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CN111809126A - A method for eliminating AM microstructure in FeCrNiMn quaternary high-entropy alloys - Google Patents

A method for eliminating AM microstructure in FeCrNiMn quaternary high-entropy alloys Download PDF

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CN111809126A
CN111809126A CN202010515558.9A CN202010515558A CN111809126A CN 111809126 A CN111809126 A CN 111809126A CN 202010515558 A CN202010515558 A CN 202010515558A CN 111809126 A CN111809126 A CN 111809126A
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entropy alloy
fecrnimn
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陈逸
张帅今
程亮
邢晨
朱彬
卢雅琳
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Jiangsu University of Technology
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    • C22METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
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Abstract

本发明公开一种消除FeCrNiMn四元高熵合金中调幅组织的方法。包括:(1)高熵合金热处理式样的制作:将FeCrNiMn四元高熵合金切割成热处理式样;(2)高熵合金热处理式样的热处理:将高熵合金热处理式样升温煅烧,并保温;(3)高熵合金热处理式样的冷却处理:将保温后的高熵合金热处理式样冷却;(4)高熵合金热处理式样的后处理:将冷却处理后的高熵合金热处理式样研磨,抛光。本发明的方法简单、成本低;本发明通过热处理将FeCrNiMn四元高熵合金中的FeCr相溶解,消除FeCr相给高熵合金带来的硬脆等影响,改善了高熵合金的韧性及抗冲击性,从而提高了高熵合金的力学性能,有利于高熵合金的二次加工及使用。

Figure 202010515558

The invention discloses a method for eliminating the amplitude modulation structure in FeCrNiMn quaternary high-entropy alloy. Including: (1) production of high-entropy alloy heat treatment pattern: cutting FeCrNiMn quaternary high-entropy alloy into heat-treatment patterns; (2) heat treatment of high-entropy alloy heat-treatment pattern: heating and calcining the high-entropy alloy heat-treatment pattern, and keeping the temperature; (3) ) Cooling treatment of the heat-treated high-entropy alloy pattern: cooling the heat-treated high-entropy alloy pattern after heat preservation; (4) Post-treatment of the heat-treated high-entropy alloy pattern: grinding and polishing the heat-treated high-entropy alloy pattern after cooling. The method of the invention is simple and low in cost; the invention dissolves the FeCr phase in the FeCrNiMn quaternary high-entropy alloy through heat treatment, eliminates the hard and brittle effects of the FeCr phase on the high-entropy alloy, and improves the toughness and resistance of the high-entropy alloy. impact, thereby improving the mechanical properties of the high-entropy alloy, which is beneficial to the secondary processing and use of the high-entropy alloy.

Figure 202010515558

Description

一种消除FeCrNiMn四元高熵合金中调幅组织的方法A method for eliminating AM microstructure in FeCrNiMn quaternary high-entropy alloys

技术领域technical field

本发明涉及金属材料热处理领域,具体涉及一种消除FeCrNiMn四元高熵合金中调幅组织的方法。The invention relates to the field of heat treatment of metal materials, in particular to a method for eliminating amplitude modulation structures in FeCrNiMn quaternary high-entropy alloys.

背景技术Background technique

相比于传统合金中一种元素为主要成分,加入少量其他元素的设计理念不同,高熵合金则采用了一种新型的设计理念,将多种(通常为5中或5种以上,最近研究人员将4种元素的合金也定义为高熵合金)主元等原子比混合。由于高熵合金中的四大效应,因此形成了固溶体结构的高熵合金。由于其优异的性能,在高温部件,高速切削用刀具,抗辐射用等运用广泛。Compared with traditional alloys in which one element is the main component and a small amount of other elements are added, the design concept of high-entropy alloys adopts a new design concept. The alloys of 4 elements are also defined as high-entropy alloys) mixtures of principal elements in equal atomic ratios. Due to the four major effects in high-entropy alloys, high-entropy alloys with solid solution structure are formed. Due to its excellent performance, it is widely used in high-temperature parts, high-speed cutting tools, and radiation resistance.

