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CN113477942B - SLM-based preparation method of high-strength high-plasticity Inconel718 alloy - Google Patents

SLM-based preparation method of high-strength high-plasticity Inconel718 alloy Download PDF

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CN113477942B
CN113477942B CN202110745448.6A CN202110745448A CN113477942B CN 113477942 B CN113477942 B CN 113477942B CN 202110745448 A CN202110745448 A CN 202110745448A CN 113477942 B CN113477942 B CN 113477942B
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徐轶
何思逸
郭双全
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Southwest Jiaotong University
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    • BPERFORMING OPERATIONS; TRANSPORTING
    • B22CASTING; POWDER METALLURGY
    • B22FWORKING METALLIC POWDER; MANUFACTURE OF ARTICLES FROM METALLIC POWDER; MAKING METALLIC POWDER; APPARATUS OR DEVICES SPECIALLY ADAPTED FOR METALLIC POWDER
    • B22F10/00Additive manufacturing of workpieces or articles from metallic powder
    • B22F10/20Direct sintering or melting
    • B22F10/28Powder bed fusion, e.g. selective laser melting [SLM] or electron beam melting [EBM]
    • BPERFORMING OPERATIONS; TRANSPORTING
    • B22CASTING; POWDER METALLURGY
    • B22FWORKING METALLIC POWDER; MANUFACTURE OF ARTICLES FROM METALLIC POWDER; MAKING METALLIC POWDER; APPARATUS OR DEVICES SPECIALLY ADAPTED FOR METALLIC POWDER
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    • B33ADDITIVE MANUFACTURING TECHNOLOGY
    • B33YADDITIVE MANUFACTURING, i.e. MANUFACTURING OF THREE-DIMENSIONAL [3-D] OBJECTS BY ADDITIVE DEPOSITION, ADDITIVE AGGLOMERATION OR ADDITIVE LAYERING, e.g. BY 3-D PRINTING, STEREOLITHOGRAPHY OR SELECTIVE LASER SINTERING
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    • C22F1/10Changing the physical structure of non-ferrous metals or alloys by heat treatment or by hot or cold working of nickel or cobalt or alloys based thereon
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Abstract

A preparation method of an SLM-based high-strength high-plasticity Inconel718 alloy comprises the following steps: s1, selective laser melting and forming: printing an Inconel718 alloy blank by a selective laser melting method, and sequentially carrying out step S2 isostatic pressing heat treatment, step S3 stress relief annealing treatment, step S4 solution treatment and step S5 double-stage aging treatment on the Inconel718 alloy blank; the hot isostatic pressing heat treatment temperature is 1165-1170 ℃, the pressure is 125-135 Mpa, and the time is 210-270 min; the stress relief annealing temperature is 790-810 ℃, and the time is 20-40 min; the temperature of the solution treatment is 940-960 ℃, and the time is 20-40 min; the temperature of the first-stage aging treatment of the two-stage aging treatment is 750-770 ℃, the time is 470-490 min, the temperature of the second-stage aging treatment is 640-660 ℃, and the time is 470-490 min. The Inconel718 alloy prepared by the method has the advantages of strength, plasticity and hardness, excellent comprehensive mechanical properties and capability of expanding the application of the Inconel718 alloy to the field of more precise and complex structures.

Description

基于SLM的高强高塑性Inconel718合金的制备方法Preparation method of high strength and high plasticity Inconel718 alloy based on SLM

技术领域technical field

本发明涉及一种基于SLM的高强高塑性Inconel718合金的制备方法,属于合金增材制造技术领域。The invention relates to a preparation method of a high-strength and high-plastic Inconel718 alloy based on SLM, and belongs to the technical field of alloy additive manufacturing.

背景技术Background technique

高温合金是一种可以在600℃以上温度及一定应力条件下长时间工作的高性能材料。Inconel718合金是一种沉淀强化型镍基高温合金,由于其在650℃下具有较高的强度、优异的抗疲劳与蠕变性能以及良好的抗氧化与抗腐蚀能力"被广泛地应用在航空航天、核电及能源领域。Superalloy is a high-performance material that can work for a long time at temperatures above 600°C and under certain stress conditions. Inconel718 alloy is a precipitation-strengthened nickel-based superalloy, which is widely used in aerospace due to its high strength at 650 °C, excellent fatigue and creep resistance, and good oxidation and corrosion resistance. , nuclear power and energy fields.

Inconel718合金的力学性能主要取决于其析出相,包括:γ"(Ni3Nb)相、γ'(Ni3(Al,Ti,Nb))、δ(Ni3Nb)、Laves相等。γ"(Ni3Nb)相为主要强化相,γ'(Ni3(Al,Ti,Nb))相为辅助强化相。适量的δ(Ni3Nb)相具有钉扎晶界、阻碍晶界迁移的作用,能够改善合金冲击韧性和蠕变性能。The mechanical properties of Inconel718 alloy mainly depend on its precipitation phases, including: γ"(Ni 3 Nb) phase, γ'(Ni 3 (Al,Ti,Nb)), δ(Ni 3 Nb), Laves equal. γ"( The Ni 3 Nb) phase is the main strengthening phase, and the γ'(Ni 3 (Al,Ti,Nb)) phase is the auxiliary strengthening phase. An appropriate amount of δ(Ni 3 Nb) phase can pin the grain boundaries and hinder the migration of grain boundaries, and can improve the impact toughness and creep properties of the alloy.

传统Inconl718合金零件的制备主要包括铸造与锻造两种方式。经过多年的发展与改进,铸锻件性能已经得到了较大的提升,但依然避免不了两种方式先天的缺陷。铸件中仍然存在元素偏析严重、晶粒粗大、缩孔疏松等问题;而锻件的性能虽高于铸态,但由于工艺限制,难以成形形状复杂的零部件,还存在黑斑、白点等缺陷。而且,上述两种加工方式属于减材制造,成本高、制造周期长,且很难用于制造结构复杂的零部件。The preparation of traditional Inconl718 alloy parts mainly includes casting and forging. After years of development and improvement, the performance of castings and forgings has been greatly improved, but the inherent defects of the two methods are still unavoidable. There are still serious segregation of elements, coarse grains, and porosity in castings. Although the performance of forgings is higher than that of as-cast, it is difficult to form parts with complex shapes due to process limitations, and there are defects such as black spots and white spots. . Moreover, the above two processing methods belong to subtractive manufacturing, which has high cost and long manufacturing cycle, and is difficult to manufacture components with complex structures.

增材制造(Additive Manufacturing,AM),是一个从三维模型数据出发,将材料逐层堆积制造物体的过程。这种无需原胚和模具的制造方法可以给行业带来新的设计灵活性,减少能源使用和缩短上市时间。激光选区熔化SLM(Selective Laser Melting)成形方法就是一种常用的增材制造方法。采用SLM成形方法制备Inconel718合金不仅解决了复杂零件成形问题,而且具有很高的成形质量。但金属SLM成形具有快速凝固特点,极高的冷却速率使得成形后的Inconel718合金零部件普遍存在局部热应力大,Nb元素偏析造成了脆性Laves相大量析出,γ"、γ'、δ相的析出受抑制、熔道的边界重熔区易产生显微裂纹等缺陷,一般配合后续热处理以改善上述缺陷,但效果都不理想。现有技术还没有一种制备方法可制备出同时兼顾强度、塑性、硬度等力学性能的Inconel718合金,限制了其在很多领域的应用。Additive Manufacturing (AM) is a process of building objects layer by layer from 3D model data. This blank and mold-free manufacturing method could bring new design flexibility to the industry, reducing energy usage and time-to-market. Laser selective melting SLM (Selective Laser Melting) forming method is a commonly used additive manufacturing method. The preparation of Inconel718 alloy by the SLM forming method not only solves the forming problem of complex parts, but also has high forming quality. However, the metal SLM forming has the characteristics of rapid solidification. The extremely high cooling rate makes the formed Inconel718 alloy parts generally have large local thermal stress. The segregation of Nb element causes a large number of brittle Laves phase precipitation, and the precipitation of γ", γ' and δ phases. Defects such as microcracks are easily produced in the boundary remelting zone of the suppressed and molten track, and the above-mentioned defects are generally improved with the follow-up heat treatment, but the effect is not satisfactory. The prior art also does not have a preparation method that can prepare both strength and plasticity at the same time. , hardness and other mechanical properties of Inconel718 alloy, which limits its application in many fields.

