CN114411035B - Precipitation strengthening type medium-entropy alloy suitable for laser additive manufacturing and preparation method thereof - Google Patents

Precipitation strengthening type medium-entropy alloy suitable for laser additive manufacturing and preparation method thereof Download PDF

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CN114411035B
CN114411035B CN202210067106.8A CN202210067106A CN114411035B CN 114411035 B CN114411035 B CN 114411035B CN 202210067106 A CN202210067106 A CN 202210067106A CN 114411035 B CN114411035 B CN 114411035B
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何峰
郭博静
谢浩宇
王志军
李俊杰
王锦程
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Northwestern Polytechnical University
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Abstract

本发明提供适用于激光增材制造的析出强化型中熵合金及其制备方法,所述析出强化型中熵合金为NiaCobCrcAldMe,其中,M为Ti、Ta、Nb和Mo中的一种或多种元素,a、b、c、d和e分别代表对应各元素的摩尔百分比,b=20%‑40%,c=20%‑25%,d>1%,e>0,d+e<7%,a+b+c+d+e=100%。本发明析出强化型中熵合金采用激光选区熔化成形技术或激光立体成形技术进行制备,实现了高致密、无裂纹、综合力学性能优异的新型析出强化型中熵合金的制备。The present invention provides a precipitation-enhanced medium-entropy alloy suitable for laser additive manufacturing and a preparation method thereof, wherein the precipitation-enhanced medium-entropy alloy is Ni a Co b Cr c Al d Me , wherein M is Ti, Ta, Nb and one or more elements in Mo, a, b, c, d and e respectively represent the molar percentages of the corresponding elements, b=20%-40%, c=20%-25%, d>1%, e>0, d+e<7%, a+b+c+d+e=100%. The precipitation-enhanced medium-entropy alloy of the present invention is prepared by laser selective melting forming technology or laser three-dimensional forming technology, and realizes the preparation of a new type of precipitation-enhanced medium-entropy alloy with high density, no cracks and excellent comprehensive mechanical properties.

Description

适用于激光增材制造的析出强化型中熵合金及其制备方法Precipitation-enhanced medium-entropy alloy suitable for laser additive manufacturing and preparation method thereof

技术领域technical field

本发明涉及金属材料激光增材制造技术领域,尤其涉及一种适用于激光增材制造的析出强化型中熵合金及其制备方法。The invention relates to the technical field of laser additive manufacturing of metal materials, in particular to a precipitation-enhanced medium-entropy alloy suitable for laser additive manufacturing and a preparation method thereof.

背景技术Background technique

高/中熵合金以全新的合金设计策略,采用几种等浓度或近等浓度的主元素作为合金元素,表现出优异的强度、延展性和断裂韧性的结合,具有广泛的结构化和功能化应用前景。FCC结构的高/中熵合金表现出良好的韧性但其强度普遍偏低,难以满足结构材料的应用需求,目前,在FCC高/中熵合金中引入析出相是实现FCC高/中熵合金强韧化的有效方法。High/medium-entropy alloys use a new alloy design strategy, using several iso-concentration or near-iso-concentration main elements as alloying elements, exhibiting an excellent combination of strength, ductility and fracture toughness, with a wide range of structuring and functionalization Application prospects. High/medium entropy alloys with FCC structure exhibit good toughness, but their strength is generally low, which is difficult to meet the application requirements of structural materials. Effective method of toughening.

高/中熵合金传统制备方法以电弧熔炼为主,存在形状尺寸单一、易出现成分偏析、缩松、缩孔等缺陷,难以成形全致密高性能结构复杂的高/中熵合金部件,极大限制了高/中熵合金的进一步应用与发展。The traditional preparation method of high/medium-entropy alloys is mainly based on arc melting, which has defects such as single shape and size, prone to component segregation, shrinkage porosity, and shrinkage cavities. The further application and development of high/medium entropy alloys are limited.

激光增材制造技术基于材料逐点、逐线、逐层累积的原理,通过高能激光束与金属粉末的快速作用,以极高的制造灵活性,实现了复杂结构或定制部件的近净成形。该技术具有材料利用率高、制造过程高柔性、周期短、微观组织均匀细小等优势,为制备综合性能优异,高精度全致密及形状复杂的高/中熵合金构件提供了巨大的潜力。然而,增材制造过程中高的温度梯度和大的冷却速率,通常会导致高的热残余应力,容易产生裂纹等冶金缺陷。尤其对于析出强化型高/中熵合金,打印过程中极易出现液化开裂及应变时效开裂等缺陷,影响构件的组织完整性和综合性能。因此,设计出适用于激光增材制造的析出强化型高/中熵合金是本领域亟需解决的关键问题。Laser additive manufacturing technology is based on the principle of point-by-point, line-by-line, and layer-by-layer accumulation of materials. Through the rapid action of high-energy laser beams and metal powders, with high manufacturing flexibility, the near-net shape of complex structures or customized parts is realized. This technology has the advantages of high material utilization, high flexibility in the manufacturing process, short cycle time, uniform and fine microstructure, etc., and provides great potential for the preparation of high-/medium-entropy alloy components with excellent comprehensive performance, high-precision full-density and complex shapes. However, the high temperature gradient and large cooling rate in the additive manufacturing process usually lead to high thermal residual stress, which is prone to metallurgical defects such as cracks. Especially for precipitation-strengthened high/medium entropy alloys, defects such as liquefaction cracking and strain aging cracking are prone to occur during the printing process, which affects the structural integrity and comprehensive performance of the component. Therefore, designing precipitation-strengthened high/medium entropy alloys suitable for laser additive manufacturing is a key problem that needs to be solved urgently in this field.

发明内容Contents of the invention

本发明的目的在于克服传统高/中熵合金制备方法的缺点,提供适用于激光增材制造的析出强化型中熵合金及其制备方法,实现高致密、无裂纹、综合力学性能优异的新型析出强化型中熵合金的制备。The purpose of the present invention is to overcome the shortcomings of traditional high/medium entropy alloy preparation methods, provide a precipitation-strengthened medium-entropy alloy suitable for laser additive manufacturing and its preparation method, and realize a new type of precipitation with high density, no cracks, and excellent comprehensive mechanical properties. Preparation of strengthened medium entropy alloys.

本发明通过以下技术方案实现:The present invention is realized through the following technical solutions:

适用于激光增材制造的析出强化型中熵合金,所述析出强化型中熵合金为NiaCobCrcAldMe,其中,M为Ti、Ta、Nb和Mo中的一种或多种元素,a、b、c、d和e分别代表对应各元素的摩尔百分比,b=20%-40%,c=20%-25%,d>1%,e>0,d+e<7%,a+b+c+d+e=100%。A precipitation-enhanced medium-entropy alloy suitable for laser additive manufacturing, wherein the precipitation-enhanced medium-entropy alloy is Ni a Co b Cr c Al d Me , wherein M is one of Ti, Ta, Nb and Mo or A variety of elements, a, b, c, d and e respectively represent the mole percentage of each element, b=20%-40%, c=20%-25%, d>1%, e>0, d+e <7%, a+b+c+d+e=100%.

优选的,采用激光选区熔化成形技术进行制备。Preferably, it is prepared by laser selective melting forming technology.

进一步的,包括:Further, including:

步骤1,中熵合金粉末制备及预处理Step 1, preparation and pretreatment of medium entropy alloy powder

按照权利要求1所述摩尔百分比,取各元素对应的金属原料,采用真空气雾化法制备中熵合金预合金球形粉末,过筛,烘干,得到中熵合金粉末;According to the mole percentage described in claim 1, the metal raw materials corresponding to each element are taken, and the pre-alloyed spherical powder of the medium-entropy alloy is prepared by vacuum atomization, sieved, and dried to obtain the medium-entropy alloy powder;

步骤2,激光选区熔化成形NiaCobCrcAldMe析出强化型中熵合金Step 2, laser selective melting forming Ni a Co b Cr c Al d Me precipitation strengthened medium entropy alloy

根据待制备的中熵合金构件的几何形状建立三维实体模型并转换为STL格式的文件,导入激光选区熔化成形设备的建造软件中,进行分层处理;通入高纯氩气,使成形舱室内氧气含量低于300ppm,根据所设定的激光选区熔化成形的工艺参数及扫描策略,将中熵合金粉末逐层熔化成形,制备得到中熵合金构件。Establish a three-dimensional solid model according to the geometric shape of the medium-entropy alloy component to be prepared and convert it into a file in STL format, import it into the construction software of the laser selective melting forming equipment, and perform layered processing; inject high-purity argon gas to make the forming chamber The oxygen content is lower than 300ppm. According to the set process parameters and scanning strategy of laser selective melting and forming, the medium-entropy alloy powder is melted and formed layer by layer, and the medium-entropy alloy component is prepared.