然而作为一种新型合金,其存在很多值得探索的问题。由于高熵合金中的“迟滞扩散”效应,因此易形成纳米结构的调幅组织。在含有Fe和Cr元素的高熵合金中,Fe-Cr的混合焓为-1KJ/mol,因此,及其容易成形FeCr相与基体BCC相混合而成的调幅组织。大量研究发现,这种调幅组织的力学性能主要表现为硬、脆,这种硬脆的力学性能对高熵合金之后的二次加工存在极大的约束,并且对其使用带来了巨大的困难。并且目前没有研究人员提出一种高效的消除高熵合金中调幅组织的方法。However, as a new type of alloy, there are many problems worth exploring. Due to the "retarded diffusion" effect in high-entropy alloys, it is easy to form nanostructured amplitude-modulated structures. In the high-entropy alloys containing Fe and Cr elements, the mixing enthalpy of Fe-Cr is -1KJ/mol, so it is easy to form an amplitude-modulated structure formed by mixing FeCr phase and matrix BCC phase. A large number of studies have found that the mechanical properties of this amplitude-modulated structure are mainly hard and brittle. The hard and brittle mechanical properties have great constraints on the secondary processing of high-entropy alloys, and bring great difficulties to their use. . And no researchers have proposed an efficient method to eliminate the AM structure in HEA.

针对这一问题,本发明提出了一种消除FeCrNiMn四元高熵合金中调幅组织的方法,从而极大地改善了高熵合金的力学性能,有利于高熵合金的二次加工及使用。Aiming at this problem, the present invention proposes a method for eliminating the amplitude modulated structure in FeCrNiMn quaternary high-entropy alloys, thereby greatly improving the mechanical properties of the high-entropy alloys and facilitating the secondary processing and use of the high-entropy alloys.

发明内容SUMMARY OF THE INVENTION

本发明的目的在于提供一种简单、有效的消除FeCrNiMn四元高熵合金中调幅组织的方法,大幅改善了高熵合金的力学性能,有利于高熵合金的二次加工及使用。The purpose of the present invention is to provide a simple and effective method for eliminating the amplitude modulation structure in FeCrNiMn quaternary high-entropy alloys, which greatly improves the mechanical properties of the high-entropy alloys and is beneficial to the secondary processing and use of the high-entropy alloys.

本发明是通过如下技术方案实现的:The present invention is achieved through the following technical solutions:

一种消除FeCrNiMn四元高熵合金中调幅组织的方法,其特征在于,该方法包括如下步骤:A method for eliminating amplitude modulation structure in FeCrNiMn quaternary high-entropy alloy, characterized in that the method comprises the following steps:

(1)高熵合金热处理式样的制作:将FeCrNiMn四元高熵合金切割成热处理式样;(1) Production of high-entropy alloy heat treatment patterns: cutting FeCrNiMn quaternary high-entropy alloys into heat-treatment patterns;

(2)高熵合金热处理式样的热处理:将高熵合金热处理式样升温煅烧,升温完成后进行保温处理;(2) Heat treatment of the high-entropy alloy heat treatment sample: the high-entropy alloy heat treatment sample is heated and calcined, and the heat preservation treatment is performed after the heating is completed;

(3)高熵合金热处理式样的冷却处理:将保温处理后的高熵合金热处理式样立刻采取冷却处理;(3) Cooling treatment of the high-entropy alloy heat treatment pattern: immediately take the cooling treatment of the high-entropy alloy heat treatment pattern after the heat preservation treatment;

(4)高熵合金热处理式样的后处理:将冷却处理后的高熵合金热处理式样先进行研磨,然后再进行抛光处理。(4) Post-treatment of the high-entropy alloy heat-treatment pattern: the cooling-treated high-entropy alloy heat-treatment pattern is first ground, and then polished.