发明内容SUMMARY OF THE INVENTION

本发明的发明目的是提供一种基于SLM的高强高塑性Inconel718合金的制备方法,该方法制备的Inconel718合金兼具强度、塑性和硬度,具有优异的综合力学性能,且可使Inconel718合金的应用拓展到更为精密、复杂的结构领域。The purpose of the present invention is to provide a preparation method of high strength and high plasticity Inconel718 alloy based on SLM, the Inconel718 alloy prepared by the method has both strength, plasticity and hardness, has excellent comprehensive mechanical properties, and can expand the application of Inconel718 alloy to more sophisticated and complex structures.

本发明实现其发明目的所采用的技术方案是:一种基于SLM的高强高塑性Inconel718合金的制备方法,包括以下步骤:The technical scheme adopted by the present invention to achieve the purpose of the invention is: a preparation method of a high-strength and high-plastic Inconel718 alloy based on SLM, comprising the following steps:

S1、激光选区熔化成型:通过激光选区熔化的方法打印Inconel718合金坯件;S1. Laser selective melting molding: Inconel718 alloy blanks are printed by laser selective melting;

S2、等静压热处理:将激光选区熔化成型的Inconel718合金坯件置于等静压热处理设备中,抽真空,在真空条件下进行等静压热处理,热等静压热处理温度为1165℃~1170℃,压强为125~135Mpa,时间为210min~270min,等静压热处理后向等静压热处理设备中通入氩气快速冷却至室温;S2. Isostatic pressing heat treatment: place the Inconel718 alloy blank formed by laser selective melting in the isostatic pressing heat treatment equipment, vacuumize, and perform isostatic pressing heat treatment under vacuum conditions. The hot isostatic pressing heat treatment temperature is 1165 ℃ ~ 1170 ℃, the pressure is 125~135Mpa, the time is 210min~270min, after isostatic pressing heat treatment, argon gas is introduced into the isostatic pressing heat treatment equipment to rapidly cool to room temperature;

S3、去应力退火处理:将经过等静压热处理后的Inconel718合金坯件置于热处理炉的高温加热内膛中,在氩气气氛保护下进行去应力退火,去应力退火温度为790℃~810℃,时间为20min~40min;S3. Stress relief annealing treatment: place the Inconel718 alloy blank after isostatic pressing heat treatment in the high temperature heating inner chamber of the heat treatment furnace, and perform stress relief annealing under the protection of argon atmosphere. The stress relief annealing temperature is 790℃~810℃ ℃, the time is 20min~40min;

S4、固溶处理:去应力退火处理操作完成后,保持所述高温加热内膛的在氩气气氛保护,升高加热内膛的温度对去应力退火处理后的Inconel718合金坯件进行固溶处理,固溶处理温度为940℃~960℃,时间为20min~40min,固溶处理后向热处理炉中充氩气快速冷却至500℃以下;S4. Solution treatment: After the stress relief annealing operation is completed, keep the high temperature heating inner chamber protected in an argon atmosphere, and increase the temperature of the heating inner chamber to perform solution treatment on the Inconel718 alloy blank after stress relief annealing treatment , the solution treatment temperature is 940 ℃ ~ 960 ℃, the time is 20min ~ 40min, after the solution treatment, the heat treatment furnace is filled with argon and rapidly cooled to below 500 ℃;

S5、双级时效处理:将固溶处理后的Inconel718合金坯件置于热处理炉的高温加热内膛中,在氩气气氛保护下进行双级时效处理,一级时效处理的温度为750℃~770℃,时间为470min~490min,二级时效处理的温度为640℃~660℃,时间为470min~490min,时效处理后向热处理炉中充氩气快速冷却至200℃以下,出炉,即完成高强高塑性Inconel718合金的制备。S5. Double-stage aging treatment: place the solution-treated Inconel718 alloy blank in the high-temperature heating inner chamber of the heat treatment furnace, and carry out double-stage aging treatment under the protection of argon atmosphere. The temperature of the first-stage aging treatment is 750℃~ 770℃, the time is 470min~490min, the temperature of the secondary aging treatment is 640℃~660℃, and the time is 470min~490min, after the aging treatment, the heat treatment furnace is filled with argon and rapidly cooled to below 200℃, and the furnace is released, that is, the high strength is completed. Preparation of high plasticity Inconel718 alloy.

与现有技术相比,本发明的有益效果是:Compared with the prior art, the beneficial effects of the present invention are:

一、本发明采用激光选区熔化打印Inconel718合金坯件,材料利用率高,节约材料成本,生产过程更灵活,成形质量高,且解决了复杂零件成形问题。1. The present invention adopts laser selective melting and printing of Inconel718 alloy blanks, which has high material utilization rate, material cost saving, more flexible production process, high forming quality, and solves the forming problem of complex parts.

二、本发明通过对激光选区熔化成型的Inconel718合金坯件进行温度1165℃~1170℃、压强125~135Mpa的等静压热处理210min~270min,可消除试样内部显微孔隙,应变诱导边界迁移,溶解脆性Laves相,进而减少元素偏析、均匀组织、促进晶粒再结晶。2. In the present invention, by performing isostatic pressure heat treatment at a temperature of 1165 ℃ to 1170 ℃ and a pressure of 125 to 135 Mpa for 210 to 270 minutes on the Inconel718 alloy blank formed by laser selective melting, the microscopic pores inside the sample can be eliminated, and the strain-induced boundary migration can be eliminated. Dissolve the brittle Laves phase, thereby reducing element segregation, uniform structure, and promoting grain recrystallization.

三、本发明通过对经过等静压热处理后的Inconel718合金坯件进行温度为790℃~810℃,时间为20min~40min的去应力退火处理,可以使得具有特殊位向界面的分解和快速迁移,促使孪晶界形核和生长,最终形成“团簇”退火孪晶界,且优先在晶界以及孪晶界析出δ相以钉扎强化晶界。3. In the present invention, the Inconel718 alloy blank after isostatic pressing heat treatment is subjected to stress relief annealing at a temperature of 790°C to 810°C and a time of 20min to 40min, so that the decomposition and rapid migration of the interface with special orientation can be achieved. It promotes the nucleation and growth of the twin boundary, and finally forms a "cluster" annealing twin boundary, and preferentially precipitates δ phase at the grain boundary and the twin boundary to pin and strengthen the grain boundary.

四、本发明在去应力退火处理后,采用940℃~960℃的温度固溶处理20min~40min,可使得基体内碳化物、γ″相、γ'相等溶解以得到均匀的过饱和固溶体,便于时效时重新析出颗粒细小、分布均匀的碳化物、γ″相和γ'等强化相。固溶处理后通过充入氮气快速冷却可得到过饱和固溶体。4. In the present invention, after the stress relief annealing treatment, the temperature of 940℃~960℃ is used for solution treatment for 20min~40min, which can make the carbide, γ″ phase and γ′ in the matrix dissolve equally to obtain a uniform supersaturated solid solution, which is convenient for During aging, fine-grained and uniformly distributed carbides, γ″ phase and γ' phase and other strengthening phases are re-precipitated. After solution treatment, supersaturated solid solution can be obtained by filling with nitrogen and rapidly cooling.