进一步的,激光选区熔化成形的工艺参数如下:激光功率P为160~360W,扫描速率v为600~1000mm/s,扫描间距h为60-80μm,铺粉层厚t为30-50μm,光斑直径为80μm,体能量密度VED范围为140J/mm3<VED<240J/mm3,其中VED=P/vht。Further, the process parameters of laser selective melting and forming are as follows: laser power P is 160-360W, scanning speed v is 600-1000mm/s, scanning distance h is 60-80μm, powder layer thickness t is 30-50μm, spot diameter is 80 μm, and the range of volume energy density VED is 140J/mm 3 <VED<240J/mm 3 , where VED=P/vht.

进一步的,扫描策略为67°旋转扫描、往复扫描、往复交织扫描或45°旋转分区扫描。Further, the scanning strategy is 67° rotating scanning, reciprocating scanning, reciprocating interlaced scanning or 45° rotating partition scanning.

进一步的,还包括热处理步骤:将中熵合金构件升温至600℃~800℃保温12h≤t≤480h,保温结束后水冷,得到热处理后的中熵合金。Further, a heat treatment step is also included: raising the temperature of the medium-entropy alloy component to 600° C. to 800° C. for 12 hours ≤ t ≤ 480 hours, and water cooling after the heat preservation is completed to obtain the heat-treated medium-entropy alloy.

优选的,采用激光立体成形技术进行制备。Preferably, it is prepared by laser stereoforming technology.

进一步的,包括:Further, including:

步骤1,中熵合金粉末制备及预处理Step 1, preparation and pretreatment of medium entropy alloy powder

按照权利要求1所述摩尔百分比,取各元素对应的金属原料,采用真空气雾化法制备中熵合金预合金球形粉末,过筛,烘干,得到中熵合金粉末;According to the mole percentage described in claim 1, the metal raw materials corresponding to each element are taken, and the pre-alloyed spherical powder of the medium-entropy alloy is prepared by vacuum atomization, sieved, and dried to obtain the medium-entropy alloy powder;

步骤2激光立体成形NiaCobCrcAldMe析出强化型中熵合金Step 2 Laser Stereo Forming Ni a Co b Cr c Al d M e Precipitation Strengthened Medium Entropy Alloy

根据待制备的中熵合金构件的几何形状建立三维实体模型并转换为STL格式传送到激光立体成形设备,设置打印工艺参数及激光扫描路径,将中熵合金粉末送至激光立体成形设备中高能激光束所形成的熔池中,通过在基材上逐点、逐线、逐层沉积原材料的方式,打印得到中熵合金构件。Establish a three-dimensional solid model according to the geometric shape of the medium-entropy alloy component to be prepared, convert it into STL format and send it to the laser three-dimensional forming equipment, set the printing process parameters and laser scanning path, and send the medium-entropy alloy powder to the high-energy laser in the laser three-dimensional forming equipment In the molten pool formed by the beam, the medium-entropy alloy components are printed by depositing raw materials point by point, line by line, and layer by layer on the substrate.

进一步的,打印工艺参数如下:激光功率为2KW~3.5KW,扫描速率为300~800mm/min,送粉速度为5-8g/min,Z轴抬升量为0.4-1.0mm,搭接率为50%,光斑直径为3mm,扫描路径为往复交织扫描路径。Further, the printing process parameters are as follows: laser power is 2KW-3.5KW, scanning speed is 300-800mm/min, powder feeding speed is 5-8g/min, Z-axis lift is 0.4-1.0mm, lap rate is 50 %, the spot diameter is 3mm, and the scanning path is a reciprocating interlaced scanning path.

进一步的,还包括热处理步骤:将中熵合金构件升温至600℃~800℃保温3h≤t≤480h,保温结束后水冷,得到热处理后的中熵合金。Further, a heat treatment step is also included: raising the temperature of the medium-entropy alloy member to 600° C. to 800° C. for 3 hours ≤ t ≤ 480 hours, and water cooling after the heat preservation is completed to obtain the heat-treated medium-entropy alloy.

与现有技术相比,本发明具有如下的有益效果:Compared with the prior art, the present invention has the following beneficial effects:

本发明设计了适用于激光增材制造的析出强化型中熵合金,在NiaCobCrc基体中通过多主元化的形式,添加Al以及Ti、Ta、Nb或Mo元素,促进γ'相产生并显著增强γ'析出相的强化效果。规定上述Al、Ti、Ta、Nb、Mo之和小于7%,原因在于一方面克服了由于高体积分数的γ'相所导致的增材制造过程成形性差等问题,即降低了合金在激光增材制造中高的液化开裂及应变时效开裂等敏感性;另一方面能够获得具有优异强化效果的γ'析出相。本发明按照上述的配方,分别采用激光选区熔化成形技术与激光立体成形技术实现了高致密、无裂纹、综合力学性能优异的新型析出强化型中熵合金的制备。The present invention designs a precipitation-strengthened medium-entropy alloy suitable for laser additive manufacturing. In the form of multi-principalization in the Ni a Co b Cr c matrix, Al and Ti, Ta, Nb or Mo elements are added to promote γ' phase produced and significantly enhanced the strengthening effect of the γ' precipitated phase. The sum of the above-mentioned Al, Ti, Ta, Nb, and Mo is stipulated to be less than 7%. The reason is that on the one hand, the problem of poor formability in the additive manufacturing process caused by the high volume fraction of the γ' phase is overcome, that is, the alloy is reduced in the laser amplified phase. High susceptibility to liquefaction cracking and strain aging cracking in material manufacturing; on the other hand, it can obtain γ' precipitated phase with excellent strengthening effect. According to the above formula, the present invention respectively adopts the laser selective melting forming technology and the laser three-dimensional forming technology to realize the preparation of a new type of precipitation-strengthened medium-entropy alloy with high density, no cracks and excellent comprehensive mechanical properties.

进一步的,通过对激光增材制造样品进行热处理促进γ'析出相的产生,同时获得具有部分再结晶的非均匀组织,大幅度提高了本发明所设计的析出强化型中熵合金的综合力学性能,实现了激光增材制造中熵合金的进一步强韧化。Further, by heat-treating the laser additive manufacturing samples to promote the generation of γ' precipitates, and at the same time obtain a heterogeneous structure with partial recrystallization, which greatly improves the comprehensive mechanical properties of the precipitation-strengthened medium-entropy alloy designed in the present invention , to achieve further strengthening and toughening of entropy alloys in laser additive manufacturing.

附图说明Description of drawings

图1为本发明实施例1激光选区熔化成形Ni35Co35Cr25Ti3Al2中熵合金粉末形貌。Fig. 1 is the morphology of the medium-entropy alloy powder of Ni 35 Co 35 Cr 25 Ti 3 Al 2 formed by laser selective melting in Example 1 of the present invention.

图2为本发明实施例1激光选区熔化技术制备的Ni35Co35Cr25Ti3Al2中熵合金块体样品。Fig. 2 is a Ni 35 Co 35 Cr 25 Ti 3 Al 2 medium entropy alloy bulk sample prepared by laser selective melting technology in Example 1 of the present invention.

图3为本发明实施例1中激光选区熔化技术制备的Ni35Co35Cr25Ti3Al2中熵合金的致密度随体能量密度的变化规律。Fig. 3 shows the change law of the compactness of the Ni 35 Co 35 Cr 25 Ti 3 Al 2 medium entropy alloy with the bulk energy density prepared by laser selective melting technology in Example 1 of the present invention.

图4为本发明实施例1中分别采用铸造和激光选区熔化技术制备的Ni35Co35Cr25Ti3Al2中熵合金的扫描电镜图片,其中(a)为铸态,(b)为沉积态。Figure 4 is a scanning electron microscope image of the Ni 35 Co 35 Cr 25 Ti 3 Al 2 medium entropy alloy prepared by casting and laser selective melting techniques in Example 1 of the present invention, where (a) is cast and (b) is deposited state.

