CN115846689A - Solution treatment method for melting GH3230 alloy by laser powder bed and GH3230 alloy - Google Patents

Solution treatment method for melting GH3230 alloy by laser powder bed and GH3230 alloy Download PDF

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CN115846689A
CN115846689A CN202211430098.5A CN202211430098A CN115846689A CN 115846689 A CN115846689 A CN 115846689A CN 202211430098 A CN202211430098 A CN 202211430098A CN 115846689 A CN115846689 A CN 115846689A
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alloy
solution treatment
powder bed
treatment method
laser powder
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CN115846689B (en
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林丹阳
席鑫
李子涵
马瑞
宋晓国
石志峰
胡继旭
檀财旺
董志波
白洁
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Beijing Power Machinery Institute
Harbin Institute of Technology Weihai
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Harbin Institute of Technology Weihai
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Abstract

The invention relates to a solid solution treatment method for a laser powder bed melting GH3230 alloy and the GH3230 alloy, belonging to the field of high temperature alloyThe technical field of gold. In order to solve the problem that the prior art lacks a solid solution treatment method for melting GH3230 alloy by a laser powder bed, the invention provides a solid solution treatment method for melting GH3230 alloy by a laser powder bed, which comprises the following steps: preparing GH3230 alloy through a laser powder bed melting additive manufacturing system; and then heating the GH3230 alloy to 1130-1280 ℃ for solution treatment, preserving the heat for 1-3 h, and cooling to room temperature. The invention improves M while adapting to the laser powder bed fusion forming technology 6 Volume fraction and morphological distribution of C carbide in the alloy such that M 6 The average size of C is reduced, the stress concentration in the stretching process is reduced, the elongation of the alloy is greatly improved on the premise of ensuring higher strength of the alloy, and the GH3230 alloy with both strength and plasticity is obtained.

Description

一种激光粉末床熔融GH3230合金的固溶处理方法及GH3230 合金A solid solution treatment method of laser powder bed fusion GH3230 alloy and GH3230 alloy

技术领域technical field

本发明属于高温合金技术领域,尤其涉及一种激光粉末床熔融GH3230合金的固溶处理方法及GH3230合金。The invention belongs to the technical field of superalloys, and in particular relates to a solid solution treatment method for laser powder bed melting GH3230 alloy and the GH3230 alloy.

背景技术Background technique

高性能航空飞行器的发展需要提高发动机推重比,这对发动机热端部件提出了更高的要求,包括采用具有更高高温强度的材料服役,以及一体化结构设计减重。GH3230合金是一种固溶强化型Ni-Cr-W-Mo高温合金,该合金在900℃以下长期使用具有良好的持久和抗蠕变性能,短期工作温度可达1100℃,长期暴露在1150℃的环境仍具有优异抗氧化能力和热稳定性,被广泛应用于航空发动机热端部件。The development of high-performance aerospace vehicles requires an increase in the thrust-to-weight ratio of the engine, which puts forward higher requirements for the hot-end parts of the engine, including the use of materials with higher high-temperature strength for service, and integrated structural design for weight reduction. GH3230 alloy is a solid solution strengthened Ni-Cr-W-Mo high-temperature alloy. The alloy has good durability and creep resistance for long-term use below 900°C. The short-term working temperature can reach 1100°C, and the long-term exposure to 1150°C The environment still has excellent oxidation resistance and thermal stability, and is widely used in aero-engine hot-end parts.

采用传统材料制造发动机热端部件存在新型拓扑结构加工难度大、加工周期长和材料浪费等问题,严重阻碍了航空发动机技术的快速迭代。激光粉末床熔融加工是一个非平衡凝固过程,成形过程中熔池经历107K/s量级的超快速熔凝,造成激光粉末床熔融GH3230合金具有外延生长的不均匀亚结构和位错网,且Cr、B、C、Si等低熔点元素在晶界和亚晶界富集导致的低塑性和高温服役过程组织转变带来的性能不稳定性使得GH3230合金不适宜在沉积态直接进行服役。The use of traditional materials to manufacture engine hot-end components has problems such as difficult processing of new topological structures, long processing cycles, and material waste, which seriously hinder the rapid iteration of aero-engine technology. Laser powder bed fusion processing is a non-equilibrium solidification process. During the forming process, the molten pool undergoes ultra-fast solidification on the order of 10 7 K/s, resulting in the inhomogeneous substructure and dislocation network of epitaxial growth in laser powder bed fusion GH3230 alloy. , and Cr, B, C, Si and other low-melting elements enriched in grain boundaries and sub-grain boundaries lead to low plasticity and performance instability caused by microstructure transformation during high-temperature service, making GH3230 alloy not suitable for direct service in the deposited state .

公开号为CN114855030A的发明专利申请《适应选区激光熔化成形的Ni-Cr-W基高温合金及制备方法》通过增加析出相含量使得合金强度超过了冷轧态Haynes230,得到高强度样品。但大量Al、Ti、Nb、B和Ta元素的引入使得该合金成分与GH3230的成分存在巨大的差异,使得合金主强化机制由固溶强化转变为析出强化,合金性质发生了改变。而且其制备的合金在沉积态存在大量的Laves相,长时间高温服役过程中Laves相的不稳定性限制了该合金在燃烧室的应用。The invention patent application with the publication number CN114855030A "Ni-Cr-W-based superalloy suitable for selective laser melting forming and its preparation method" increases the content of precipitates to make the alloy strength exceed that of cold-rolled Haynes230, and obtains high-strength samples. However, the introduction of a large amount of Al, Ti, Nb, B and Ta elements makes the composition of the alloy different from that of GH3230, which makes the main strengthening mechanism of the alloy change from solid solution strengthening to precipitation strengthening, and the properties of the alloy change. Moreover, the prepared alloy has a large amount of Laves phase in the deposited state, and the instability of the Laves phase during long-term high-temperature service limits the application of the alloy in the combustion chamber.