五、本发明对固溶处理后的Inconel718合金坯件进行双级时效处理,选择较高的时效处理温度,通过控制一级时效处理和二级时效处理的温度和时间,使得晶内基体中析出强化相γ"相及γ'相,高的时效温度结合快速冷却的操作,可保持合金晶粒形貌细小均匀,提升材料屈服强度与抗拉强度,且快速冷却操作可以提高过冷度,有利于更高效析出强化相。5. The present invention performs double-stage aging treatment on the Inconel718 alloy blank after solution treatment, selects a higher aging treatment temperature, and controls the temperature and time of the first-stage aging treatment and the second-stage aging treatment, so that the precipitation in the intragranular matrix is made. The strengthening phase γ" phase and γ' phase, high aging temperature combined with rapid cooling operation, can keep the alloy grain morphology fine and uniform, improve the yield strength and tensile strength of the material, and the rapid cooling operation can improve the degree of supercooling. Conducive to more efficient precipitation of strengthening phase.

总之,本发明首先通过激光选取熔化成型了组织均匀、晶粒细小、致密度高的Inconel718合金坯件,再结合高温等静压热处理、去应力退火处理、固溶处理、双级时效处理,消除了激光选区熔化成型Inconel718合金坯件中存在的脆性Laves相和合金内部显微孔隙,有效促进强化相的析出,生成孪晶界以及在晶界生成δ相,使得制备的合金在不牺牲强度的基础上,塑性大幅提升。本发明与热处理前的合金坯件相比,室温抗拉强度提高了37.06%,室温屈服强度提高了70.14%,室温硬度提高了61.18%,断后伸长率高于锻件标准(12.00%),达到23.10%。即本发明制备方法在显著提高Inconel718合金室温强度的同时较大程度保留了其延展性,获得了具有优异综合力学性能的Inconel718合金,对拓宽Inconel718合金的应用范围具有重大意义。In a word, the present invention firstly selects and melts an Inconel718 alloy blank with uniform structure, fine grain size and high density through laser selection, and then combines high temperature isostatic pressing heat treatment, stress relief annealing treatment, solid solution treatment, and double-stage aging treatment to eliminate the The brittle Laves phase and the internal micro-pores in the Inconel718 alloy blanks formed by laser selective melting are studied, which can effectively promote the precipitation of the strengthening phase, generate twin grain boundaries and generate δ phase at the grain boundaries, so that the prepared alloy can be prepared without sacrificing strength. On the basis, the plasticity is greatly improved. Compared with the alloy blank before heat treatment, the invention has the advantages that the tensile strength at room temperature is increased by 37.06%, the yield strength at room temperature is increased by 70.14%, the hardness at room temperature is increased by 61.18%, and the elongation after fracture is higher than the forging standard (12.00%), reaching 23.10%. That is, the preparation method of the present invention significantly improves the room temperature strength of the Inconel718 alloy while retaining its ductility to a large extent, and obtains the Inconel718 alloy with excellent comprehensive mechanical properties, which is of great significance for widening the application range of the Inconel718 alloy.

进一步,本发明所述步骤S1激光选区熔化成型打印Inconel718合金坯件的打印参数是:打印功率为190W~210W、层高为29μm~31μm、扫描速度为890mm/s~910mm/s、扫描间距为0.98mm~1.2mm。Further, in the step S1 of the present invention, the printing parameters of the laser selective melting molding and printing of the Inconel718 alloy blank are: the printing power is 190W~210W, the layer height is 29μm~31μm, the scanning speed is 890mm/s~910mm/s, and the scanning distance is 0.98mm~1.2mm.

实验验证,上述SLM工艺参数可成型出组织均匀、晶粒细小、致密度高、形状复杂的Inconel718合金坯件。Experiments have verified that the above SLM process parameters can form Inconel718 alloy blanks with uniform structure, fine grains, high density and complex shapes.

进一步,本发明所述步骤S1激光选区熔化成型所用的Inconel718合金粉末粒径为45~60μm。Further, the particle size of the Inconel718 alloy powder used in the laser selective melting and forming in step S1 of the present invention is 45-60 μm.

试验验证,45~60μm粉末粒径在流动性、抑制飞溅及熔化均匀性上做到了较好的均衡,采取粉末粒径为45~60μm的8合金粉末进行激光选区熔化成型得到的Inconel718合金坯件成型质量好,结合后续处理可得到力学性能优异的Inconel718合金。Experiments have verified that the particle size of 45-60μm powder has a good balance in fluidity, splash inhibition and melting uniformity. The Inconel718 alloy blank is obtained by using 8 alloy powder with a powder particle size of 45-60μm for laser selective melting and molding The forming quality is good, and the Inconel718 alloy with excellent mechanical properties can be obtained in combination with the subsequent treatment.

进一步,本发明所述步骤S2等静压热处理在不高于6.67×10-2Pa的真空条件下进行。Further, the isostatic pressing heat treatment in step S2 of the present invention is performed under vacuum conditions not higher than 6.67×10 −2 Pa.

进一步,本发明所述步骤S2热等静压热处理的时间为235min~245min。Further, the time of the hot isostatic pressing heat treatment in step S2 of the present invention is 235min-245min.

试验验证,235min~245min的热等静压热处理,可保证在充分溶解Laves相的同时控制晶粒尺寸过大。Experiments have verified that the hot isostatic pressing heat treatment for 235min-245min can ensure that the Laves phase can be fully dissolved and the grain size can be controlled to be too large.

进一步,本发明所述步骤S3去应力退火处理的温度为795℃~805℃,时间为25min~35min。Further, the temperature of the stress relief annealing treatment in step S3 of the present invention is 795° C.˜805° C., and the time is 25 min˜35 min.

试验验证,上述去应力退火处理的温度及时间有利于在更多的产生孪晶界的同时,在晶界处析出δ相以钉扎强化晶界。Experiments have verified that the temperature and time of the stress relief annealing treatment are beneficial to generate more twin boundaries and at the same time precipitate δ phase at the grain boundaries to pin and strengthen the grain boundaries.

进一步,本发明所述步骤S4固溶处理的温度为945℃~955℃,时间为25min~35min。Further, the temperature of the solution treatment in step S4 of the present invention is 945°C to 955°C, and the time is 25min to 35min.

试验验证,上述固溶处理的温度及时间可以保证在充分形成过饱和固溶体的同时,避免晶界处δ相的溶解以及晶粒的再次长大。Experiments have verified that the temperature and time of the above-mentioned solution treatment can ensure that the supersaturated solid solution is fully formed, and at the same time, the dissolution of the δ phase at the grain boundary and the regrowth of the grains can be avoided.

进一步,本发明所述步骤S4中,去应力退火处理操作完成后,保持所述高温加热内膛的在氩气气氛保护,以8℃/min~10℃/min的升温速率升高加热内膛的温度对去应力退火处理后的Inconel718合金坯件进行固溶处理。Further, in the step S4 of the present invention, after the stress relief annealing operation is completed, the high temperature heating inner chamber is kept protected in an argon atmosphere, and the heating inner chamber is raised at a temperature rise rate of 8°C/min to 10°C/min. The temperature of the Inconel718 alloy blank after stress relief annealing treatment is solution treatment.

进一步,本发明所述步骤S5双级时效处理中,一级时效的温度为755℃~765℃,时间为475min~485min,二级时效处理的温度为645℃~655℃,时间为475min~485min。Further, in the double-stage aging treatment in step S5 of the present invention, the temperature of the first-stage aging treatment is 755°C~765°C, and the time is 475min~485min, and the temperature of the second-stage aging treatment is 645°C~655°C, and the time is 475min~485min .

采用上述时效处理温度及时间,有利于控制γ″相、γ'相的形貌,保持形貌细小均匀。The use of the above-mentioned aging treatment temperature and time is beneficial to control the morphology of the γ" phase and the γ' phase, and keep the morphology fine and uniform.

进一步,本发明所述步骤S5双级时效处理中,一级时效处理后,控制加热内膛的温度以40℃/h~60℃/h的降温速率炉冷至二级时效处理温度。Further, in the double-stage aging treatment in step S5 of the present invention, after the first-stage aging treatment, the temperature of the heating inner chamber is controlled to be furnace-cooled to the second-stage aging treatment temperature at a cooling rate of 40°C/h to 60°C/h.