图5为本发明实施例1中铸态和激光选区熔化成形Ni35Co35Cr25Ti3Al2中熵合金的室温拉伸应力-应变曲线。Fig. 5 is the tensile stress-strain curve at room temperature of the as-cast and laser selective melting formed Ni 35 Co 35 Cr 25 Ti 3 Al 2 medium entropy alloys in Example 1 of the present invention.

图6为本发明实施例1激光选区熔化成形Ni35Co35Cr25Ti3Al2中熵合金经600℃/12h热处理后的扫描电镜图片(a)和透射电镜选区电子衍射图(b)。Fig. 6 is a scanning electron microscope picture (a) and a transmission electron microscope selective area electron diffraction picture (b) of a Ni 35 Co 35 Cr 25 Ti 3 Al 2 medium entropy alloy heat-treated at 600°C/12h in Example 1 of the present invention.

图7为本发明实施例1激光选区熔化成形Ni35Co35Cr25Ti3Al2中熵合金经不同热处理温度和时间后的室温拉伸应力-应变曲线。Fig. 7 is the tensile stress-strain curve at room temperature of the Ni 35 Co 35 Cr 25 Ti 3 Al 2 medium entropy alloy formed by laser selective melting in Example 1 of the present invention after different heat treatment temperatures and times.

图8为本发明实施例2激光立体成形Ni35Co35Cr25Ti3Al2中熵合金粉末形貌。Fig. 8 is the morphology of the medium entropy alloy powder of the laser stereoforming Ni 35 Co 35 Cr 25 Ti 3 Al 2 in Example 2 of the present invention.

图9为本发明实施例2激光立体成形Ni35Co35Cr25Ti3Al2中熵合金块体样品。Fig. 9 is a sample of a Ni 35 Co 35 Cr 25 Ti 3 Al 2 medium-entropy alloy bulk formed by laser stereoforming in Example 2 of the present invention.

图10为本发明实施例2中采用不同激光功率制备的Ni35Co35Cr25Ti3Al2中熵合金的室温拉伸应力-应变曲线。Fig. 10 is the tensile stress-strain curve at room temperature of the Ni 35 Co 35 Cr 25 Ti 3 Al 2 medium entropy alloy prepared with different laser powers in Example 2 of the present invention.

图11为本发明实施例2中激光立体成形Ni35Co35Cr25Ti3Al2中熵合金的微观组织特征。Fig. 11 is the microstructure characteristics of the laser stereoforming Ni 35 Co 35 Cr 25 Ti 3 Al 2 medium entropy alloy in Example 2 of the present invention.

图12为本发明实施例2中采用最优激光立体成形工艺参数制备的Ni35Co35Cr25Ti3Al2中熵合金的室温拉伸应力-应变曲线。Fig. 12 is the tensile stress-strain curve at room temperature of the Ni 35 Co 35 Cr 25 Ti 3 Al 2 medium entropy alloy prepared by using the optimal laser stereoforming process parameters in Example 2 of the present invention.

图13为本发明实施例2激光立体成形Ni35Co35Cr25Ti3Al2中熵合金经热处理后的扫描电镜图片。Fig. 13 is a scanning electron micrograph of the heat-treated medium-entropy alloy of the laser stereoforming Ni 35 Co 35 Cr 25 Ti 3 Al 2 in Example 2 of the present invention.

图14为本发明实施例2激光立体成形Ni35Co35Cr25Ti3Al2中熵合金经热处理后的显微硬度。Fig. 14 shows the microhardness of the laser stereoforming Ni 35 Co 35 Cr 25 Ti 3 Al 2 medium entropy alloy in Example 2 of the present invention after heat treatment.

图15为本发明实施例2激光立体成形Ni35Co35Cr25Ti3Al2中熵合金经700℃/3h热处理后(LSF-HT)的室温拉伸应力-应变曲线。Fig. 15 is the tensile stress-strain curve at room temperature (LSF-HT) of the laser three-dimensional formed Ni 35 Co 35 Cr 25 Ti 3 Al 2 medium entropy alloy in Example 2 of the present invention after heat treatment at 700°C/3h (LSF-HT).

具体实施方式detailed description

为了进一步理解本发明,下面结合实施例对本发明进行描述,这些描述只是进一步解释本发明的特征和优点,并非用于限制本发明的权利要求。In order to further understand the present invention, the present invention will be described below in conjunction with the examples. These descriptions are only to further explain the features and advantages of the present invention, and are not intended to limit the claims of the present invention.

本发明所述的适用于激光增材制造的强塑性优异的析出强化型中熵合金,所述析出强化型中熵合金的合金组分为NiaCobCrcAldMe,其中a、b、c、d、e分别代表对应各元素的摩尔百分比,a为余量,b=20-40at.%,c=20-25at.%,d>1at.%,e>0,d+e<7at.%,a+b+c+d+e=100at.%,所述微量元素M包括Ti、Ta、Nb、Mo中的一种或多种成分。所选用中熵合金为真空气雾化或等离子旋转电极法制备的预合金球形粉末,纯度大于99.9%。The precipitation-strengthened medium-entropy alloy with excellent strong plasticity suitable for laser additive manufacturing described in the present invention, the alloy composition of the precipitation-strengthened medium-entropy alloy is Ni a Co b Cr c Al d Me , wherein a, b, c, d, e respectively represent the mole percentage of each element, a is the balance, b=20-40at.%, c=20-25at.%, d>1at.%, e>0, d+e <7 at.%, a+b+c+d+e=100 at.%, the trace element M includes one or more of Ti, Ta, Nb, Mo. The selected medium entropy alloy is pre-alloyed spherical powder prepared by vacuum atomization or plasma rotating electrode method, and the purity is greater than 99.9%.

本发明提供了上述析出强化型中熵合金的激光选区熔化成形技术的制备方法,包括以下步骤:The present invention provides a preparation method of the above-mentioned precipitation-enhanced medium-entropy alloy by laser selective melting and forming technology, comprising the following steps:

1、中熵合金粉末制备及预处理1. Preparation and pretreatment of medium entropy alloy powder

根据所述中熵合金名义化学成分中的各元素摩尔百分比进行配比,采用真空气雾化法制备中熵合金预合金球形粉末,将预合金球形粉末进行过筛,选用粉末粒径为15-53μm。氧含量及氮含量低于300ppm,优选的氧含量为131ppm,氮含量为53ppm。进行激光选区熔化前,将预合金球形粉末进行80℃,4h的烘干处理,去除粉末中的水分,随后将其放置于激光选区熔化设备送粉缸内。Proportioning is carried out according to the mole percentage of each element in the nominal chemical composition of the medium-entropy alloy, and the pre-alloyed spherical powder of the medium-entropy alloy is prepared by the vacuum atomization method, and the pre-alloyed spherical powder is sieved, and the particle size of the selected powder is 15- 53 μm. The oxygen content and nitrogen content are less than 300ppm, the preferred oxygen content is 131ppm, and the nitrogen content is 53ppm. Before laser selective melting, the pre-alloyed spherical powder is dried at 80°C for 4 hours to remove the moisture in the powder, and then placed in the powder feeding cylinder of the laser selective melting equipment.

2、基板表面处理2. Substrate surface treatment

选取不锈钢或碳钢基板,打磨待沉积面,并依次用丙酮和酒精清洗以去除表面油污,随后吹干,将基板安装在成型平台上并进行调平。在打印之前,将基板预热到100℃-200℃,优选的基板预热温度为200℃。Select a stainless steel or carbon steel substrate, polish the surface to be deposited, and clean it with acetone and alcohol in order to remove surface oil, then dry it, install the substrate on the forming platform and level it. Before printing, the substrate is preheated to 100°C-200°C, and the preferred substrate preheating temperature is 200°C.