固溶强化是调控合金微观组织进而改善合金力学性能的有效手段,晶粒内部大量颗粒状M6C碳化物的析出可以有效提高高温合金的强度和抗蠕变性能,但粗大的M6C颗粒会成为应力集中点,降低裂纹萌生临界载荷,严重影响合金的拉伸塑性。Solid solution strengthening is an effective means to control the microstructure of alloys and improve the mechanical properties of alloys. The precipitation of a large number of granular M 6 C carbides in the grains can effectively improve the strength and creep resistance of superalloys, but the coarse M 6 C particles It will become a stress concentration point, reduce the critical load of crack initiation, and seriously affect the tensile plasticity of the alloy.

公开号为CN114635059A的发明专利申请《一种Ni-Cr-W基合金及其制备方法》通过合金成分改变后的熔炼、锻造、热轧、冷轧和固溶热处理的方式制备了Ni-Cr-W基合金。该方法的合金经调控后具有均匀生长的晶粒和二次碳化物,相比于传统GH3230固溶处理的高温持久性能得到提升。然而,二次碳化物高温环境不稳定会导致合金高温服役过程中的性能不稳定,而且固溶处理后合金的塑性并没有得到提升。The invention patent application with the publication number CN114635059A "A Ni-Cr-W-based Alloy and Its Preparation Method" prepared Ni-Cr-W- W base alloy. The alloy of this method has uniformly grown grains and secondary carbides after adjustment, and the high-temperature durability performance is improved compared with the traditional GH3230 solution treatment. However, the unstable high-temperature environment of secondary carbides will lead to unstable performance of the alloy during high-temperature service, and the plasticity of the alloy has not been improved after solution treatment.

可见,现有的Ni-Cr-W合金的固溶处理方式是针对传统铸造、锻造和轧制制备合金提出的,而对于激光粉末床熔融固溶强化GH3230合金非平衡凝固后微观组织和高温稳定一次碳化物尺寸特征的均匀调控和强塑性综合性能调控等问题还没有解决。It can be seen that the existing solid solution treatment method of Ni-Cr-W alloy is proposed for the preparation of alloy by traditional casting, forging and rolling, but for the microstructure and high temperature stability of GH3230 alloy after non-equilibrium solidification by laser powder bed fusion solid solution The uniform control of the size characteristics of primary carbides and the control of the comprehensive properties of strong plasticity have not yet been resolved.

发明内容Contents of the invention

为解决现有技术缺乏针对激光粉末床熔融GH3230合金的固溶处理方法的问题,本发明提供了一种激光粉末床熔融GH3230合金的固溶处理方法及GH3230合金。In order to solve the problem that the prior art lacks a solution treatment method for laser powder bed fusion GH3230 alloy, the present invention provides a solution treatment method for laser powder bed fusion GH3230 alloy and the GH3230 alloy.

本发明的技术方案:Technical scheme of the present invention:

一种激光粉末床熔融GH3230合金的固溶处理方法,包括如下步骤:A solid solution treatment method for laser powder bed fusion GH3230 alloy, comprising the steps of:

步骤一、制备GH3230合金:Step 1, preparation of GH3230 alloy:

在惰性气氛保护下通过激光粉末床熔融增材制造系统制备GH3230合金;GH3230 alloy was prepared by laser powder bed fusion additive manufacturing system under the protection of inert atmosphere;

步骤二、GH3230合金的固溶处理:Step 2, solution treatment of GH3230 alloy:

在压强不大于1000Pa的真空环境中将步骤一制备的GH3230合金升温至1130~1280℃进行固溶处理,保温1~3h后,冷却至室温。In a vacuum environment with a pressure not greater than 1000 Pa, heat the GH3230 alloy prepared in step 1 to 1130-1280° C. for solution treatment, keep it warm for 1-3 hours, and then cool it to room temperature.

进一步的,步骤一制备GH3230合金使用的GH3230球形粉末的成分按质量百分数满足:C:0.05~0.15%,Si:0.25~0.75%,Mn:0.30~1%,Cr:20~24%,Fe:≤3%,Mo:1~3%,Co:≤5%,W:13~15%,Al:0.2~0.5%,Ti:≤0.1%,Cu:≤0.5%,La:0.005~0.05%,B:≤0.005%,余量为Ni。Further, the composition of the GH3230 spherical powder used in the preparation of the GH3230 alloy in step 1 satisfies the following mass percentages: C: 0.05-0.15%, Si: 0.25-0.75%, Mn: 0.30-1%, Cr: 20-24%, Fe: ≤3%, Mo: 1~3%, Co: ≤5%, W: 13~15%, Al: 0.2~0.5%, Ti: ≤0.1%, Cu: ≤0.5%, La: 0.005~0.05%, B: ≤0.005%, the balance being Ni.

进一步的,步骤一制备GH3230合金使用的GH3230球形粉末的成分按质量百分数满足:C:0.07%,Si:0.35%,Mn:0.5%,Cr:21.74%,Fe:1.9%,Mo:2.8%,Co:2.1%,W:14.7%,Al:0.45%,Ti:0.1%,Cu:0.01%,La:0.01%,B:0.001%,余量为Ni。Further, the composition of the GH3230 spherical powder used in the preparation of the GH3230 alloy in step 1 meets the following mass percentages: C: 0.07%, Si: 0.35%, Mn: 0.5%, Cr: 21.74%, Fe: 1.9%, Mo: 2.8%, Co: 2.1%, W: 14.7%, Al: 0.45%, Ti: 0.1%, Cu: 0.01%, La: 0.01%, B: 0.001%, and the balance is Ni.