采用上述降温速率,既可避免产生应力集中和微裂纹的同时,有有利于控制第二级时效的效果,同时保证了热处理生产效率。The above cooling rate can not only avoid stress concentration and micro-cracks, but also help to control the effect of the second-stage aging, and at the same time ensure the production efficiency of heat treatment.

附图说明Description of drawings

图1为本发明实施例一步骤S1制备的Inconel718合金坯件的1000倍光镜图。FIG. 1 is a 1000 times optical microscope view of the Inconel718 alloy blank prepared in step S1 in the first embodiment of the present invention.

图2为本发明实施例一制备的高强高塑性Inconel718合金的100倍光镜图。FIG. 2 is a 100 times optical microscope view of the high-strength and high-plastic Inconel718 alloy prepared in Example 1 of the present invention.

图3为本发明实施例一制备的高强高塑性Inconel718合金背散射电子衍射孪晶界图。FIG. 3 is a backscattered electron diffraction twin boundary diagram of the high-strength and high-plastic Inconel718 alloy prepared in Example 1 of the present invention.

图4为本发明实施例二制备的高强高塑性Inconel718合金的100倍光镜图。FIG. 4 is a 100 times optical microscope view of the high-strength and high-plastic Inconel718 alloy prepared in Example 2 of the present invention.

图5为本发明实施例二制备的高强高塑性Inconel718合金背散射电子衍射应力应变图。FIG. 5 is a stress-strain diagram of backscattered electron diffraction of the high-strength and high-plastic Inconel718 alloy prepared in Example 2 of the present invention.

图6为本发明实施例一制备的高强高塑性Inconel718合金的扫描电镜图。6 is a scanning electron microscope image of the high-strength and high-plastic Inconel718 alloy prepared in Example 1 of the present invention.

图7为本发明实施例二制备的高强高塑性Inconel718合金的扫描电镜图。7 is a scanning electron microscope image of the high-strength and high-plastic Inconel718 alloy prepared in Example 2 of the present invention.

图8为本发明实施例一和实施例二制备的高强高塑性Inconel718合金的拉伸曲线图。FIG. 8 is a tensile curve diagram of the high-strength and high-plastic Inconel718 alloy prepared in the first and second embodiments of the present invention.

具体实施方式Detailed ways

实施例一Example 1

一种基于SLM的高强高塑性Inconel718合金的制备方法,包括以下步骤:A preparation method of a high-strength and high-plastic Inconel718 alloy based on SLM, comprising the following steps:

S1、激光选区熔化成型:通过激光选区熔化的方法打印Inconel718合金坯件,激光选区熔化成型所用的Inconel718合金粉末粒径为45~60μm,打印参数是:打印功率为200W、层高为30μm、扫描速度为900mm/s、扫描间距为1mm;取打印成型的Inconel718合金坯件试样,观察其微观结构,见图1;S1. Laser selective melting molding: Inconel718 alloy blanks are printed by laser selective melting. The particle size of Inconel718 alloy powder used in laser selective melting molding is 45-60 μm. The printing parameters are: printing power of 200W, layer height of 30 μm, scanning The speed is 900mm/s and the scanning interval is 1mm; take the printed Inconel718 alloy blank sample and observe its microstructure, as shown in Figure 1;

S2、等静压热处理:将激光选区熔化成型的Inconel718合金坯件置于等静压热处理设备中,抽真空,在不高于6.67×10-2Pa的真空条件下进行等静压热处理,热等静压热处理温度为1165℃,压强为130Mpa,时间为240min,等静压热处理后向等静压热处理设备中通入氩气快速冷却至室温;S2. Isostatic pressing heat treatment: place the Inconel718 alloy blank formed by laser selective melting in the isostatic pressing heat treatment equipment, vacuumize, and perform isostatic pressing heat treatment under the vacuum condition of not higher than 6.67×10 -2 Pa. The temperature of isostatic pressing heat treatment is 1165℃, the pressure is 130Mpa, and the time is 240min. After the isostatic pressing heat treatment, argon gas is introduced into the isostatic pressing heat treatment equipment to rapidly cool to room temperature;

S3、去应力退火处理:将经过等静压热处理后的Inconel718合金坯件置于热处理炉的高温加热内膛中,在氩气气氛保护下进行去应力退火,去应力退火温度为800℃,时间为30min;S3. Stress relief annealing treatment: The Inconel718 alloy blank after isostatic pressing heat treatment is placed in the high temperature heating inner chamber of the heat treatment furnace, and stress relief annealing is carried out under the protection of argon atmosphere. The stress relief annealing temperature is 800 ℃, and the time is 30min;

S4、固溶处理:去应力退火处理操作完成后,保持所述高温加热内膛的在氩气气氛保护,以8℃/min的升温速率升高加热内膛的温度对去应力退火处理后的Inconel718合金坯件进行固溶处理,固溶处理温度为950℃,时间为30min,固溶处理后向热处理炉中充氩气快速冷却至500℃以下;S4, solution treatment: after the stress relief annealing treatment operation is completed, keep the high temperature heating inner chamber protected in an argon atmosphere, and increase the temperature of the heating inner chamber at a heating rate of 8°C/min. The Inconel718 alloy blanks are solution-treated, the solution-treatment temperature is 950°C, and the time is 30min. After the solution-treatment, the heat treatment furnace is filled with argon and rapidly cooled to below 500°C;

S5、双级时效处理:将固溶处理后的Inconel718合金坯件置于热处理炉的高温加热内膛中,在氩气气氛保护下进行双级时效处理,一级时效处理的温度为760℃,时间为480min,一级时效处理后,控制加热内膛的温度以50℃/h的降温速率炉冷至二级时效处理温度650℃,二级时效处理时间为480min,时效处理后向热处理炉中充氩气快速冷却至200℃以下,出炉,即完成高强高塑性Inconel718合金的制备。S5. Double-stage aging treatment: The Inconel718 alloy blank after solution treatment is placed in the high-temperature heating inner chamber of the heat treatment furnace, and the double-stage aging treatment is carried out under the protection of argon atmosphere. The temperature of the first-stage aging treatment is 760 ℃, The time is 480min. After the first-level aging treatment, the temperature of the heating inner chamber is controlled to cool down to the second-level aging treatment temperature of 650℃ at a cooling rate of 50℃/h. The second-level aging treatment time is 480min. Filling with argon gas is quickly cooled to below 200 ° C, and the furnace is released, that is, the preparation of high-strength and high-plastic Inconel718 alloy is completed.

实施例二Embodiment 2

一种基于SLM的高强高塑性Inconel718合金的制备方法,包括以下步骤:A preparation method of a high-strength and high-plastic Inconel718 alloy based on SLM, comprising the following steps:

S1、激光选区熔化成型:通过激光选区熔化的方法打印Inconel718合金坯件,激光选区熔化成型所用的Inconel718合金粉末粒径为45~60μm,打印参数是:打印功率为200W、层高为30μm、扫描速度为900mm/s、扫描间距为1mm;S1. Laser selective melting molding: Inconel718 alloy blanks are printed by laser selective melting. The particle size of Inconel718 alloy powder used in laser selective melting molding is 45-60 μm. The printing parameters are: printing power of 200W, layer height of 30 μm, scanning The speed is 900mm/s and the scanning distance is 1mm;

S2、等静压热处理:将激光选区熔化成型的Inconel718合金坯件置于等静压热处理设备中,抽真空,在不高于6.67×10-2Pa的真空条件下进行等静压热处理,热等静压热处理温度为1170℃,压强为130Mpa,时间为220min,等静压热处理后向等静压热处理设备中通入氩气快速冷却至室温;S2. Isostatic pressing heat treatment: place the Inconel718 alloy blank formed by laser selective melting in the isostatic pressing heat treatment equipment, vacuumize, and perform isostatic pressing heat treatment under the vacuum condition of not higher than 6.67×10 -2 Pa. The temperature of isostatic pressing heat treatment is 1170℃, the pressure is 130Mpa, and the time is 220min. After isostatic pressing heat treatment, argon gas is introduced into the isostatic pressing heat treatment equipment to rapidly cool to room temperature;