3、激光选区熔化成形NiaCobCrcAldMe析出强化型中熵合金3. Ni a Co b Cr c Al d Me precipitation-strengthened medium-entropy alloy formed by laser selective melting

在计算机上建立三维实体模型并转换为STL格式的文件,将其导入激光选区熔化成形设备的建造软件中,进行分层处理。激光选区熔化成形的工艺参数如下:激光功率P为160~360W,扫描速率v为600~1000mm/s,扫描间距h为60-80μm,铺粉层厚t为30-50μm,光斑直径为80μm,扫描策略可选择67°旋转扫描、往复扫描、往复交织扫描以及45°旋转分区扫描路径。打印之前,通入纯度为99.99wt.%的高纯氩气,使成形舱室内氧气含量低于300ppm。根据所设定的激光选区熔化成形的工艺参数及扫描路径,将NiaCobCrcAldMe中熵合金预合金球形粉末逐层熔化成形,制备出块体样品。本发明采用激光选区熔化成形的方式制备NiaCobCrcAldMe析出强化型中熵合金,通过选用优化的激光选区熔化成形工艺参数,即高的体能量密度VED(140J/mm3<VED<240J/mm3,VED=P/vht),可以极大提高打印合金的致密度,进而提高其综合力学性能,实现高致密、无裂纹、性能优异的析出强化型中熵合金复杂结构件的一体化精密成形。Create a three-dimensional solid model on the computer and convert it into a file in STL format, and import it into the construction software of the laser selection melting forming equipment for layering processing. The process parameters of laser selective melting and forming are as follows: laser power P is 160-360W, scanning speed v is 600-1000mm/s, scanning distance h is 60-80μm, powder layer thickness t is 30-50μm, spot diameter is 80μm, The scanning strategy can choose 67° rotating scanning, reciprocating scanning, reciprocating interleaving scanning and 45° rotating partition scanning path. Before printing, high-purity argon gas with a purity of 99.99wt.% is injected to keep the oxygen content in the forming chamber below 300ppm. According to the set process parameters and scanning path of laser selective melting forming, Ni a Co b Cr c Al d Me mesophilic alloy pre-alloyed spherical powder was melted layer by layer to prepare block samples. In the present invention, Ni a Co b Cr c Al d Me precipitation-enhanced medium-entropy alloy is prepared by laser selective melting and forming, and by selecting optimized laser selective melting and forming process parameters, that is, high volume energy density VED ( 140J /mm 3 <VED<240J/mm 3 , VED=P/vht), which can greatly increase the density of the printed alloy, thereby improving its comprehensive mechanical properties, and realizing a high-density, crack-free, and excellent-performance precipitation-strengthened medium-entropy alloy complex structure Integrated precision forming of parts.

本发明还提供了上述析出强化型中熵合金的激光立体成形技术的制备方法,包括以下步骤:The present invention also provides a preparation method of the above-mentioned precipitation-strengthened medium-entropy alloy by laser three-dimensional forming technology, comprising the following steps:

1、中熵合金粉末制备及预处理1. Preparation and pretreatment of medium entropy alloy powder

根据所述中熵合金名义化学成分中的各元素摩尔百分比进行配比,采用真空气雾化法制备中熵合金预合金球形粉末,将预合金球形粉末进行过筛,选用粉末粒径为45-150μm。氧含量及氮含量低于300ppm,优选的氧含量为131ppm,氮含量为53ppm。进行激光立体成形实验前,将粉末烘干处理以避免粉末中吸附的水分对材料成形产生的影响,随后将粉末放置于激光立体成形设备送粉器内。Proportioning is carried out according to the mole percentage of each element in the nominal chemical composition of the medium-entropy alloy, and the pre-alloyed spherical powder of the medium-entropy alloy is prepared by the vacuum atomization method, and the pre-alloyed spherical powder is sieved, and the particle size of the selected powder is 45- 150 μm. The oxygen content and nitrogen content are less than 300ppm, the preferred oxygen content is 131ppm, and the nitrogen content is 53ppm. Before the laser three-dimensional forming experiment, the powder was dried to avoid the influence of the moisture absorbed in the powder on the material forming, and then the powder was placed in the powder feeder of the laser three-dimensional forming equipment.

2、基板表面处理2. Substrate surface treatment

选取不锈钢或碳钢基板,打磨待沉积面,并依次用丙酮和酒精清洗以去除表面油污,随后吹干,将基板固定于成型平台。Select a stainless steel or carbon steel substrate, polish the surface to be deposited, and clean it with acetone and alcohol in order to remove surface oil, then dry it, and fix the substrate on the forming platform.

3、激光立体成形NiaCobCrcAldMe析出强化型中熵合金3. Laser three-dimensional forming Ni a Co b Cr c Al d Me precipitation strengthening type medium entropy alloy

根据中熵合金构件的几何形状在计算机上建立三维实体模型并转换为STL格式传送到激光成形设备,设置打印工艺参数及激光扫描路径,在数控系统的控制下,中熵合金球形粉末经同轴送粉喷嘴送至高能激光束所形成的熔池中,通过在基材上逐点、逐线、逐层沉积原材料的方式,实现特定形状及尺寸的复杂构件成形。上述激光立体成形的工艺参数如下:激光功率为2KW~3.5KW,扫描速率为300~800mm/min,送粉速度为5-8g/min,Z轴抬升量为0.4-1.0mm,搭接率为50%,光斑直径为3mm,扫描策略选择往复交织扫描,即在同一沉积层,扫描路径呈S型,相邻沉积层,扫描方向旋转90°。上述激光立体成形过程采用高纯氩气作为保护气体和载粉气体,打印过程中氧气含量低于2000ppm。根据上述设定的激光立体成形的工艺参数及扫描路径,将NiaCobCrcAldMe中熵合金粉末逐层熔化成形,制备出块体样品。通过优化激光功率、扫描速度、送粉速度以及Z轴抬升量,可以提高打印合金的质量并优化微观组织,进一步提高其综合力学性能,实现全致密、无缺陷、综合性能优异的析出强化型中熵合金复杂结构件的一体化精密成形。According to the geometric shape of the medium-entropy alloy component, a three-dimensional solid model is established on the computer and converted into STL format and sent to the laser forming equipment. The printing process parameters and laser scanning path are set. Under the control of the numerical control system, the medium-entropy alloy spherical powder is coaxially The powder feeding nozzle is sent to the molten pool formed by the high-energy laser beam, and the formation of complex components of specific shapes and sizes is realized by depositing raw materials point by point, line by line, and layer by layer on the substrate. The process parameters of the above laser three-dimensional forming are as follows: laser power is 2KW ~ 3.5KW, scanning speed is 300 ~ 800mm/min, powder feeding speed is 5-8g/min, Z-axis lift is 0.4-1.0mm, lap rate 50%, the diameter of the spot is 3mm, and the scanning strategy is reciprocating and interlaced scanning, that is, in the same deposition layer, the scanning path is S-shaped, and the scanning direction is rotated 90° for adjacent deposition layers. The above-mentioned laser three-dimensional forming process uses high-purity argon as the protective gas and powder-carrying gas, and the oxygen content in the printing process is lower than 2000ppm. According to the process parameters and scanning path of the laser stereoforming set above, the Ni a Co b Cr c Al d Me mestropic alloy powder was melted layer by layer to prepare a block sample. By optimizing the laser power, scanning speed, powder feeding speed and Z-axis lift, the quality of the printed alloy can be improved and the microstructure can be optimized to further improve its comprehensive mechanical properties and achieve a precipitation-strengthened medium with full density, no defects and excellent comprehensive performance. Integrated precision forming of complex structural parts of entropy alloys.

本发明还提供了上述激光增材制造技术制备NiaCobCrcAldMe析出强化型中熵合金的热处理方法,包括以下步骤:The present invention also provides a heat treatment method for preparing Ni a Co b Cr c Al d Me precipitation-enhanced medium-entropy alloy by the above-mentioned laser additive manufacturing technology, comprising the following steps:

在本发明中,为促进高体积分数的析出相产生,对激光增材制造NiaCobCrcAldMe型析出强化型中熵合金进行热处理。所述热处理的方式优选包括:将激光增材制造制备的NiaCobCrcAldMe析出强化型中熵合金升温至600℃~800℃保温,所选时间12h≤t≤480h(激光选区熔化成形)或者3h≤t≤480h(激光立体成形),保温结束后水冷,得到热处理后的中熵合金。通过对上述激光增材制造NiaCobCrcAldMe中熵合金进行热处理,可有效促进高体积分数的析出相的析出,同时得到不完全再结晶的组织,进一步优化激光增材制造NiaCobCrcAldMe中熵合金的综合力学性能,实现高强高韧中熵合金的制备。In the present invention, in order to promote the generation of precipitates with a high volume fraction, heat treatment is performed on the Ni a Co b Cr c Al d Me type precipitation-strengthened medium-entropy alloy produced by laser additive manufacturing. The heat treatment method preferably includes: heating the Ni a Co b Cr c Al d Me precipitation-strengthened medium-entropy alloy prepared by laser additive manufacturing to 600°C-800°C and keeping it warm for a selected time of 12h≤t≤480h (laser Selective melting and forming) or 3h≤t≤480h (laser three-dimensional forming), water cooling after heat preservation, to obtain a heat-treated medium-entropy alloy. Heat treatment of the above-mentioned laser additive manufacturing Ni a Co b Cr c Al d Me medium entropy alloy can effectively promote the precipitation of precipitated phases with a high volume fraction, and at the same time obtain an incompletely recrystallized structure, further optimizing laser additive manufacturing The comprehensive mechanical properties of Ni a Co b Cr c Al d Me e medium entropy alloy, to achieve the preparation of high strength and high toughness medium entropy alloy.

