as follows:
(1)采用三维造型软件设计出铝合金材料构件的三维模型并切片分层，转成STL文件，以备进行激光选区熔化加工；(1) Use 3D modeling software to design a 3D model of aluminum alloy material components, slice and layer them, and convert them into STL files for laser selective melting processing;
(2)原料准备：选用粒径范围在15～45微米球形铝合金粉末，经干燥后在真空环境下存储；(2) Raw material preparation: select spherical aluminum alloy powder with a particle size ranging from 15 to 45 microns, and store it in a vacuum environment after drying;
(3)将洁净干燥的铝合金基板放在成形设备工作台上，预先通入一定量的高纯氩气(≥99.99％)，使腔内氧含量小于0.01％。其中高能激光束源为Yb光纤激光，铝合金粉末激光吸收率低，为了保证成形效果良好，激光功率选择400W，扫描速度720mm/s，间距0.12mm，层厚0.03mm。在基板表面铺一层粉末，高能激光束按照预先设计轨迹成形第一层，随后将扫描方向旋转90°再次扫描，重新熔化已凝固区域。然后基板下降一个高度，将下一层粉末铺在基板上。重复上述操作成形1-5层，在基板与成形件之间形成优良的冶金结合效果，在5层以后，不再重复扫描，仅仅改变层与层之间激光扫描方向旋转67°，直至成形件整体成形。等零件自然冷却后，切割分离零件和基板，得到最终铝合金材料。(3) Put the clean and dry aluminum alloy substrate on the workbench of the forming equipment, and pre-flow a certain amount of high-purity argon gas (≥99.99%) to make the oxygen content in the cavity less than 0.01%. The high-energy laser beam source is Yb fiber laser, and the laser absorption rate of aluminum alloy powder is low. In order to ensure a good forming effect, the laser power is 400W, the scanning speed is 720mm/s, the spacing is 0.12mm, and the layer thickness is 0.03mm. Spread a layer of powder on the surface of the substrate, and the high-energy laser beam forms the first layer according to the pre-designed trajectory, and then rotates the scanning direction by 90° to scan again to re-melt the solidified area. Then the substrate is lowered to a height, and the next layer of powder is spread on the substrate. Repeat the above operations to form 1-5 layers, forming an excellent metallurgical bonding effect between the substrate and the formed part. After the 5th layer, no repeat scanning, just change the laser scanning direction between layers and rotate 67° until the formed part Overall shape. After the parts are cooled naturally, the parts and the substrate are cut and separated to obtain the final aluminum alloy material.
对实施例1、2、3及对比例1成形材料进行力学测试，四种材料为添加稀土不同含量的铝基材料，测试方法为ASTM E8/E8M标准，使用上海新三思制作的C43.104 30kN高温电子万能材料试验机测试标准拉伸样的室温拉伸性能，测试速度1.5mm/min，测试结果如表1所述。Carry out mechanical tests on the forming materials of Examples 1, 2, 3 and Comparative Example 1. The four materials are aluminum-based materials with different contents of rare earth added. The test method is ASTM E8/E8M standard, and C43.104 30kN produced by Shanghai Xinsansi is used. The high-temperature electronic universal material testing machine tested the room temperature tensile properties of the standard tensile sample, and the test speed was 1.5mm/min. The test results are shown in Table 1.
表1测试结果Table 1 Test results
通过表1可知，本发明方法能够大幅度提高材料力学性能，实施例2中拉伸强度与塑性最佳，添加更多稀土含量后，拉伸强度与塑性有所降低。It can be seen from Table 1 that the method of the present invention can greatly improve the mechanical properties of the material. In Example 2, the tensile strength and plasticity are the best. After adding more rare earth content, the tensile strength and plasticity are reduced.
本领域的技术人员容易理解，以上所述仅为本发明的较佳实施例而已，并不用以限制本发明，凡在本发明的精神和原则之内所作的任何修改、等同替换和改进等，均应包含在本发明的保护范围之内。It is easy for those skilled in the art to understand that the above descriptions are only preferred embodiments of the present invention, and are not intended to limit the present invention. Any modifications, equivalent replacements and improvements made within the spirit and principles of the present invention, All should be included within the protection scope of the present invention.
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