S3、去应力退火处理:将经过等静压热处理后的Inconel718合金坯件置于热处理炉的高温加热内膛中,在氩气气氛保护下进行去应力退火,去应力退火温度为810℃,时间为30min;S3. Stress relief annealing treatment: Place the Inconel718 alloy blank after isostatic pressing heat treatment in the high temperature heating inner chamber of the heat treatment furnace, and perform stress relief annealing under the protection of argon atmosphere. The stress relief annealing temperature is 810°C, and the time is 30min;

S4、固溶处理:去应力退火处理操作完成后,保持所述高温加热内膛的在氩气气氛保护,以8℃/min的升温速率升高加热内膛的温度对去应力退火处理后的Inconel718合金坯件进行固溶处理,固溶处理温度为950℃,时间为40min,固溶处理后向热处理炉中充氩气快速冷却至500℃以下;S4, solution treatment: after the stress relief annealing treatment operation is completed, keep the high temperature heating inner chamber protected in an argon atmosphere, and increase the temperature of the heating inner chamber at a heating rate of 8°C/min. Inconel718 alloy blanks are solution treated, the solution treatment temperature is 950℃, and the time is 40min. After the solution treatment, the heat treatment furnace is filled with argon and rapidly cooled to below 500℃;

S5、双级时效处理:将固溶处理后的Inconel718合金坯件置于热处理炉的高温加热内膛中,在氩气气氛保护下进行双级时效处理,一级时效处理的温度为760℃,时间为470min,一级时效处理后,控制加热内膛的温度以60℃/h的降温速率炉冷至二级时效处理温度650℃,二级时效处理时间为480min,时效处理后向热处理炉中充氩气快速冷却至200℃以下,出炉,即完成高强高塑性Inconel718合金的制备。S5. Double-stage aging treatment: The Inconel718 alloy blank after solution treatment is placed in the high-temperature heating inner chamber of the heat treatment furnace, and the double-stage aging treatment is carried out under the protection of argon atmosphere. The temperature of the first-stage aging treatment is 760 ℃, The time is 470min. After the primary aging treatment, the temperature of the heating inner chamber is controlled to be cooled to the secondary aging treatment temperature of 650 °C at a cooling rate of 60℃/h. The secondary aging treatment time is 480min. Filling with argon gas is quickly cooled to below 200 ° C, and the furnace is released, that is, the preparation of high-strength and high-plastic Inconel718 alloy is completed.

取实施例一和实施例二制备的高强高塑性Inconel718合金试样进行表征。The high-strength and high-plastic Inconel718 alloy samples prepared in Example 1 and Example 2 were used for characterization.

图1为实施例一步骤S1制备的Inconel718合金坯件的1000倍光镜图,显示Inconel718合金坯件的显微组织图,图中可以看到,合金基体显微组织由细小的胞状晶以及细长的柱状晶组成,还能看到明显的打印熔池边界,此种形态对力学性能有不利影响。Figure 1 is a 1000x optical microscope image of the Inconel718 alloy blank prepared in step S1 of Example 1, showing the microstructure of the Inconel718 alloy blank. As can be seen from the figure, the microstructure of the alloy matrix consists of fine cellular crystals and fine The composition of long columnar crystals can also see the obvious printed melt pool boundary, which has an adverse effect on the mechanical properties.

图2和图4分别为实施例一和实施例二制备的高强高塑性Inconel718合金的100倍光镜图。从图中可以看出,经过步骤S2-S5的热处理,合金晶粒出现明显的再结晶,晶粒尺寸较原始试样增大明显,且在晶粒内部和晶界可观察到大量孪晶的形成。FIG. 2 and FIG. 4 are 100 times optical microscope images of the high-strength and high-plastic Inconel718 alloy prepared in Example 1 and Example 2, respectively. It can be seen from the figure that after the heat treatment in steps S2-S5, the alloy grains are obviously recrystallized, the grain size is significantly larger than that of the original sample, and a large number of twinned crystals can be observed inside the grains and at the grain boundaries. form.

图3为实施例一制备的高强高塑性Inconel718合金背散射电子衍射孪晶界图,从图中可以看出,经过步骤S2-S5的热处理,合金基体显微组织生成大量的孪晶界(黑粗线标出)。Figure 3 is the backscattered electron diffraction twin grain boundary diagram of the high-strength and high-plastic Inconel718 alloy prepared in Example 1. It can be seen from the figure that after the heat treatment in steps S2-S5, a large number of twin grain boundaries (black and black) are formed in the microstructure of the alloy matrix. bold lines).

图5为实施例二制备的高强高塑性Inconel718合金背散射电子衍射应力应变图。从图中可以看出,经过步骤S2-S5的热处理,合金基体显微组织内应力(高亮白点区域)已基本消除。FIG. 5 is a stress-strain diagram of backscattered electron diffraction of the high-strength and high-plastic Inconel718 alloy prepared in Example 2. FIG. It can be seen from the figure that after the heat treatment in steps S2-S5, the internal stress (high-bright white point area) in the microstructure of the alloy matrix has been basically eliminated.

图6和图7分别为实施例一和实施例二制备的高强高塑性Inconel718合金的扫描电镜图。图中可以看出,经过步骤S2-S5的热处理,合金基体显微组织晶粒边界均匀分布着短棒状和细针状δ相,基体上还分布着少量MC相,MC相成分为TiC,NbC的面心立方碳化物相,性质稳定,熔点高,但是数量很少,具有高硬度和高熔点等陶瓷特性,对合金起到一定的第二相强化作用。FIG. 6 and FIG. 7 are scanning electron microscope images of the high-strength and high-plastic Inconel718 alloy prepared in Example 1 and Example 2, respectively. It can be seen from the figure that after the heat treatment in steps S2-S5, the microstructure and grain boundaries of the alloy matrix are uniformly distributed with short rod-shaped and fine needle-shaped δ phases, and a small amount of MC phase is also distributed on the matrix. The MC phase composition is TiC, NbC The face-centered cubic carbide phase has stable properties and high melting point, but the number is very small. It has ceramic properties such as high hardness and high melting point, which plays a certain role in strengthening the second phase of the alloy.

从图中可以看出,经过1160℃、130MPa的热等静压处理,原始样品的激光扫描边界消失,树枝晶及胞状晶亚结构被再结晶晶粒所取代,同时树枝晶间析出的大量脆性Laves相基本溶解,并释放了材料快速成型时积累的内应力(如图5所示),此时晶界在1160℃高温的作用下快速移动,开始再结晶,并生成退火孪晶,高温下受130MPa压力的作用,合金产生微变形,位错与合金中退火孪晶界的相互作用,导致退火孪晶界上出现大量a/6<112>不全位错,致使连续界面(晶界和退火孪晶界)逐渐演变为不连续界面;在随后的790℃~810℃去应力退火过程中,具有特殊位向界面的分解和快速迁移,促使孪晶界形核和生长,最终形成“团簇”退火孪晶界(如图2、图3和图4所示),且优先在晶界以及孪晶界析出δ相(如图6、7所示)以钉扎强化晶界,以提升整体力学性能,并抑制下一步固溶时晶粒的长大。It can be seen from the figure that after the hot isostatic pressing at 1160 °C and 130 MPa, the laser scanning boundary of the original sample disappeared, the dendrites and cellular substructures were replaced by recrystallized grains, and a large amount of brittleness precipitated between the dendrites. The Laves phase basically dissolves and releases the internal stress accumulated during rapid prototyping of the material (as shown in Figure 5). At this time, the grain boundary moves rapidly under the action of a high temperature of 1160 °C, starts to recrystallize, and generates annealing twins. Under the action of 130MPa pressure, the alloy is slightly deformed, and the interaction of dislocations with the annealing twin boundaries in the alloy leads to a large number of a/6<112> incomplete dislocations on the annealing twin boundaries, resulting in continuous interfaces (grain boundaries and annealing twin boundaries). twin boundary) gradually evolved into a discontinuous interface; in the subsequent stress relief annealing process at 790 °C ~ 810 °C, the decomposition and rapid migration of the interface with special orientations promoted the nucleation and growth of the twin boundary, and finally formed "clusters". "annealing twin grain boundaries (as shown in Figure 2, Figure 3 and Figure 4), and preferentially precipitates delta phases (as shown in Figures 6 and 7) at the grain boundaries and twin boundaries to pin and strengthen the grain boundaries to improve the overall mechanical properties, and inhibit the growth of grains during the next solid solution.