实施例1Example 1

一种适用于激光增材制造的析出强化型中熵合金,该中熵合金的化学式为Ni35Co35Cr25Ti3Al2;其中,各元素的比例为摩尔百分比。所选用中熵合金为气雾化预合金球形粉末,纯度大于99.9%。A precipitation-strengthened medium-entropy alloy suitable for laser additive manufacturing. The chemical formula of the medium-entropy alloy is Ni 35 Co 35 Cr 25 Ti 3 Al 2 ; wherein, the ratio of each element is a mole percentage. The selected medium entropy alloy is a gas-atomized pre-alloyed spherical powder with a purity greater than 99.9%.

本实施例1采用激光选区熔化技术制备中熵合金成形过程如下:In Example 1, the forming process of the medium entropy alloy prepared by laser selective melting technology is as follows:

1、中熵合金粉末制备及预处理1. Preparation and pretreatment of medium entropy alloy powder

将根据上述中熵合金名义化学成分中的各元素摩尔比进行配比,采用真空气雾化法制备中熵合金预合金球形粉末,将预合金粉末进行过筛,选用粒粉末粒径为15-53μm,其典型形态如图1所示。氧含量为131ppm,氮含量为53ppm。进行激光选区熔化前,将粉末进行80℃,4h的烘干处理,去除粉末中的水分。随后将其放置于激光选区熔化设备送粉缸内。According to the molar ratio of each element in the nominal chemical composition of the above-mentioned medium-entropy alloy, the medium-entropy alloy pre-alloyed spherical powder is prepared by vacuum atomization method, and the pre-alloyed powder is sieved, and the particle size of the selected powder is 15- 53 μm, and its typical shape is shown in Figure 1. The oxygen content was 131 ppm and the nitrogen content was 53 ppm. Before laser selective melting, the powder is dried at 80°C for 4 hours to remove the moisture in the powder. Then it is placed in the powder feeding cylinder of the laser selective melting equipment.

2、基板表面处理2. Substrate surface treatment

选取316L不锈钢基板,打磨待沉积面,并依次用丙酮和酒精清洗以去除表面油污,随后吹干,将基板安装在成型平台上并进行调平。在打印之前,将基板预热到200℃。Select a 316L stainless steel substrate, polish the surface to be deposited, and clean it with acetone and alcohol in order to remove surface oil, then dry it, install the substrate on the forming platform and level it. Before printing, the substrate was preheated to 200 °C.

3、激光选区熔化成形Ni35Co35Cr25Ti3Al2析出强化型中熵合金3. Ni 35 Co 35 Cr 25 Ti 3 Al 2 precipitation-strengthened medium-entropy alloy formed by laser selective melting

在计算机上建立三维实体模型并转换为STL格式的文件,将其导入选区激光熔化成形设备的建造软件中,进行分层处理。激光选区熔化成形的工艺参数如下:激光功率为160~360W,扫描速率为600~1000mm/s,扫描间距为60-80μm,铺粉层厚为30-50μm,光斑直径为80μm,扫描策略为67°旋转扫描。打印之前,通入纯度为99.99wt.%的高纯氩气,使成形舱室内氧气含量低于300ppm。Create a three-dimensional solid model on the computer and convert it into a file in STL format, and import it into the construction software of the laser melting forming equipment for layering. The process parameters of laser selective melting and forming are as follows: laser power is 160-360W, scanning speed is 600-1000mm/s, scanning distance is 60-80μm, powder layer thickness is 30-50μm, spot diameter is 80μm, scanning strategy is 67 ° Rotate scan. Before printing, high-purity argon gas with a purity of 99.99wt.% is injected to keep the oxygen content in the forming chamber below 300ppm.

通过表1所示参数,调整激光功率、扫描速率、扫描间距,固定铺粉层厚为30μm进行激光选区熔化成形实验,得到激光选区熔化成形样品如图2所示。并对样品致密度进行测试,结果如图3所示。According to the parameters shown in Table 1, the laser power, scanning rate, and scanning distance were adjusted, and the thickness of the powder layer was fixed at 30 μm to carry out the laser selective melting forming experiment. The laser selective melting forming sample was obtained as shown in Figure 2. The density of the samples was tested, and the results are shown in Figure 3.

表1实验参数Table 1 Experimental parameters

Figure BDA0003480584020000081
Figure BDA0003480584020000081

Figure BDA0003480584020000091
Figure BDA0003480584020000091

通过表1所示实验确定了最优的工艺参数:激光功率为320W,扫描速度为1000mm/s,扫描间距为70μm,铺粉层厚为30μm。The optimal process parameters are determined through the experiments shown in Table 1: the laser power is 320W, the scanning speed is 1000mm/s, the scanning distance is 70μm, and the powder layer thickness is 30μm.

4、激光选区熔化成形样品组织表征及性能测试4. Structural characterization and performance testing of laser selective melting forming samples

采用扫描电子显微镜(SEM)观察在最优激光选区熔化参数成形样品的显微组织,如图4(b)所示,合金成形质量较好,未观察到裂纹等缺陷,经测试得到成形件相对致密度大于99.6%。与铸态(采用真空电弧熔炼法制备)组织相比,激光选区熔化沉积所制备的Ni35Co35Cr25Ti3Al2析出强化型中熵合金微观组织更加细小均匀。实施例1选用最优工艺参数所成形的激光选区熔化Ni35Co35Cr25Ti3Al2中熵合金(SLM)的室温屈服强度为671MPa,抗拉强度为913MPa,延伸率为36%,硬度为310HV。其强度远高于铸态,拉伸塑性与铸态相当,如图5所示,其中Ni35Co35Cr25Ti3Al2中熵合金铸态(Cast)的屈服强度为342MPa,抗拉强度为648MPa,延伸率为38%。A scanning electron microscope (SEM) was used to observe the microstructure of the sample formed with the optimal laser selective melting parameters. As shown in Figure 4(b), the alloy forming quality was good, and no defects such as cracks were observed. Density greater than 99.6%. Compared with the as-cast (prepared by vacuum arc melting method), the microstructure of Ni 35 Co 35 Cr 25 Ti 3 Al 2 precipitation-strengthened medium-entropy alloy prepared by laser selective melting deposition is finer and more uniform. Example 1 The room temperature yield strength of the laser selective melting Ni 35 Co 35 Cr 25 Ti 3 Al 2 medium entropy alloy (SLM) formed by selecting the optimal process parameters is 671MPa, the tensile strength is 913MPa, the elongation is 36%, and the hardness It is 310HV. Its strength is much higher than that of the as - cast state, and its tensile plasticity is equivalent to that of the as - cast state. It is 648MPa and the elongation is 38%.

5、激光选区熔化成形Ni35Co35Cr25Ti3Al2中熵合金热处理5. Heat treatment of Ni 35 Co 35 Cr 25 Ti 3 Al 2 medium entropy alloy formed by laser selective melting

通过时效处理促进激光选区熔化成形Ni35Co35Cr25Ti3Al2中熵合金析出相的产生从而实现进一步的强韧化。在本发明中,所述热处理的方式包括,将采用最优激光选区熔化参数成形的Ni35Co35Cr25Ti3Al2中熵合金升温至600℃~800℃保温,所选时间为12h≤t≤480h,保温结束后水冷,得到热处理后的中熵合金。The aging treatment promotes the formation of entropy alloy precipitates in Ni 35 Co 35 Cr 25 Ti 3 Al 2 formed by laser selective melting to achieve further strengthening and toughening. In the present invention, the heat treatment method includes raising the temperature of the Ni 35 Co 35 Cr 25 Ti 3 Al 2 medium-entropy alloy formed with optimal laser selective melting parameters to 600°C-800°C and keeping it warm for a selected time of 12h≤ t ≤ 480h, water cooling after heat preservation, to obtain a heat-treated medium entropy alloy.