进一步的,步骤一制备GH3230合金使用的GH3230球形粉末的粒径尺寸为15~53μm。Further, the particle size of the GH3230 spherical powder used in the preparation of the GH3230 alloy in Step 1 is 15-53 μm.

进一步的,步骤一所述惰性气氛为氩气气氛,所述氩气气氛的含氧量低于100ppm。Further, the inert atmosphere in Step 1 is an argon atmosphere, and the oxygen content of the argon atmosphere is lower than 100ppm.

进一步的,步骤一所述激光粉末床熔融增材制造系统中光源为YAG固体激光,激光功率为120~300W,光斑直径为0.087mm,激光扫描速率为500~1300mm/s,铺粉厚度为0.02~0.05mm,扫描间距为0.05~0.12mm,扫描策略为67°交叉条带状扫描,基板预热温度为80~160℃。Further, the light source in the laser powder bed fusion additive manufacturing system described in step 1 is a YAG solid-state laser, the laser power is 120-300W, the spot diameter is 0.087mm, the laser scanning rate is 500-1300mm/s, and the powder coating thickness is 0.02 ~0.05mm, the scanning distance is 0.05~0.12mm, the scanning strategy is 67° cross-strip scanning, and the substrate preheating temperature is 80~160℃.

进一步的,步骤二所述GH3230合金升温是从室温以8~10℃/min的速度升温到1130℃~1280℃。Further, the temperature rise of the GH3230 alloy in step 2 is from room temperature to 1130°C to 1280°C at a rate of 8-10°C/min.

进一步的,步骤二所述冷却至室温是采用高压氩气快速冷却。Further, the cooling to room temperature described in step 2 is rapid cooling with high-pressure argon.

一种本发明激光粉末床熔融GH3230合金的固溶处理方法处理得到的GH3230合金,处理所得GH3230合金的基体为全奥氏体组织,晶粒尺寸控制在40~80μm范围内。A GH3230 alloy obtained by the laser powder bed fusion GH3230 alloy solid solution treatment method of the present invention, the matrix of the processed GH3230 alloy is a full austenite structure, and the grain size is controlled within the range of 40-80 μm.

进一步的,析出碳化物为M6C,M6C在GH3230合金中的体积分数小于10%,原晶界位置M6C平均尺寸小于2μm,晶内M6C平均尺寸小于0.3μm。Further, the precipitated carbide is M 6 C, the volume fraction of M 6 C in the GH3230 alloy is less than 10%, the average size of M 6 C at the original grain boundary position is less than 2 μm, and the average size of M 6 C in the grain is less than 0.3 μm.

本发明的有益效果:Beneficial effects of the present invention:

本发明提供的激光粉末床熔融GH3230固溶处理方法,能够消除沉积态试样亚结构和位错网,促进再结晶的发生,达到改善组织,优化合金性能的目的。本发明在适应激光粉末床熔融成形技术的同时,可以有效调控一次稳定碳化物M6C的特征,使M23C6碳化物向高温稳定M6C转变,析出碳化物中M6C占90%以上,改善M6C碳化物在GH3230合金中的体积分数和形态分布,通过调节固溶温度使M6C平均尺寸减小,降低了拉伸过程中的应力集中,抑制脆性开裂,保证激光粉末床熔融GH3230合金具有较高强度的前提下大幅提高其延伸率。经过本发明固溶处理方法得到的GH3230合金的极限抗拉强度可达沉积态GH3230合金70%以上,同时其最大延伸率较沉积态GH3230合金提高1.5倍以上。The laser powder bed fusion GH3230 solid solution treatment method provided by the invention can eliminate the substructure and dislocation network of the deposited sample, promote the occurrence of recrystallization, achieve the purpose of improving the structure and optimizing the performance of the alloy. While adapting to the laser powder bed fusion forming technology, the present invention can effectively control the characteristics of the primary stable carbide M 6 C, so that the M 23 C 6 carbide can transform into a high-temperature stable M 6 C, and M 6 C accounts for 90% of the precipitated carbide. % or more, improve the volume fraction and morphological distribution of M 6 C carbides in GH3230 alloy, reduce the average size of M 6 C by adjusting the solution temperature, reduce the stress concentration in the stretching process, inhibit brittle cracking, and ensure that the laser The powder bed fusion GH3230 alloy has a high strength and greatly improves its elongation. The ultimate tensile strength of the GH3230 alloy obtained by the solution treatment method of the invention can reach more than 70% of the deposited GH3230 alloy, and its maximum elongation is more than 1.5 times higher than that of the deposited GH3230 alloy.

本发明激光粉末床熔融GH3230固溶处理方法简单,调控效果显著,实现了激光粉末床熔融GH3230合金强度和延伸率的可控化,为其应用奠定了基础。由本发明固溶处理方法得到的强度和塑性兼具的GH3230合金特别适用于900℃以上高温环境下长期使用的部件,如航空涡扇发动机燃烧室、轴流轮等。The laser powder bed fusion GH3230 solid solution treatment method of the present invention is simple, and the control effect is remarkable, realizes the controllability of the strength and elongation of the laser powder bed fusion GH3230 alloy, and lays the foundation for its application. The GH3230 alloy obtained by the solid solution treatment method of the present invention has both strength and plasticity is especially suitable for components used for a long time in a high temperature environment above 900°C, such as an aviation turbofan engine combustion chamber, an axial flow wheel, and the like.