采用X射线衍射分析实施例一和实施例二制备的高强高塑性Inconel718合金的析出相,检测到δ相、γ"相及γ'相,采用显微维氏硬度计和电子万能试验机测试其力学性能,检测得到:实施例一制备的高强高塑性Inconel718合金的室温硬度为458HV,室温抗拉强度为1395MPa,室温屈服强度为1138MPa,室温断后伸长率为21.80%;实施例二制备的高强高塑性Inconel718合金的室温硬度为472HV,室温抗拉强度为1433MPa,室温屈服强度为1184MPa,室温断后伸长率为22.90%,实施例一和实施例二制备的高强高塑性Inconel718合金的拉伸曲线图见图8。The precipitation phase of the high-strength and high-plastic Inconel718 alloy prepared in Example 1 and Example 2 was analyzed by X-ray diffraction, and δ phase, γ" phase and γ' phase were detected, and the micro-Vickers hardness tester and electronic universal testing machine were used to test their Mechanical properties, it is found that the room temperature hardness of the high-strength and high-plastic Inconel718 alloy prepared in Example 1 is 458HV, the tensile strength at room temperature is 1395MPa, the yield strength at room temperature is 1138MPa, and the elongation after fracture at room temperature is 21.80%; The room temperature hardness of the high plasticity Inconel718 alloy is 472HV, the room temperature tensile strength is 1433MPa, the room temperature yield strength is 1184MPa, and the room temperature elongation after fracture is 22.90%. Figure 8.

综上所述,按照本发明制备方法制备的Inconel718合金试样,其内部显微孔隙及元素偏析基本消除,孪晶分布均匀,第二相均匀析出,其室温抗拉强度、室温屈服强度、断后伸长率均高于锻件标准。可满足Inconel718合金的结构件高强度、高塑性的要求。To sum up, the Inconel718 alloy sample prepared according to the preparation method of the present invention basically eliminates the internal microporosity and element segregation, the twin crystals are evenly distributed, and the second phase is uniformly precipitated. The elongation is higher than the forging standard. It can meet the requirements of high strength and high plasticity of structural parts of Inconel718 alloy.

实施例三Embodiment 3

一种基于SLM的高强高塑性Inconel718合金的制备方法,包括以下步骤:A preparation method of a high-strength and high-plastic Inconel718 alloy based on SLM, comprising the following steps:

S1、激光选区熔化成型:通过激光选区熔化的方法打印Inconel718合金坯件,激光选区熔化成型所用的Inconel718合金粉末粒径为45~60μm,打印参数是:打印功率为190W、层高为31μm、扫描速度为890mm/s、扫描间距为0.98mm;取打印成型的Inconel718合金坯件试样;S1. Laser selective melting molding: Inconel718 alloy blanks are printed by laser selective melting. The particle size of Inconel718 alloy powder used in laser selective melting molding is 45-60 μm. The printing parameters are: printing power of 190W, layer height of 31 μm, scanning The speed is 890mm/s, and the scanning distance is 0.98mm; take the printed Inconel718 alloy blank sample;

S2、等静压热处理:将激光选区熔化成型的Inconel718合金坯件置于等静压热处理设备中,抽真空,在不高于6.67×10-2Pa的真空条件下进行等静压热处理,热等静压热处理温度为1168℃,压强为125Mpa,时间为270min,等静压热处理后向等静压热处理设备中通入氩气快速冷却至室温;S2. Isostatic pressing heat treatment: place the Inconel718 alloy blank formed by laser selective melting in the isostatic pressing heat treatment equipment, vacuumize, and perform isostatic pressing heat treatment under the vacuum condition of not higher than 6.67×10 -2 Pa. The temperature of isostatic pressing heat treatment is 1168℃, the pressure is 125Mpa, and the time is 270min. After isostatic pressing heat treatment, argon gas is introduced into the isostatic pressing heat treatment equipment to rapidly cool to room temperature;

S3、去应力退火处理:将经过等静压热处理后的Inconel718合金坯件置于热处理炉的高温加热内膛中,在氩气气氛保护下进行去应力退火,去应力退火温度为790℃,时间为40min;S3. Stress relief annealing treatment: Place the Inconel718 alloy blank after isostatic pressing heat treatment in the high temperature heating inner chamber of the heat treatment furnace, and perform stress relief annealing under the protection of argon atmosphere. The stress relief annealing temperature is 790 °C, and the time is 40min;

S4、固溶处理:去应力退火处理操作完成后,保持所述高温加热内膛的在氩气气氛保护,以8℃/min的升温速率升高加热内膛的温度对去应力退火处理后的Inconel718合金坯件进行固溶处理,固溶处理温度为940℃,时间为40min,固溶处理后向热处理炉中充氩气快速冷却至500℃以下;S4, solution treatment: after the stress relief annealing treatment operation is completed, keep the high temperature heating inner chamber protected in an argon atmosphere, and increase the temperature of the heating inner chamber at a heating rate of 8°C/min. The Inconel718 alloy blanks were solution treated at a temperature of 940°C for 40 minutes. After solution treatment, the heat treatment furnace was filled with argon and rapidly cooled to below 500°C;

S5、双级时效处理:将固溶处理后的Inconel718合金坯件置于热处理炉的高温加热内膛中,在氩气气氛保护下进行双级时效处理,一级时效处理的温度为750℃,时间为490min,一级时效处理后,控制加热内膛的温度以50℃/h的降温速率炉冷至二级时效处理温度640℃,二级时效处理时间为490min,时效处理后向热处理炉中充氩气快速冷却至200℃以下,出炉,即完成高强高塑性Inconel718合金的制备。S5. Double-stage aging treatment: The Inconel718 alloy blank after solution treatment is placed in the high-temperature heating inner chamber of the heat treatment furnace, and double-stage aging treatment is carried out under the protection of argon atmosphere. The temperature of the first-stage aging treatment is 750 ℃, The time is 490min. After the first-level aging treatment, the temperature of the heating inner chamber is controlled to cool down to the second-level aging treatment temperature of 640℃ at a cooling rate of 50℃/h. The second-level aging treatment time is 490min. Filling with argon gas is quickly cooled to below 200 ° C, and the furnace is released, that is, the preparation of high-strength and high-plastic Inconel718 alloy is completed.

实施例四Embodiment 4

一种基于SLM的高强高塑性Inconel718合金的制备方法,包括以下步骤:A preparation method of a high-strength and high-plastic Inconel718 alloy based on SLM, comprising the following steps:

S1、激光选区熔化成型:通过激光选区熔化的方法打印Inconel718合金坯件,激光选区熔化成型所用的Inconel718合金粉末粒径为45~60μm,打印参数是:打印功率为210W、层高为29μm、扫描速度为910mm/s、扫描间距为1.2mm;取打印成型的Inconel718合金坯件试样;S1. Laser selective melting and molding: Inconel718 alloy blanks are printed by laser selective melting. The particle size of Inconel718 alloy powder used in laser selective melting and molding is 45-60 μm. The printing parameters are: printing power of 210W, layer height of 29 μm, scanning The speed is 910mm/s, and the scanning distance is 1.2mm; take the printed Inconel718 alloy blank sample;