具体进行三组实验,一组实验中,在600℃热处理12h,另一组实验中,在700℃热处理12h,再一组实验中,在700℃热处理480h。Specifically, three groups of experiments were carried out. In one group of experiments, heat treatment was performed at 600° C. for 12 hours, in another group of experiments, heat treatment was performed at 700° C. for 12 hours, and in another group of experiments, heat treatment was performed at 700° C. for 480 hours.

图6为激光选区熔化成形Ni35Co35Cr25Ti3Al2中熵合金经600℃/12h热处理后的扫描电镜图片(a)和透射电镜选区电子衍射图(b),从图6(a)中可以观察到沉积态组织发生了部分再结晶,图6(b)中可同时观察到FCC相和γ'析出相的衍射斑点。对激光选区熔化成形Ni35Co35Cr25Ti3Al2中熵合金热处理样品进行室温拉伸性能测试,结果如图7所示,结果表明,热处理后强度大幅度提高,沉积态经700℃/480h热处理后屈服强度可达到1098MPa,抗拉强度为1466MPa,延伸率为25%,该室温拉伸性能是迄今为止激光增材制造高/中熵合金的最高水平。Figure 6 is the scanning electron microscope image (a) and the transmission electron microscope selected area electron diffraction pattern (b) of the Ni 35 Co 35 Cr 25 Ti 3 Al 2 medium entropy alloy formed by laser selective melting and heat treatment at 600 °C/12h, from Figure 6 (a ), it can be observed that the deposited structure has partially recrystallized, and the diffraction spots of the FCC phase and the γ' precipitated phase can be observed simultaneously in Figure 6(b). The room temperature tensile property test was carried out on the heat-treated samples of Ni 35 Co 35 Cr 25 Ti 3 Al 2 medium-entropy alloys formed by laser selective melting. After 480h heat treatment, the yield strength can reach 1098MPa, the tensile strength is 1466MPa, and the elongation is 25%.

实施例2Example 2

一种适用于激光增材制造的析出强化型中熵合金,该中熵合金的化学式为Ni35Co35Cr25Ti3Al2;其中,各元素的比例为摩尔百分比。所选用中熵合金为气雾化预合金球形粉末,纯度大于99.9%。A precipitation-strengthened medium-entropy alloy suitable for laser additive manufacturing. The chemical formula of the medium-entropy alloy is Ni 35 Co 35 Cr 25 Ti 3 Al 2 ; wherein, the ratio of each element is a mole percentage. The selected medium entropy alloy is a gas-atomized pre-alloyed spherical powder with a purity greater than 99.9%.

本实施例2采用激光立体成形技术制备中熵合金成形过程如下:Present embodiment 2 adopts laser three-dimensional forming technology to prepare medium entropy alloy forming process as follows:

1、中熵合金粉末制备及预处理1. Preparation and pretreatment of medium entropy alloy powder

将根据所述中熵合金名义化学成分中的各元素摩尔比进行配比,采用真空气雾化法制备中熵合金预合金球形粉末,将预合金球形粉末进行过筛,选用粉末粒径为45-150μm,其典型形貌如图8所示。氧含量为131ppm,氮含量为53ppm。进行激光立体成形实验前,将粉末烘干处理以避免粉末中吸附的水分对材料成形产生的影响,随后将粉末放置于激光立体成形设备送粉器内。According to the molar ratio of each element in the nominal chemical composition of the medium-entropy alloy, the medium-entropy alloy pre-alloyed spherical powder is prepared by vacuum atomization method, and the pre-alloyed spherical powder is sieved, and the particle size of the powder is 45 -150μm, its typical morphology is shown in Figure 8. The oxygen content was 131 ppm and the nitrogen content was 53 ppm. Before the laser three-dimensional forming experiment, the powder was dried to avoid the influence of the moisture absorbed in the powder on the material forming, and then the powder was placed in the powder feeder of the laser three-dimensional forming equipment.

2、基板表面处理2. Substrate surface treatment

选取316L不锈钢基板,将待沉积面打磨,并依次用丙酮和酒精清洗以去除表面油污,随后吹干,将基板固定夹在成型平台。Select a 316L stainless steel substrate, polish the surface to be deposited, and clean it with acetone and alcohol in order to remove surface oil, then dry it, and fix the substrate on the forming platform.

3、激光立体成形Ni35Co35Cr25Ti3Al2析出强化型中熵合金3. Laser three-dimensional forming Ni 35 Co 35 Cr 25 Ti 3 Al 2 precipitation-strengthened medium-entropy alloy

根据中熵合金构件的几何形状在计算机上建立三维实体模型并转换为STL格式传送到激光成形设备,设置打印工艺参数及激光扫描路径,在数控系统的控制下,中熵合金粉末经同轴送粉喷嘴送至高能激光束所形成的熔池中,通过在基材上逐点、逐线、逐层沉积原材料的方式,实现特定形状及尺寸的复杂构件成形。上述激光立体成形的工艺参数如下:激光功率为2KW~3.5KW,扫描速率为300~800mm/min,送粉速度为5-8g/min,Z轴抬升量为0.4-1.0mm,搭接率为50%,光斑直径为3mm,扫描策略选择往复交织扫描,即在同一沉积层,扫描路径呈S型,相邻沉积层,扫描方向旋转90°。上述激光立体成形过程采用高纯氩气作为保护气体和载粉气体,打印过程中氧气含量低于2000ppm。According to the geometric shape of the medium-entropy alloy component, a three-dimensional solid model is established on the computer and converted into STL format and sent to the laser forming equipment. The printing process parameters and laser scanning path are set. Under the control of the numerical control system, the medium-entropy alloy powder is sent coaxially. The powder nozzle is sent to the molten pool formed by the high-energy laser beam, and the complex components of specific shapes and sizes are formed by depositing raw materials point by point, line by line, and layer by layer on the substrate. The process parameters of the above laser three-dimensional forming are as follows: laser power is 2KW ~ 3.5KW, scanning speed is 300 ~ 800mm/min, powder feeding speed is 5-8g/min, Z-axis lift is 0.4-1.0mm, lap rate 50%, the diameter of the spot is 3mm, and the scanning strategy is reciprocating and interlaced scanning, that is, in the same deposition layer, the scanning path is S-shaped, and the scanning direction is rotated 90° for adjacent deposition layers. The above-mentioned laser three-dimensional forming process uses high-purity argon as the protective gas and powder-carrying gas, and the oxygen content in the printing process is lower than 2000ppm.

调整激光功率、扫描速率、送粉速度、Z轴抬升量进行最优工艺探索,并打印具有不同线能量密度的块体样品,具体采用的工艺参数如表2所示。Adjust the laser power, scanning rate, powder feeding speed, and Z-axis lift to explore the optimal process, and print block samples with different linear energy densities. The specific process parameters used are shown in Table 2.

表2实施例2的具体实验参数The concrete experimental parameter of table 2 embodiment 2

Figure BDA0003480584020000111
Figure BDA0003480584020000111

采用以上激光立体成形工艺参数制备了Ni35Co35Cr25Ti3Al2中熵合金块体样品,其典型宏观形貌如图9所示。对3个样品分别进行室温拉伸性能测试,结果如图10所示。通过力学性能测试结果,确定了最优的工艺参数:激光功率为2800W,扫描速度为300mm/min,送粉速度为5g/min,Z轴抬升量0.5mm,搭接率为50%。The Ni 35 Co 35 Cr 25 Ti 3 Al 2 medium entropy alloy bulk sample was prepared using the above laser stereoforming process parameters, and its typical macroscopic morphology is shown in Figure 9. Three samples were tested for tensile properties at room temperature, and the results are shown in Figure 10. Through the mechanical performance test results, the optimal process parameters are determined: laser power is 2800W, scanning speed is 300mm/min, powder feeding speed is 5g/min, Z-axis lift is 0.5mm, and the overlap rate is 50%.