附图说明Description of drawings

图1为激光粉末床熔融增材制备GH3230合金的成形过程示意图;Figure 1 is a schematic diagram of the forming process of GH3230 alloy prepared by laser powder bed fusion additive;

图2为实施例1中激光粉末床熔融增材制备所得沉积态GH3230合金成形试样不同部位的微观组织照片;Fig. 2 is the microstructure photo of different parts of the deposited state GH3230 alloy forming sample prepared by laser powder bed fusion additive in embodiment 1;

图3为实施例1-实施例4不同固溶处理方法所得GH3230合金的微观组织照片和碳化物形态照片;Fig. 3 is the microstructure photo and the carbide morphology photo of the GH3230 alloy obtained by different solution treatment methods of embodiment 1-embodiment 4;

图4为沉积态GH3230合金和实施例1-实施例4不同固溶处理方法所得GH3230合金的晶粒特征照片;Fig. 4 is the grain feature photo of GH3230 alloy obtained by different solution treatment methods of deposited state GH3230 alloy and embodiment 1-embodiment 4;

图5为沉积态GH3230合金和实施例1-实施例4不同固溶处理方法所得GH3230合金的工程应力应变曲线对比图;Fig. 5 is the contrast diagram of engineering stress-strain curves of deposited state GH3230 alloy and GH3230 alloy obtained by different solution treatment methods of embodiment 1-embodiment 4;

图6为沉积态GH3230合金和实施例1-实施例4不同固溶处理方法所得GH3230合金的抗拉强度和延伸率对比图。Fig. 6 is a comparison chart of the tensile strength and elongation of the as-deposited GH3230 alloy and the GH3230 alloy obtained by different solution treatment methods in Example 1-Example 4.

具体实施方式Detailed ways

下面结合实施例对本发明的技术方案做进一步的说明,但并不局限于此,凡是对本发明技术方案进行修改或者等同替换,而不脱离本发明技术方案的精神和范围,均应涵盖在本发明的保护范围中。下列实施例中未具体注明的工艺设备或装置均采用本领域内的常规设备或装置,若未特别指明,本发明实施例中所用的原料等均可市售获得;若未具体指明,本发明实施例中所用的技术手段均为本领域技术人员所熟知的常规手段。The technical solution of the present invention will be further described below in conjunction with the examples, but it is not limited thereto. Any modification or equivalent replacement of the technical solution of the present invention without departing from the spirit and scope of the technical solution of the present invention should be covered by the present invention within the scope of protection. The process equipment or devices not specifically indicated in the following examples all adopt conventional equipment or devices in the art. If not specified, the raw materials used in the examples of the present invention, etc. can be commercially available; if not specified, this The technical means used in the embodiments of the invention are conventional means well known to those skilled in the art.

实施例1Example 1

本实施例提供了一种激光粉末床熔融GH3230合金的固溶处理方法,包括如下步骤:This embodiment provides a solution treatment method for laser powder bed fusion GH3230 alloy, comprising the following steps:

步骤一、在惰性气氛保护下通过激光粉末床熔融增材制造系统制备GH3230合金。Step 1, under the protection of an inert atmosphere, the GH3230 alloy is prepared by a laser powder bed fusion additive manufacturing system.

本实施例使用的GH3230合金球形粉末的成分按质量百分数满足:Ni:55.26%,Cr:21.74%,W:14.7%,Mo:2.8%,Fe:1.9%,Co:2.1%,Mn:0.5%,Si:0.35%,Al:0.45%,C:0.07%,Ti:0.1%,Cu:0.01%,La:0.01%,B:0.001%。The composition of the GH3230 alloy spherical powder used in this example satisfies by mass percentage: Ni: 55.26%, Cr: 21.74%, W: 14.7%, Mo: 2.8%, Fe: 1.9%, Co: 2.1%, Mn: 0.5% , Si: 0.35%, Al: 0.45%, C: 0.07%, Ti: 0.1%, Cu: 0.01%, La: 0.01%, B: 0.001%.

将尺寸为15~53μm的GH3230合金球形粉末放入粉仓中,将316L不锈钢基板放入成形舱中,关闭舱门后冲入氩气,使氧含量控制在100ppm以下,通过平台电阻加热方式将基板预热到100℃,开始激光粉末床熔融GH3230合金加工。Put the GH3230 alloy spherical powder with a size of 15-53 μm into the powder bin, put the 316L stainless steel substrate into the forming cabin, close the cabin door and pour in argon gas to keep the oxygen content below 100ppm, and heat it through platform resistance heating. The substrate is preheated to 100°C, and the laser powder bed fusion GH3230 alloy processing starts.

本实施例使用的激光器为YAG激光器,将GH3230粉末均匀铺在基板上,通过扫描振镜摆动激光束将GH3230粉末熔化沉积在316L基板上,平台下降,再次铺粉熔化,如此往复,制备出所需要的试样。The laser used in this example is a YAG laser. The GH3230 powder is evenly spread on the substrate, and the GH3230 powder is melted and deposited on the 316L substrate by swinging the laser beam through the scanning galvanometer. The platform is lowered, and the powder is spread and melted again. of samples.

本实施例激光粉末床熔融增材制造GH3230合金的工艺参数为:激光功率为245W,光斑直径为0.087mm,激光扫描速率为900mm/s,铺粉厚度为0.04mm,扫描间距为0.11mm,扫描策略为67°交叉条带状扫描;成形尺寸为71mm×10mm×10mm,成形过程示意图如图1所示。The process parameters of laser powder bed fusion additive manufacturing GH3230 alloy in this embodiment are as follows: laser power is 245W, spot diameter is 0.087mm, laser scanning rate is 900mm/s, powder coating thickness is 0.04mm, scanning distance is 0.11mm, scanning The strategy is 67° cross-strip scanning; the forming size is 71mm×10mm×10mm, and the schematic diagram of the forming process is shown in Figure 1.

本实施例所得沉积态GH3230成形试样的极限抗拉强度为937MPa,延伸率为15%,其微观结构如图2所示,沉积态合金的微观结构呈现出奥氏体柱状晶粒,晶粒内部为柱状树枝状和细小的胞状亚结构,在亚结构边界分布有大量的位错网。The ultimate tensile strength of the deposited GH3230 formed sample obtained in this embodiment is 937MPa, and the elongation is 15%. The interior is columnar dendritic and fine cellular substructures, and a large number of dislocation networks are distributed at the boundaries of the substructures.