进一步,步骤(1)中所述高熵合金热处理式样的制作:采用线切割机将FeCrNiMn四元高熵合金切割成尺寸为10mm×10mm×10mm的热处理式样。Further, the preparation of the high-entropy alloy heat treatment pattern in step (1): the FeCrNiMn quaternary high-entropy alloy is cut into a heat-treatment pattern with a size of 10mm×10mm×10mm by using a wire cutting machine.

进一步,步骤(2)中所述高熵合金热处理式样的热处理:将FeCrNiMn四元高熵合金热处理式样放入马弗炉中升温煅烧,控制升温速率为10-20℃/min、升温至900-1200℃,升温完成后进行0.5-24小时的保温处理。将FeCrNiMn四元高熵合金升温至FeCr相溶解温度之上,随后对其进行保温处理,保温处理后立即对高熵合金进行冷却处理,避免了高熵合金中调幅组织的生成,消除FeCr相给高熵合金带来的硬、脆力学性能的影响。Further, the heat treatment of the high-entropy alloy heat treatment pattern described in the step (2): the FeCrNiMn quaternary high-entropy alloy heat treatment pattern is put into a muffle furnace for heating and calcination, and the temperature rise rate is controlled to be 10-20 ℃/min, and be heated to 900- 1200 ° C, after the temperature rise is completed, heat preservation treatment is performed for 0.5-24 hours. The FeCrNiMn quaternary high-entropy alloy is heated to above the dissolution temperature of FeCr phase, and then subjected to heat preservation treatment. Immediately after the heat preservation treatment, the high-entropy alloy is cooled to avoid the formation of amplitude-modulated structure in the high-entropy alloy and eliminate the FeCr phase contribution. The effect of hard and brittle mechanical properties brought by high-entropy alloys.

进一步,步骤(3)中所述高熵合金热处理式样的冷却处理:将保温处理后的FeCrNiMn四元高熵合金热处理式样立即进行空气冷却处理或淬火处理。Further, the cooling treatment of the high-entropy alloy heat treatment pattern described in the step (3): the FeCrNiMn quaternary high-entropy alloy heat-treatment pattern after the heat preservation treatment is immediately subjected to air cooling treatment or quenching treatment.

进一步,所述淬火处理过程中所使用的溶液为水、盐水或机油中任一种。Further, the solution used in the quenching process is any one of water, brine or engine oil.

进一步,步骤(4)中所述高熵合金热处理式样的后处理:采用二氧化硅砂纸对冷却处理后的FeCrNiMn四元高熵合金热处理式样进行研磨,将研磨后的FeCrNiMn四元高熵合金热处理式样再用抛光膏在抛光机上进行手动抛光。通过二氧化硅砂纸将高熵合金热处理后的式样研磨至7000#为止,将研磨后的高熵合金热处理式样用抛光膏在抛光机上进行手动抛光,抛光至高熵合金热处理式样的表面没有二氧化硅砂纸研磨的划痕为止。Further, the post-processing of the high-entropy alloy heat treatment pattern described in step (4): the FeCrNiMn quaternary high-entropy alloy heat-treatment pattern after the cooling treatment is ground with silica sandpaper, and the ground FeCrNiMn quaternary high-entropy alloy heat-treatment pattern is ground. The pattern is then hand polished on a polishing machine with polishing paste. Grind the high-entropy alloy heat-treated pattern to 7000# with silica sandpaper, and manually polish the ground high-entropy alloy heat-treated pattern with polishing paste on a polishing machine until the surface of the high-entropy alloy heat-treated pattern has no silica sand. The paper grinds to scratches.