4、激光立体成形样品组织表征及性能测试4. Structural characterization and performance test of laser three-dimensional forming samples

采用电子背散射衍射(EBSD)和扫描电子显微镜(SEM)观察最优参数下成形样品的显微组织,如图11所示,合金成形质量较好,未观察到裂纹,孔隙,融合不良等缺陷。并且采用激光立体成形技术制备的Ni35Co35Cr25Ti3Al2中熵合金组织中存在少量的γ'纳米级析出相的产生,如图11(b)所示。采用优选的工艺参数制备的激光立体成形Ni35Co35Cr25Ti3Al2中熵合金的室温力学性能如图12所示,沿建造方向(纵向)屈服强度为723MPa,抗拉强度为1078MPa,延伸率为39%,硬度为355HV;沿扫描方向(横向)屈服强度为566MPa,抗拉强度为1011MPa,延伸率为47%,硬度为284HV。与传统铸造相比,采用激光立体成形方法所制备的Ni35Co35Cr25Ti3Al2中熵合金样品具有高的强塑性结合。Electron backscatter diffraction (EBSD) and scanning electron microscopy (SEM) were used to observe the microstructure of the formed sample under optimal parameters. As shown in Figure 11, the alloy forming quality is good, and no cracks, pores, poor fusion and other defects are observed. . And there is a small amount of γ' nano-scale precipitates in the Ni 35 Co 35 Cr 25 Ti 3 Al 2 entropy alloy microstructure prepared by laser stereoforming technology, as shown in Figure 11(b). The room temperature mechanical properties of the laser stereoforming Ni 35 Co 35 Cr 25 Ti 3 Al 2 medium-entropy alloy prepared with optimal process parameters are shown in Figure 12. The yield strength along the construction direction (longitudinal direction) is 723MPa, and the tensile strength is 1078MPa. The elongation is 39%, the hardness is 355HV; the yield strength along the scanning direction (transverse direction) is 566MPa, the tensile strength is 1011MPa, the elongation is 47%, and the hardness is 284HV. Compared with traditional casting, the Ni 35 Co 35 Cr 25 Ti 3 Al 2 medium entropy alloy sample prepared by laser stereoforming method has high strong plastic bonding.

5、激光立体成形Ni35Co35Cr25Ti3Al2中熵合金热处理。5. Laser stereoforming Ni 35 Co 35 Cr 25 Ti 3 Al 2 medium entropy alloy heat treatment.

进一步通过时效处理促进激光立体成形Ni35Co35Cr25Ti3Al2中熵合金析出相的产生从而实现进一步的强韧化。在本发明中,所述热处理的方式包括,将最优工艺参数下激光立体成形的Ni35Co35Cr25Ti3Al2中熵合金升温至700℃保温,所选时间为3h,保温结束后水冷,得到热处理后的中熵合金。Furthermore, the aging treatment is used to promote the generation of entropy alloy precipitates in the laser stereoforming Ni 35 Co 35 Cr 25 Ti 3 Al 2 to achieve further strengthening and toughening. In the present invention, the heat treatment method includes raising the temperature of the Ni 35 Co 35 Cr 25 Ti 3 Al 2 medium-entropy alloy formed by laser stereoforming under the optimal process parameters to 700°C for a selected time of 3 hours. Water cooling to obtain a heat-treated medium entropy alloy.

图13显示了激光立体成形Ni35Co35Cr25Ti3Al2中熵合金经700℃/3h热处理后的高倍扫描电镜图片,可以看到,相比于原始沉积态组织,析出相的体积分数显著增加。图14显示了采用不同激光功率制备的Ni35Co35Cr25Ti3Al2中熵合金在热处理后的显微硬度变化规律。经热处理后,由于高体积分数的析出相产生,可以看到硬度明显提高,激光功率为2.8KW的样品经700℃/3h热处理后的硬度约为415HV。图15显示了激光功率为2.8KW的Ni35Co35Cr25Ti3Al2中熵合金在700℃/3h热处理后的拉伸性能,其屈服强度为808MPa,抗拉强度为1168MPa,延伸率为32%,相比于沉积态样品,由于析出相的产生,其强度有了显著的提升。Figure 13 shows the high-magnification scanning electron microscope pictures of the laser stereoforming Ni 35 Co 35 Cr 25 Ti 3 Al 2 medium entropy alloy after heat treatment at 700℃/3h. It can be seen that compared with the original deposited state structure, the volume fraction of the precipitated phase A significant increase. Fig. 14 shows the variation law of microhardness after heat treatment of Ni 35 Co 35 Cr 25 Ti 3 Al 2 medium entropy alloys prepared with different laser powers. After heat treatment, due to the high volume fraction of precipitates, it can be seen that the hardness is significantly improved. The hardness of the sample with a laser power of 2.8KW is about 415HV after heat treatment at 700℃/3h. Figure 15 shows the tensile properties of the Ni 35 Co 35 Cr 25 Ti 3 Al 2 medium entropy alloy with a laser power of 2.8KW after heat treatment at 700°C/3h. The yield strength is 808MPa, the tensile strength is 1168MPa, and the elongation is 32%, compared with the as-deposited sample, its strength has been significantly improved due to the generation of precipitated phases.

Claims (6)