步骤二、GH3230合金的固溶处理:Step 2, solution treatment of GH3230 alloy:

将步骤一制备的沉积态GH3230试样放入真空热处理炉中,在压强不大于1000Pa的真空环境中,以10℃/min的加热速率将试样加热至1130℃进行固溶处理,保温2h后通入高压氩气快速冷却至室温。Put the deposited GH3230 sample prepared in step 1 into a vacuum heat treatment furnace, heat the sample to 1130°C at a heating rate of 10°C/min in a vacuum environment with a pressure not greater than 1000Pa for solution treatment, and keep it for 2 hours Rapidly cool to room temperature with high-pressure argon.

本实施例中1130℃固溶处理后GH3230合金的极限抗拉强度为900MPa,延伸率为16.7%。In this embodiment, the ultimate tensile strength of the GH3230 alloy after solution treatment at 1130° C. is 900 MPa, and the elongation is 16.7%.

实施例2Example 2

本实施例提供了一种激光粉末床熔融GH3230合金的固溶处理方法,本实施例固溶处理方法与实施例1的区别仅在于:本实施例的步骤二具体固溶温度和时间为:This embodiment provides a solution treatment method for laser powder bed fusion GH3230 alloy. The difference between the solution treatment method of this embodiment and Example 1 is that the specific solution temperature and time of step 2 of this embodiment are:

将步骤一制备的沉积态GH3230试样放入真空热处理炉中,在压强不大于1000Pa的真空环境中,以10℃/min的加热速率将试样加热至1180℃进行固溶处理,保温2h后通入高压氩气快速冷却至室温。Put the deposited GH3230 sample prepared in step 1 into a vacuum heat treatment furnace, heat the sample to 1180°C at a heating rate of 10°C/min in a vacuum environment with a pressure not greater than 1000Pa for solution treatment, and keep it for 2 hours Rapidly cool to room temperature with high-pressure argon.

本实施例中1180℃固溶处理后GH3230合金的极限抗拉强度为803MPa,延伸率为18%。In this example, the ultimate tensile strength of the GH3230 alloy after solution treatment at 1180° C. is 803 MPa, and the elongation is 18%.

实施例3Example 3

本实施例提供了一种激光粉末床熔融GH3230合金的固溶处理方法,本实施例固溶处理方法与实施例1的区别仅在于:本实施例的步骤二具体固溶温度和时间为:This embodiment provides a solution treatment method for laser powder bed fusion GH3230 alloy. The difference between the solution treatment method of this embodiment and Example 1 is that the specific solution temperature and time of step 2 of this embodiment are:

将步骤一制备的沉积态GH3230试样放入真空热处理炉中,在压强不大于1000Pa的真空环境中,以10℃/min的加热速率将试样加热至1230℃进行固溶处理,保温2h后通入高压氩气快速冷却至室温。Put the deposited GH3230 sample prepared in step 1 into a vacuum heat treatment furnace, heat the sample to 1230°C at a heating rate of 10°C/min in a vacuum environment with a pressure not greater than 1000Pa for solution treatment, and keep it warm for 2 hours Rapidly cool to room temperature with high-pressure argon.

本实施例中1230℃固溶处理后GH3230合金的极限抗拉强度为750MPa,延伸率为21%。In this example, the ultimate tensile strength of the GH3230 alloy after solution treatment at 1230° C. is 750 MPa, and the elongation is 21%.

实施例4Example 4

本实施例提供了一种激光粉末床熔融GH3230合金的固溶处理方法,本实施例固溶处理方法与实施例1的区别仅在于:本实施例的步骤二具体固溶温度和时间为:This embodiment provides a solution treatment method for laser powder bed fusion GH3230 alloy. The difference between the solution treatment method of this embodiment and Example 1 is that the specific solution temperature and time of step 2 of this embodiment are:

将步骤一制备的沉积态GH3230试样放入真空热处理炉中,在压强不大于1000Pa的真空环境中,以10℃/min的加热速率将试样加热至1280℃进行固溶处理,保温2h后通入高压氩气快速冷却至室温。Put the deposited GH3230 sample prepared in step 1 into a vacuum heat treatment furnace, heat the sample to 1280°C at a heating rate of 10°C/min in a vacuum environment with a pressure not greater than 1000Pa for solution treatment, and keep it warm for 2 hours Rapidly cool to room temperature with high-pressure argon.

本实施例中1280℃固溶处理后GH3230合金的极限抗拉强度为670MPa,延伸率为42%。In this example, the ultimate tensile strength of the GH3230 alloy after solution treatment at 1280° C. is 670 MPa, and the elongation is 42%.

图3为实施例1-实施例4不同固溶处理方法所得GH3230合金的微观组织照片和碳化物形态照片;上排照片为微观组织照片,下排照片为碳化物形态照片;其中a图为实施例1所得GH3230合金的微观组织照片,b图为实施例2所得GH3230合金的微观组织照片,c图为实施例3所得GH3230合金的微观组织照片,d图为实施例4所得GH3230合金的微观组织照片。Fig. 3 is the microstructure photo and the carbide morphology photo of the GH3230 alloy obtained by different solution treatment methods of embodiment 1-embodiment 4; the upper row of photos is a microstructure photo, and the lower row of photos is a carbide morphology photo; wherein a is for implementation The microstructure photograph of the GH3230 alloy gained in Example 1, the b figure is the microstructure photograph of the GH3230 alloy gained in Example 2, the c figure is the microstructure photograph of the GH3230 alloy gained in Example 3, and the d figure is the microstructure photograph of the GH3230 alloy gained in Example 4 photo.