S2、等静压热处理:将激光选区熔化成型的Inconel718合金坯件置于等静压热处理设备中,抽真空,在不高于6.67×10-2Pa的真空条件下进行等静压热处理,热等静压热处理温度为1168℃,压强为135Mpa,时间为210min,等静压热处理后向等静压热处理设备中通入氩气快速冷却至室温;S2. Isostatic pressing heat treatment: place the Inconel718 alloy blank formed by laser selective melting in the isostatic pressing heat treatment equipment, vacuumize, and perform isostatic pressing heat treatment under the vacuum condition of not higher than 6.67×10 -2 Pa. The temperature of isostatic pressing heat treatment is 1168℃, the pressure is 135Mpa, and the time is 210min. After isostatic pressing heat treatment, argon gas is poured into the isostatic pressing heat treatment equipment to rapidly cool to room temperature;

S3、去应力退火处理:将经过等静压热处理后的Inconel718合金坯件置于热处理炉的高温加热内膛中,在氩气气氛保护下进行去应力退火,去应力退火温度为805℃,时间为25min;S3. Stress relief annealing treatment: The Inconel718 alloy blank after isostatic pressing heat treatment is placed in the high temperature heating inner chamber of the heat treatment furnace, and stress relief annealing is carried out under the protection of argon atmosphere. The stress relief annealing temperature is 805 ℃, and the time is 25min;

S4、固溶处理:去应力退火处理操作完成后,保持所述高温加热内膛的在氩气气氛保护,以8℃/min的升温速率升高加热内膛的温度对去应力退火处理后的Inconel718合金坯件进行固溶处理,固溶处理温度为960℃,时间为20min,固溶处理后向热处理炉中充氩气快速冷却至500℃以下;S4, solution treatment: after the stress relief annealing treatment operation is completed, keep the high temperature heating inner chamber protected in an argon atmosphere, and increase the temperature of the heating inner chamber at a heating rate of 8°C/min. The Inconel718 alloy blanks were solution treated at a temperature of 960°C for 20 minutes. After solution treatment, the heat treatment furnace was filled with argon and rapidly cooled to below 500°C;

S5、双级时效处理:将固溶处理后的Inconel718合金坯件置于热处理炉的高温加热内膛中,在氩气气氛保护下进行双级时效处理,一级时效处理的温度为770℃,时间为470min,一级时效处理后,控制加热内膛的温度以40℃/h的降温速率炉冷至二级时效处理温度660℃,二级时效处理时间为470min,时效处理后向热处理炉中充氩气快速冷却至200℃以下,出炉,即完成高强高塑性Inconel718合金的制备。S5. Double-stage aging treatment: The Inconel718 alloy blank after solution treatment is placed in the high-temperature heating inner chamber of the heat treatment furnace, and the double-stage aging treatment is carried out under the protection of an argon atmosphere. The temperature of the first-stage aging treatment is 770 ℃, The time is 470min. After the first-stage aging treatment, the temperature of the heating inner chamber is controlled to cool down to the second-stage aging treatment temperature of 660°C at a cooling rate of 40℃/h. The second-stage aging treatment time is 470min. Filling with argon gas is quickly cooled to below 200 ° C, and the furnace is released, that is, the preparation of high-strength and high-plastic Inconel718 alloy is completed.

实施例五Embodiment 5

一种基于SLM的高强高塑性Inconel718合金的制备方法,包括以下步骤:A preparation method of a high-strength and high-plastic Inconel718 alloy based on SLM, comprising the following steps:

S1、激光选区熔化成型:通过激光选区熔化的方法打印Inconel718合金坯件,激光选区熔化成型所用的Inconel718合金粉末粒径为45~60μm,打印参数是:打印功率为200W、层高为30μm、扫描速度为900mm/s、扫描间距为1mm;取打印成型的Inconel718合金坯件试样;S1. Laser selective melting molding: Inconel718 alloy blanks are printed by laser selective melting. The particle size of Inconel718 alloy powder used in laser selective melting molding is 45-60 μm. The printing parameters are: printing power of 200W, layer height of 30 μm, scanning The speed is 900mm/s, and the scanning interval is 1mm; take the printed Inconel718 alloy blank sample;

S2、等静压热处理:将激光选区熔化成型的Inconel718合金坯件置于等静压热处理设备中,抽真空,在不高于6.67×10-2Pa的真空条件下进行等静压热处理,热等静压热处理温度为1168℃,压强为130Mpa,时间为235min,等静压热处理后向等静压热处理设备中通入氩气快速冷却至室温;S2. Isostatic pressing heat treatment: place the Inconel718 alloy blank formed by laser selective melting in the isostatic pressing heat treatment equipment, vacuumize, and perform isostatic pressing heat treatment under the vacuum condition of not higher than 6.67×10 -2 Pa. The temperature of isostatic pressing heat treatment is 1168℃, the pressure is 130Mpa, and the time is 235min. After the isostatic pressing heat treatment, argon gas is poured into the isostatic pressing heat treatment equipment to rapidly cool to room temperature;

S3、去应力退火处理:将经过等静压热处理后的Inconel718合金坯件置于热处理炉的高温加热内膛中,在氩气气氛保护下进行去应力退火,去应力退火温度为795℃,时间为35min;S3. Stress relief annealing treatment: The Inconel718 alloy blank after isostatic pressing heat treatment is placed in the high temperature heating inner chamber of the heat treatment furnace, and stress relief annealing is carried out under the protection of argon atmosphere. The stress relief annealing temperature is 795 ℃, and the time is 35min;

S4、固溶处理:去应力退火处理操作完成后,保持所述高温加热内膛的在氩气气氛保护,以8℃/min的升温速率升高加热内膛的温度对去应力退火处理后的Inconel718合金坯件进行固溶处理,固溶处理温度为945℃,时间为35min,固溶处理后向热处理炉中充氩气快速冷却至500℃以下;S4, solution treatment: after the stress relief annealing treatment operation is completed, keep the high temperature heating inner chamber protected in an argon atmosphere, and increase the temperature of the heating inner chamber at a heating rate of 8°C/min. Inconel 718 alloy blanks are solution treated, the solution treatment temperature is 945℃, and the time is 35min. After the solution treatment, the heat treatment furnace is filled with argon and rapidly cooled to below 500℃;

S5、双级时效处理:将固溶处理后的Inconel718合金坯件置于热处理炉的高温加热内膛中,在氩气气氛保护下进行双级时效处理,一级时效处理的温度为755℃,时间为485min,一级时效处理后,控制加热内膛的温度以50℃/h的降温速率炉冷至二级时效处理温度645℃,二级时效处理时间为485min,时效处理后向热处理炉中充氩气快速冷却至200℃以下,出炉,即完成高强高塑性Inconel718合金的制备。S5. Double-stage aging treatment: The Inconel718 alloy blank after solution treatment is placed in the high-temperature heating inner chamber of the heat treatment furnace, and the double-stage aging treatment is carried out under the protection of an argon atmosphere. The temperature of the first-stage aging treatment is 755 ℃, The time is 485min. After the primary aging treatment, the temperature of the heating inner chamber is controlled to cool down to the secondary aging treatment temperature of 645 °C at a cooling rate of 50℃/h. The secondary aging treatment time is 485min. Filling with argon gas is quickly cooled to below 200 ° C, and the furnace is released, that is, the preparation of high-strength and high-plastic Inconel718 alloy is completed.