1.适用于激光增材制造的析出强化型中熵合金,其特征在于,所述析出强化型中熵合金为NiaCobCrcAldMe,其中,M为Ti、Ta、Nb和Mo中的一种或多种元素,a、b、c、d和e分别代表对应各元素的摩尔百分比,b=20%~40%,c=20%~25%,d > 1%,e >0,d+e < 7%,a+b+c+d+e=100%;1. The precipitation strengthening type medium entropy alloy suitable for laser additive manufacturing is characterized in that, the precipitation strengthening type medium entropy alloy is Ni a Co b Cr c Al d Me , wherein, M is Ti, Ta, Nb and One or more elements in Mo, a, b, c, d and e respectively represent the mole percentage of each element, b=20%~40%, c=20%~25%, d > 1%, e >0, d+e < 7%, a+b+c+d+e=100%; 所述析出强化型中熵合金采用激光选区熔化成形技术进行制备;包括:The precipitation-strengthened medium-entropy alloy is prepared by laser selective melting forming technology; including: 步骤1,中熵合金粉末制备及预处理Step 1, preparation and pretreatment of medium entropy alloy powder 按照上述摩尔百分比,取各元素对应的金属原料,采用真空气雾化法制备中熵合金预合金球形粉末,过筛,烘干,得到中熵合金粉末;According to the above molar percentages, the metal raw materials corresponding to each element are taken, and a medium-entropy alloy pre-alloyed spherical powder is prepared by a vacuum atomization method, sieved, and dried to obtain a medium-entropy alloy powder; 步骤2,激光选区熔化成形NiaCobCrcAldMe析出强化型中熵合金Step 2, laser selective melting forming Ni a Co b Cr c Al d Me precipitation strengthened medium entropy alloy 根据待制备的中熵合金构件的几何形状建立三维实体模型并转换为STL格式的文件,导入激光选区熔化成形设备的建造软件中,进行分层处理;通入高纯氩气,使成形舱室内氧气含量低于300ppm,根据所设定的激光选区熔化成形的工艺参数及扫描策略,将中熵合金粉末逐层熔化成形,制备得到中熵合金构件;Establish a three-dimensional solid model according to the geometric shape of the medium-entropy alloy component to be prepared and convert it into a file in STL format, import it into the construction software of the laser selective melting forming equipment, and perform layered processing; inject high-purity argon gas to make the forming chamber The oxygen content is lower than 300ppm. According to the set process parameters and scanning strategy of laser selective melting and forming, the medium entropy alloy powder is melted layer by layer to prepare the medium entropy alloy components; 激光选区熔化成形的工艺参数如下:激光功率P为160~360W,扫描速率v为600~1000mm/s,扫描间距h为60~80μm,铺粉层厚t为30~50μm,光斑直径为80μm,体能量密度VED范围为140J/mm3 < VED < 240J/mm3,其中VED=P/vht;The process parameters of laser selective melting and forming are as follows: laser power P is 160-360W, scanning speed v is 600-1000mm/s, scanning distance h is 60-80μm, powder layer thickness t is 30-50μm, and spot diameter is 80μm. The range of volume energy density VED is 140J/mm 3 < VED < 240J/mm 3 , where VED=P/vht; 或者,所述析出强化型中熵合金采用激光立体成形技术进行制备;包括:Alternatively, the precipitation-strengthened medium-entropy alloy is prepared by laser stereoforming technology; including: 步骤1,中熵合金粉末制备及预处理Step 1, preparation and pretreatment of medium entropy alloy powder 按照上述摩尔百分比,取各元素对应的金属原料,采用真空气雾化法制备中熵合金预合金球形粉末,过筛,烘干,得到中熵合金粉末;According to the above molar percentages, the metal raw materials corresponding to each element are taken, and a medium-entropy alloy pre-alloyed spherical powder is prepared by a vacuum atomization method, sieved, and dried to obtain a medium-entropy alloy powder; 步骤2激光立体成形NiaCobCrcAldMe析出强化型中熵合金Step 2 Laser Stereo Forming Ni a Co b Cr c Al d M e Precipitation Strengthened Medium Entropy Alloy 根据待制备的中熵合金构件的几何形状建立三维实体模型并转换为STL格式传送到激光立体成形设备,设置打印工艺参数及激光扫描路径,将中熵合金粉末送至激光立体成形设备中高能激光束所形成的熔池中,通过在基材上逐点、逐线、逐层沉积原材料的方式,打印得到中熵合金构件;Establish a three-dimensional solid model according to the geometric shape of the medium-entropy alloy component to be prepared, convert it into STL format and send it to the laser three-dimensional forming equipment, set the printing process parameters and laser scanning path, and send the medium-entropy alloy powder to the high-energy laser in the laser three-dimensional forming equipment In the molten pool formed by the beam, the medium-entropy alloy components are printed by depositing raw materials point by point, line by line, and layer by layer on the substrate; 打印工艺参数如下:激光功率为2kW~3.5kW,扫描速率为300~800mm/min,送粉速度为5~8g/min,Z轴抬升量为0.4~1.0mm,搭接率为50%,光斑直径为3mm,扫描路径为往复交织扫描路径。The printing process parameters are as follows: laser power is 2kW~3.5kW, scanning speed is 300~800mm/min, powder feeding speed is 5~8g/min, Z-axis lift is 0.4~1.0mm, overlapping rate is 50%, spot The diameter is 3mm, and the scanning path is a reciprocating interweaving scanning path. 2.权利要求1所述的适用于激光增材制造的析出强化型中熵合金的制备方法,其特征在于,采用激光选区熔化成形技术进行制备;包括:2. The preparation method of the precipitation-strengthened medium-entropy alloy suitable for laser additive manufacturing according to claim 1, characterized in that, it is prepared by laser selective melting forming technology; comprising: 步骤1,中熵合金粉末制备及预处理Step 1, preparation and pretreatment of medium entropy alloy powder 按照权利要求1所述摩尔百分比,取各元素对应的金属原料,采用真空气雾化法制备中熵合金预合金球形粉末,过筛,烘干,得到中熵合金粉末;According to the mole percentage described in claim 1, the metal raw materials corresponding to each element are taken, and the pre-alloyed spherical powder of the medium-entropy alloy is prepared by vacuum atomization, sieved, and dried to obtain the medium-entropy alloy powder; 步骤2,激光选区熔化成形NiaCobCrcAldMe析出强化型中熵合金Step 2, laser selective melting forming Ni a Co b Cr c Al d Me precipitation strengthened medium entropy alloy 根据待制备的中熵合金构件的几何形状建立三维实体模型并转换为STL格式的文件,导入激光选区熔化成形设备的建造软件中,进行分层处理;通入高纯氩气,使成形舱室内氧气含量低于300ppm,根据所设定的激光选区熔化成形的工艺参数及扫描策略,将中熵合金粉末逐层熔化成形,制备得到中熵合金构件;Establish a three-dimensional solid model according to the geometric shape of the medium-entropy alloy component to be prepared and convert it into a file in STL format, import it into the construction software of the laser selective melting forming equipment, and perform layered processing; inject high-purity argon gas to make the forming chamber The oxygen content is lower than 300ppm. According to the set process parameters and scanning strategy of laser selective melting and forming, the medium entropy alloy powder is melted layer by layer to prepare the medium entropy alloy components; 激光选区熔化成形的工艺参数如下:激光功率P为160~360W,扫描速率v为600~1000mm/s,扫描间距h为60~80μm,铺粉层厚t为30~50μm,光斑直径为80μm,体能量密度VED范围为140J/mm3 < VED < 240J/mm3,其中VED=P/vht。The process parameters of laser selective melting and forming are as follows: laser power P is 160-360W, scanning speed v is 600-1000mm/s, scanning distance h is 60-80μm, powder layer thickness t is 30-50μm, and spot diameter is 80μm. The range of volume energy density VED is 140J/mm 3 < VED < 240J/mm 3 , where VED=P/vht. 3.根据权利要求2所述的适用于激光增材制造的析出强化型中熵合金的制备方法,其特征在于,扫描策略为67º旋转扫描、往复扫描、往复交织扫描或45º旋转分区扫描。3. The method for preparing a precipitation-strengthened medium-entropy alloy suitable for laser additive manufacturing according to claim 2, wherein the scanning strategy is 67°rotational scanning, reciprocating scanning, reciprocating interweaving scanning or 45°rotating partition scanning. 4.根据权利要求2所述的适用于激光增材制造的析出强化型中熵合金的制备方法,其特征在于,还包括热处理步骤:将中熵合金构件升温至600ºC~800ºC保温12h ≤ t ≤480h,保温结束后水冷,得到热处理后的中熵合金。4. The method for preparing a precipitation-strengthened medium-entropy alloy suitable for laser additive manufacturing according to claim 2, further comprising a heat treatment step: raising the temperature of the medium-entropy alloy component to 600ºC-800ºC for 12h ≤ t ≤ 480h, water cooling after heat preservation, to obtain a heat-treated medium entropy alloy. 5.权利要求1所述的适用于激光增材制造的析出强化型中熵合金的制备方法,其特征在于,采用激光立体成形技术进行制备;包括:5. The preparation method of the precipitation-strengthened medium-entropy alloy suitable for laser additive manufacturing according to claim 1, characterized in that, it is prepared by laser three-dimensional forming technology; comprising: 步骤1,中熵合金粉末制备及预处理Step 1, preparation and pretreatment of medium entropy alloy powder 按照权利要求1所述摩尔百分比,取各元素对应的金属原料,采用真空气雾化法制备中熵合金预合金球形粉末,过筛,烘干,得到中熵合金粉末;According to the mole percentage described in claim 1, the metal raw materials corresponding to each element are taken, and the pre-alloyed spherical powder of the medium-entropy alloy is prepared by vacuum atomization, sieved, and dried to obtain the medium-entropy alloy powder; 步骤2激光立体成形NiaCobCrcAldMe析出强化型中熵合金Step 2 Laser Stereo Forming Ni a Co b Cr c Al d M e Precipitation Strengthened Medium Entropy Alloy 根据待制备的中熵合金构件的几何形状建立三维实体模型并转换为STL格式传送到激光立体成形设备,设置打印工艺参数及激光扫描路径,将中熵合金粉末送至激光立体成形设备中高能激光束所形成的熔池中,通过在基材上逐点、逐线、逐层沉积原材料的方式,打印得到中熵合金构件;Establish a three-dimensional solid model according to the geometric shape of the medium-entropy alloy component to be prepared, convert it into STL format and send it to the laser three-dimensional forming equipment, set the printing process parameters and laser scanning path, and send the medium-entropy alloy powder to the high-energy laser in the laser three-dimensional forming equipment In the molten pool formed by the beam, the medium-entropy alloy components are printed by depositing raw materials point by point, line by line, and layer by layer on the substrate; 打印工艺参数如下:激光功率为2kW~3.5kW,扫描速率为300~800mm/min,送粉速度为5~8g/min,Z轴抬升量为0.4~1.0mm,搭接率为50%,光斑直径为3mm,扫描路径为往复交织扫描路径。The printing process parameters are as follows: laser power is 2kW~3.5kW, scanning speed is 300~800mm/min, powder feeding speed is 5~8g/min, Z-axis lift is 0.4~1.0mm, overlapping rate is 50%, spot The diameter is 3mm, and the scanning path is a reciprocating interweaving scanning path. 6.根据权利要求5所述的适用于激光增材制造的析出强化型中熵合金的制备方法,其特征在于,还包括热处理步骤:将中熵合金构件升温至600ºC~800ºC保温3h ≤ t ≤480h,保温结束后水冷,得到热处理后的中熵合金。6. The method for preparing a precipitation-strengthened medium-entropy alloy suitable for laser additive manufacturing according to claim 5, further comprising a heat treatment step: raising the temperature of the medium-entropy alloy component to 600ºC-800ºC for 3h ≤ t ≤ 480h, water cooling after heat preservation, to obtain a heat-treated medium entropy alloy.
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