图4为沉积态GH3230合金和实施例1-实施例4不同固溶处理方法所得GH3230合金的晶粒特征照片;a图为沉积态GH3230合金的晶粒特征照片,b图为实施例1所得GH3230合金的晶粒特征照片,c图为实施例2所得GH3230合金的晶粒特征照片,d图为实施例3所得GH3230合金的晶粒特征照片,e图为实施例4所得GH3230合金的晶粒特征照片。Fig. 4 is the grain feature photo of deposited state GH3230 alloy and embodiment 1-embodiment 4 different solid solution treatment methods of GH3230 alloy; a picture is the grain feature picture of deposited state GH3230 alloy, b picture is embodiment 1 gained GH3230 The grain characteristic photograph of alloy, c figure is the grain characteristic photograph of embodiment 2 gained GH3230 alloy, d figure is the grain characteristic photograph of embodiment 3 gained GH3230 alloy, e figure is the grain characteristic photograph of embodiment 4 gained GH3230 alloy photo.

结合图3和图4所示,实施例1所得GH3230合金的奥氏体晶粒为柱状晶,M6C大量在晶界和原始亚晶界位置析出,M6C颗粒尺寸呈现双峰分布,晶界M6C颗粒尺寸大小为180~2850nm,晶内M6C颗粒尺寸为40~280nm,碳化物体积分数为9.04vt%;As shown in Figure 3 and Figure 4, the austenite grains of the GH3230 alloy obtained in Example 1 are columnar grains, and a large amount of M 6 C precipitates at the grain boundaries and original sub-grain boundaries, and the M 6 C particle size presents a bimodal distribution. The grain boundary M 6 C particle size is 180-2850nm, the intra-granular M 6 C particle size is 40-280nm, and the carbide volume fraction is 9.04vt%;

实施例2所得GH3230合金的奥氏体晶粒仍为柱状晶,M6C发生长大,晶界M6C颗粒尺寸大小为570~3500nm,晶内M6C颗粒尺寸为60~360nm,碳化物体积分数为7.79vt%;The austenite grains of the GH3230 alloy obtained in Example 2 are still columnar grains, M 6 C grows, the grain boundary M 6 C particle size is 570-3500nm, and the intragranular M 6 C particle size is 60-360nm. The volume fraction of the substance is 7.79vt%;

实施例3所得GH3230合金的奥氏体晶粒发生再结晶转变为等轴晶,M6C大量固溶于基体,晶界M6C颗粒尺寸大小为320~2080nm,晶内M6C颗粒尺寸为30~350nm,碳化物体积分数为3.74vt%; The austenite grains of the GH3230 alloy obtained in Example 3 undergo recrystallization and transform into equiaxed grains, and a large amount of M 6 C is solid-dissolved in the matrix. 30-350nm, carbide volume fraction 3.74vt%;

实施例4所得GH3230合金的奥氏体晶粒发生完全再结晶,M6C几乎完全固溶于基体,但仍存在少量纳米析出相。The austenite grains of the GH3230 alloy obtained in Example 4 were completely recrystallized, and M 6 C was almost completely dissolved in the matrix, but there were still a small amount of nano-precipitated phases.

图5为沉积态GH3230合金和实施例1-实施例4不同固溶处理方法所得GH3230合金的工程应力应变曲线对比图;图6为沉积态GH3230合金和实施例1-实施例4不同固溶处理方法所得GH3230合金的抗拉强度和延伸率对比图。Fig. 5 is the comparison chart of engineering stress-strain curves of the deposited GH3230 alloy and the GH3230 alloy obtained by different solution treatment methods of Example 1-Example 4; Fig. 6 is the different solution treatment of the deposited GH3230 alloy and Example 1-Example 4 Comparison chart of tensile strength and elongation of GH3230 alloy obtained by the method.

由图5和图6所见,随着固溶温度的升高,极限抗拉强度逐渐下降而延伸率在不断增大,拉伸强度向延伸率的转化率也在不断增大;在升温过程中,由于微米级晶界M6C向基体发生固溶,降低了样品的应力集中,而1180℃固溶处理试样的微米级晶界M6C发生长大,这使得强度下降13%而延伸率提高16%,强度向延伸率的转换效率为1.23,在1280℃固溶处理后在晶界微米级M6C碳化物接近完全消除,激光粉末床熔融GH3230试样的延伸率则大幅度提高1.6倍,且保持较高的室温拉伸强度(下降28%),强度向延伸率的转换效率为5.71。因此,可以根据目标激光粉末床熔融GH3230合金的性能要求,选择合适的热处理方法,从而实现强度和塑性的可控性。It can be seen from Figure 5 and Figure 6 that with the increase of the solution temperature, the ultimate tensile strength gradually decreases while the elongation increases, and the conversion rate of tensile strength to elongation also increases; during the heating process In the case of solid solution of micron-sized grain boundary M 6 C in the matrix, the stress concentration of the sample is reduced, while the micron-sized grain boundary M 6 C of the solid solution treated sample at 1180°C grows, which makes the strength decrease by 13% and The elongation rate increased by 16%, and the conversion efficiency from strength to elongation rate was 1.23. After solution treatment at 1280°C, the micron-sized M 6 C carbides at the grain boundary were almost completely eliminated, and the elongation rate of the laser powder bed fusion GH3230 sample was greatly improved. Improve 1.6 times, and keep higher room temperature tensile strength (decrease 28%), the conversion efficiency of strength to elongation is 5.71. Therefore, the appropriate heat treatment method can be selected according to the performance requirements of the target laser powder bed fusion GH3230 alloy, so as to achieve the controllability of strength and plasticity.