实施例六Embodiment 6

一种基于SLM的高强高塑性Inconel718合金的制备方法,包括以下步骤:A preparation method of a high-strength and high-plastic Inconel718 alloy based on SLM, comprising the following steps:

S1、激光选区熔化成型:通过激光选区熔化的方法打印Inconel718合金坯件,激光选区熔化成型所用的Inconel718合金粉末粒径为45~60μm,打印参数是:打印功率为200W、层高为30μm、扫描速度为900mm/s、扫描间距为1mm;取打印成型的Inconel718合金坯件试样;S1. Laser selective melting molding: Inconel718 alloy blanks are printed by laser selective melting. The particle size of Inconel718 alloy powder used in laser selective melting molding is 45-60 μm. The printing parameters are: printing power of 200W, layer height of 30 μm, scanning The speed is 900mm/s, and the scanning interval is 1mm; take the printed Inconel718 alloy blank sample;

S2、等静压热处理:将激光选区熔化成型的Inconel718合金坯件置于等静压热处理设备中,抽真空,在不高于6.67×10-2Pa的真空条件下进行等静压热处理,热等静压热处理温度为1168℃,压强为130Mpa,时间为245min,等静压热处理后向等静压热处理设备中通入氩气快速冷却至室温;S2. Isostatic pressing heat treatment: place the Inconel718 alloy blank formed by laser selective melting in the isostatic pressing heat treatment equipment, vacuumize, and perform isostatic pressing heat treatment under the vacuum condition of not higher than 6.67×10 -2 Pa. The temperature of isostatic pressing heat treatment is 1168℃, the pressure is 130Mpa, and the time is 245min. After the isostatic pressing heat treatment, argon gas is introduced into the isostatic pressing heat treatment equipment to rapidly cool to room temperature;

S3、去应力退火处理:将经过等静压热处理后的Inconel718合金坯件置于热处理炉的高温加热内膛中,在氩气气氛保护下进行去应力退火,去应力退火温度为810℃,时间为20min;S3. Stress relief annealing treatment: Place the Inconel718 alloy blank after isostatic pressing heat treatment in the high temperature heating inner chamber of the heat treatment furnace, and perform stress relief annealing under the protection of argon atmosphere. The stress relief annealing temperature is 810°C, and the time is 20min;

S4、固溶处理:去应力退火处理操作完成后,保持所述高温加热内膛的在氩气气氛保护,以8℃/min的升温速率升高加热内膛的温度对去应力退火处理后的Inconel718合金坯件进行固溶处理,固溶处理温度为955℃,时间为25min,固溶处理后向热处理炉中充氩气快速冷却至500℃以下;S4, solution treatment: after the stress relief annealing treatment operation is completed, keep the high temperature heating inner chamber protected in an argon atmosphere, and increase the temperature of the heating inner chamber at a heating rate of 8°C/min. Inconel718 alloy blanks are solution treated, the solution treatment temperature is 955℃, and the time is 25min. After the solution treatment, the heat treatment furnace is filled with argon and rapidly cooled to below 500℃;

S5、双级时效处理:将固溶处理后的Inconel718合金坯件置于热处理炉的高温加热内膛中,在氩气气氛保护下进行双级时效处理,一级时效处理的温度为765℃,时间为475min,一级时效处理后,控制加热内膛的温度以50℃/h的降温速率炉冷至二级时效处理温度655℃,二级时效处理时间为475min,时效处理后向热处理炉中充氩气快速冷却至200℃以下,出炉,即完成高强高塑性Inconel718合金的制备。S5. Double-stage aging treatment: The Inconel718 alloy blank after solution treatment is placed in the high-temperature heating inner chamber of the heat treatment furnace, and the double-stage aging treatment is carried out under the protection of an argon atmosphere. The temperature of the first-stage aging treatment is 765 ℃, The time is 475min. After the first-stage aging treatment, the temperature of the heating inner chamber is controlled to cool down to the second-stage aging treatment temperature of 655°C at a cooling rate of 50℃/h. The second-stage aging treatment time is 475min. Filling with argon gas is quickly cooled to below 200 ° C, and the furnace is released, that is, the preparation of high-strength and high-plastic Inconel718 alloy is completed.

Claims (10)

1. A preparation method of an Inconel718 alloy with high strength and high plasticity based on SLM is characterized by comprising the following steps:
s1, selective laser melting and forming: printing an Inconel718 alloy blank by a selective laser melting method;
s2, isostatic pressing heat treatment: placing the Inconel718 alloy blank subjected to selective laser melting molding in isostatic pressure heat treatment equipment, vacuumizing, performing isostatic pressure heat treatment under a vacuum condition, wherein the temperature of the isostatic pressure heat treatment is 1165-1170 ℃, the pressure is 125-135 MPa, the time is 210-270 min, and introducing argon into the isostatic pressure heat treatment equipment after the isostatic pressure treatment to rapidly cool the Inconel718 alloy blank to room temperature;
s3, stress relief annealing treatment: placing the Inconel718 alloy blank subjected to isostatic pressure heat treatment in a high-temperature heating inner bore of a heat treatment furnace, and performing stress relief annealing under the protection of argon atmosphere, wherein the stress relief annealing temperature is 790-810 ℃, and the time is 20-40 min;
s4, solution treatment: after the stress relief annealing treatment operation is finished, keeping the protection of the argon atmosphere of the high-temperature heating inner chamber, raising the temperature of the heating inner chamber to perform solution treatment on the Inconel718 alloy blank subjected to the stress relief annealing treatment, wherein the solution treatment temperature is 940-960 ℃, the time is 20-40 min, and after the solution treatment, filling argon into a heat treatment furnace to be rapidly cooled to below 500 ℃;
s5, double-stage aging treatment: placing the Inconel718 alloy blank subjected to solution treatment in a high-temperature heating inner bore of a heat treatment furnace, performing two-stage aging treatment under the protection of argon atmosphere, wherein the temperature of the first-stage aging treatment is 750-770 ℃, the time is 470-490 min, the temperature of the second-stage aging treatment is 640-660 ℃, the time is 470-490 min, filling argon into the heat treatment furnace after the aging treatment, rapidly cooling to below 200 ℃, and discharging to finish the preparation of the high-strength high-plasticity Inconel718 alloy.
2. The SLM-based high-strength high-plasticity Inconel718 alloy preparation method according to claim 1, wherein the method comprises the following steps: the printing parameters of the step S1 of melting, forming and printing the Inconel718 alloy blank in the selected laser area are as follows: the printing power is 190W-210W, the layer height is 29 μm-31 μm, the scanning speed is 890 mm/s-910 mm/s, and the scanning distance is 0.98 mm-1.2 mm.
3. The method for preparing the SLM-based high-strength high-plasticity Inconel718 alloy according to claim 1 or 2, wherein the method comprises the following steps: the particle size of Inconel718 alloy powder used for selective laser melting molding in the step S1 is 45-60 mu m.
4. The SLM-based high-strength high-plasticity Inconel718 alloy preparation method according to claim 1, wherein the method comprises the following steps: the step S2 is carried out by isostatic pressing heat treatment at the temperature of not higher than 6.67 multiplied by 10 -2 Pa under vacuum.
5. The SLM-based high-strength high-plasticity Inconel718 alloy preparation method according to claim 1, wherein the method comprises the following steps: and the time of the hot isostatic pressing heat treatment in the step S2 is 235-245 min.
6. The SLM-based high-strength high-plasticity Inconel718 alloy preparation method according to claim 1, wherein the method comprises the following steps: the temperature of the stress-relief annealing treatment in the step S3 is 795-805 ℃, and the time is 25-35 min.
7. The SLM-based high-strength high-plasticity Inconel718 alloy preparation method according to claim 1, wherein the method comprises the following steps: the temperature of the solid solution treatment in the step S4 is 945-955 ℃, and the time is 25-35 min.
8. The method for preparing the SLM-based high-strength high-plasticity Inconel718 alloy according to claim 1 or 7, wherein the method comprises the following steps: in the step S4, after the stress relief annealing treatment operation is completed, the argon atmosphere protection of the high-temperature heating inner chamber is kept, and the temperature of the heating inner chamber is increased at the heating rate of 8-10 ℃/min to perform solution treatment on the Inconel718 alloy blank subjected to the stress relief annealing treatment.
9. The SLM-based high-strength high-plasticity Inconel718 alloy preparation method according to claim 1, wherein the method comprises the following steps: in the double-stage aging treatment of the step S5, the temperature of the first-stage aging treatment is 755-765 ℃, the time is 475 min-485 min, the temperature of the second-stage aging treatment is 645-655 ℃, and the time is 475 min-485 min.
10. The method for preparing the SLM-based high-strength high-plasticity Inconel718 alloy according to claim 1 or 9, wherein the method comprises the following steps: in the double-stage aging treatment of the step S5, after the first-stage aging treatment, the temperature of the heating inner chamber is controlled to be furnace-cooled to the temperature of the second-stage aging treatment at the cooling rate of 40-60 ℃/h.
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