实施例5Example 5

本实施例提供了一种激光粉末床熔融GH3230合金的固溶处理方法,本实施例固溶处理方法与实施例1的区别仅在于:本实施例的步骤二具体固溶温度和时间为:This embodiment provides a solution treatment method for laser powder bed fusion GH3230 alloy. The difference between the solution treatment method of this embodiment and Example 1 is that the specific solution temperature and time of step 2 of this embodiment are:

将步骤一制备的沉积态GH3230试样放入真空热处理炉中,在压强不大于1000Pa的真空环境中,以10℃/min的加热速率将试样加热至1130℃进行固溶处理,保温1h后通入高压氩气快速冷却至室温。Put the deposited GH3230 sample prepared in step 1 into a vacuum heat treatment furnace, and heat the sample to 1130°C at a heating rate of 10°C/min in a vacuum environment with a pressure not greater than 1000Pa for solution treatment. Rapidly cool to room temperature with high-pressure argon.

本实施例中1130℃固溶处理后GH3230合金的极限抗拉强度为910MPa,延伸率为18.5%。In this example, the ultimate tensile strength of the GH3230 alloy after solution treatment at 1130° C. is 910 MPa, and the elongation is 18.5%.

实施例6Example 6

本实施例提供了一种激光粉末床熔融GH3230合金的固溶处理方法,本实施例固溶处理方法与实施例1的区别仅在于:本实施例的步骤二具体固溶温度和时间为:This embodiment provides a solution treatment method for laser powder bed fusion GH3230 alloy. The difference between the solution treatment method of this embodiment and Example 1 is that the specific solution temperature and time of step 2 of this embodiment are:

将步骤一制备的沉积态GH3230试样放入真空热处理炉中,在压强不大于1000Pa的真空环境中,以10℃/min的加热速率将试样加热至1180℃进行固溶处理,保温1h后通入高压氩气快速冷却至室温。Put the deposited GH3230 sample prepared in step 1 into a vacuum heat treatment furnace, and heat the sample to 1180°C at a heating rate of 10°C/min in a vacuum environment with a pressure not greater than 1000Pa for solution treatment. Rapidly cool to room temperature with high-pressure argon.

本实施例中1180℃固溶处理后GH3230合金的极限抗拉强度为824MPa,延伸率为17.3%。In this example, the ultimate tensile strength of the GH3230 alloy after solution treatment at 1180° C. is 824 MPa, and the elongation is 17.3%.

实施例7Example 7

本实施例提供了一种激光粉末床熔融GH3230合金的固溶处理方法,本实施例固溶处理方法与实施例1的区别仅在于:本实施例的步骤二具体固溶温度和时间为:This embodiment provides a solution treatment method for laser powder bed fusion GH3230 alloy. The difference between the solution treatment method of this embodiment and Example 1 is that the specific solution temperature and time of step 2 of this embodiment are:

将步骤一制备的沉积态GH3230试样放入真空热处理炉中,在压强不大于1000Pa的真空环境中,以10℃/min的加热速率将试样加热至1230℃进行固溶处理,保温1h后通入高压氩气快速冷却至室温。Put the deposited GH3230 sample prepared in step 1 into a vacuum heat treatment furnace, and heat the sample to 1230°C at a heating rate of 10°C/min in a vacuum environment with a pressure not greater than 1000Pa for solution treatment. Rapidly cool to room temperature with high-pressure argon.

本实施例中1230℃固溶处理后GH3230合金的极限抗拉强度为741MPa,延伸率为23%。In this embodiment, the ultimate tensile strength of the GH3230 alloy after solution treatment at 1230° C. is 741 MPa, and the elongation is 23%.

实施例8Example 8

本实施例提供了一种激光粉末床熔融GH3230合金的固溶处理方法,本实施例固溶处理方法与实施例1的区别仅在于:本实施例的步骤二具体固溶温度和时间为:This embodiment provides a solution treatment method for laser powder bed fusion GH3230 alloy. The difference between the solution treatment method of this embodiment and Example 1 is that the specific solution temperature and time of step 2 of this embodiment are:

将步骤一制备的沉积态GH3230试样放入真空热处理炉中,在压强不大于1000Pa的真空环境中,以10℃/min的加热速率将试样加热至1280℃进行固溶处理,保温1h后通入高压氩气快速冷却至室温。Put the deposited GH3230 sample prepared in step 1 into a vacuum heat treatment furnace, and heat the sample to 1280°C at a heating rate of 10°C/min in a vacuum environment with a pressure not greater than 1000Pa for solution treatment. Rapidly cool to room temperature with high-pressure argon.

本实施例中1280℃固溶处理后GH3230合金的极限抗拉强度为657MPa,延伸率为39%。In this example, the ultimate tensile strength of the GH3230 alloy after solution treatment at 1280° C. is 657 MPa, and the elongation is 39%.

Claims (10)

1.一种激光粉末床熔融GH3230合金的固溶处理方法,其特征在于,包括如下步骤:1. a solid solution treatment method of laser powder bed fusion GH3230 alloy, is characterized in that, comprises the steps: 步骤一、制备GH3230合金:Step 1, preparation of GH3230 alloy: 在惰性气氛保护下通过激光粉末床熔融增材制造系统制备GH3230合金;GH3230 alloy was prepared by laser powder bed fusion additive manufacturing system under the protection of inert atmosphere; 步骤二、GH3230合金的固溶处理:Step 2, solution treatment of GH3230 alloy: 在压强不大于1000Pa的真空环境中将步骤一制备的GH3230合金升温至1130~1280℃进行固溶处理,保温1~3h后,冷却至室温。In a vacuum environment with a pressure not greater than 1000 Pa, heat the GH3230 alloy prepared in step 1 to 1130-1280° C. for solution treatment, keep it warm for 1-3 hours, and then cool it to room temperature. 2.根据权利要求1所述一种激光粉末床熔融GH3230合金的固溶处理方法,其特征在于,步骤一制备GH3230合金使用的GH3230球形粉末的成分按质量百分数满足:C:0.05~0.15%,Si:0.25~0.75%,Mn:0.30~1%,Cr:20~24%,Fe:≤3%,Mo:1~3%,Co:≤5%,W:13~15%,Al:0.2~0.5%,Ti:≤0.1%,Cu:≤0.5%,La:0.005~0.05%,B:≤0.005%,余量为Ni。2. A solid solution treatment method for laser powder bed fusion GH3230 alloy according to claim 1, characterized in that the composition of the GH3230 spherical powder used in step 1 to prepare the GH3230 alloy satisfies by mass percentage: C: 0.05-0.15%, Si: 0.25-0.75%, Mn: 0.30-1%, Cr: 20-24%, Fe: ≤3%, Mo: 1-3%, Co: ≤5%, W: 13-15%, Al: 0.2 ~0.5%, Ti: ≤0.1%, Cu: ≤0.5%, La: 0.005~0.05%, B: ≤0.005%, and the balance is Ni. 3.根据权利要求1或2所述一种激光粉末床熔融GH3230合金的固溶处理方法,其特征在于,步骤一制备GH3230合金使用的GH3230球形粉末的成分按质量百分数满足:C:0.07%,Si:0.35%,Mn:0.5%,Cr:21.74%,Fe:1.9%,Mo:2.8%,Co:2.1%,W:14.7%,Al:0.45%,Ti:0.1%,Cu:0.01%,La:0.01%,B:0.001%,余量为Ni。3. A solution treatment method for laser powder bed fusion GH3230 alloy according to claim 1 or 2, characterized in that the composition of the GH3230 spherical powder used in step 1 to prepare the GH3230 alloy satisfies by mass percentage: C: 0.07%, Si: 0.35%, Mn: 0.5%, Cr: 21.74%, Fe: 1.9%, Mo: 2.8%, Co: 2.1%, W: 14.7%, Al: 0.45%, Ti: 0.1%, Cu: 0.01%, La: 0.01%, B: 0.001%, and the balance is Ni. 4.根据权利要求3所述一种激光粉末床熔融GH3230合金的固溶处理方法,其特征在于,步骤一制备GH3230合金使用的GH3230球形粉末的粒径尺寸为15~53μm。4. A solution treatment method for laser powder bed fusion GH3230 alloy according to claim 3, characterized in that the particle size of the GH3230 spherical powder used in the step 1 for preparing the GH3230 alloy is 15-53 μm. 5.根据权利要求4所述一种激光粉末床熔融GH3230合金的固溶处理方法,其特征在于,步骤一所述惰性气氛为氩气气氛,所述氩气气氛的含氧量低于100ppm。5 . A solution treatment method for laser powder bed fusion GH3230 alloy according to claim 4 , wherein the inert atmosphere in step 1 is an argon atmosphere, and the oxygen content of the argon atmosphere is lower than 100 ppm. 6.根据权利要求5所述一种激光粉末床熔融GH3230合金的固溶处理方法,其特征在于,步骤一所述激光粉末床熔融增材制造系统中光源为YAG固体激光,激光功率为120~300W,光斑直径为0.087mm,激光扫描速率为500~1300mm/s,铺粉厚度为0.02~0.05mm,扫描间距为0.05~0.12mm,扫描策略为67°交叉条带状扫描,基板预热温度为80~160℃。6. A solid solution treatment method for laser powder bed fusion GH3230 alloy according to claim 5, characterized in that the light source in the laser powder bed fusion additive manufacturing system described in step 1 is a YAG solid-state laser, and the laser power is 120- 300W, the spot diameter is 0.087mm, the laser scanning rate is 500-1300mm/s, the powder coating thickness is 0.02-0.05mm, the scanning distance is 0.05-0.12mm, the scanning strategy is 67° cross-strip scanning, the substrate preheating temperature It is 80-160°C. 7.根据权利要求6所述一种激光粉末床熔融GH3230合金的固溶处理方法,其特征在于,步骤二所述GH3230合金升温是从室温以8~10℃/min的速度升温到1130℃~1280℃。7. A solution treatment method for laser powder bed fusion GH3230 alloy according to claim 6, characterized in that, the temperature rise of the GH3230 alloy in step 2 is from room temperature to 1130° C. 1280°C. 8.根据权利要求7所述一种激光粉末床熔融GH3230合金的固溶处理方法,其特征在于,步骤二所述冷却至室温是采用高压氩气快速冷却。8. A solution treatment method for laser powder bed fusion GH3230 alloy according to claim 7, characterized in that the cooling to room temperature in step 2 is rapid cooling with high-pressure argon. 9.一种如权利要求1-8任一所述的激光粉末床熔融GH3230合金的固溶处理方法处理得到的GH3230合金,其特征在于,处理所得GH3230合金的基体为全奥氏体组织,晶粒尺寸控制在40~80μm范围内。9. A GH3230 alloy obtained by the solution treatment method of the laser powder bed fusion GH3230 alloy as claimed in any one of claims 1-8, characterized in that, the substrate of the processed GH3230 alloy is a full austenite structure, and the grain The particle size is controlled within the range of 40-80 μm. 10.根据权利要求9所述激光粉末床熔融GH3230合金的固溶处理方法处理得到的GH3230合金,其特征在于,析出碳化物为M6C,M6C在GH3230合金中的体积分数小于10%,原晶界位置M6C平均尺寸小于2μm,晶内M6C平均尺寸小于0.3μm。10. According to the GH3230 alloy obtained by the solution treatment method of laser powder bed fusion GH3230 alloy according to claim 9, it is characterized in that the precipitated carbide is M 6 C, and the volume fraction of M 6 C in the GH3230 alloy is less than 10%. , the average size of M 6 C at the original grain boundary position is less than 2 μm, and the average size of M 6 C in the grain is less than 0.3 μm.
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