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

(1)本发明方法的工艺简单、高效、成本低,可以运用于实际的生产过程中,提升企业的生产效益,并且节约成本和能源;此外由于在高熵合金中没有研究者提出有效、合理的消除调幅组织的方法,因此本发明还可以供给科研人员借鉴;(1) The process of the method of the present invention is simple, efficient and low in cost, and can be used in the actual production process to improve the production efficiency of enterprises, and save costs and energy; in addition, because no researcher proposes effective and reasonable high-entropy alloys in high-entropy alloys. Therefore, the present invention can also be used for reference by scientific researchers;

(2)本发明仅用热处理的手段即可将FeCrNiMn四元高熵合金中的调幅组织消除(调幅组织为细小、硬脆的FeCr相与基体BCC相混合而成),消除调幅组织(即将FeCr相溶解)给高熵合金带来的硬、脆力学性能的影响,改善了高熵合金的韧性及抗冲击性,从而提高了高熵合金的力学性能,有利于高熵合金的二次加工及使用。(2) The present invention can eliminate the AM structure in the FeCrNiMn quaternary high-entropy alloy (the AM structure is a mixture of fine, hard and brittle FeCr phase and the matrix BCC phase) in the FeCrNiMn quaternary high-entropy alloy, and eliminate the AM structure (that is, FeCr). The effect of phase dissolution) on the hard and brittle mechanical properties of high-entropy alloys improves the toughness and impact resistance of high-entropy alloys, thereby improving the mechanical properties of high-entropy alloys, which is beneficial to the secondary processing of high-entropy alloys. use.

附图说明Description of drawings

为了更清楚地说明本发明实施例的技术方案,下面将对实施例描述中所需要使用的附图作简单地介绍,显而易见地,下面描述中的附图仅仅是本发明的一些实施例,对于本领域的普通技术人员来讲,在不付出创造性劳动的前提下,还可以根据这些附图获得其他附图。In order to illustrate the technical solutions of the embodiments of the present invention more clearly, the following briefly introduces the accompanying drawings used in the description of the embodiments. Obviously, the drawings in the following description are only some embodiments of the present invention. For those of ordinary skill in the art, other drawings can also be obtained from these drawings without any creative effort.

图1为锻态式样下FeCrNiMn四元高熵合金的显微组织图;Fig. 1 is the microstructure diagram of FeCrNiMn quaternary high-entropy alloy under the forging style;

图2为本发明中实施例1的FeCrNiMn四元高熵合金经过热处理后的显微组织图;2 is a microstructure diagram of the FeCrNiMn quaternary high-entropy alloy of Example 1 of the present invention after heat treatment;

图3为本发明中实施例2的FeCrNiMn四元高熵合金经过热处理后的显微组织图;3 is a microstructure diagram of the FeCrNiMn quaternary high-entropy alloy of Example 2 of the present invention after heat treatment;

图4为本发明中实施例3的FeCrNiMn四元高熵合金经过热处理后的显微组织图。4 is a microstructure diagram of the FeCrNiMn quaternary high-entropy alloy of Example 3 of the present invention after heat treatment.

具体实施方式Detailed ways

下面将结合本发明实施例中的附图,对本发明实施例中的技术方案进行清楚、完整地描述,显然,所描述的实施例仅仅是本发明一部分实施例,而不是全部的实施例。以下对至少一个示例性实施例的描述实际上仅仅是说明性的,决不作为对本发明及其应用或使用的任何限制。基于本发明中的实施例,本领域普通技术人员在没有作出创造性劳动前提下所获得的所有其他实施例,都属于本发明保护的范围。The technical solutions in the embodiments of the present invention will be clearly and completely described below with reference to the accompanying drawings in the embodiments of the present invention. Obviously, the described embodiments are only a part of the embodiments of the present invention, but not all of the embodiments. The following description of at least one exemplary embodiment is merely illustrative in nature and is in no way intended to limit the invention, its application, or uses. Based on the embodiments of the present invention, all other embodiments obtained by those of ordinary skill in the art without creative efforts shall fall within the protection scope of the present invention.

实施例1Example 1

本实施例1中所述的FeCrNiMn四元高熵合金为等原子比的FeCrNiMn高熵合金。The FeCrNiMn quaternary high-entropy alloy described in this Example 1 is a FeCrNiMn high-entropy alloy with an equal atomic ratio.

(1)FeCrNiMn四元高熵合金热处理式样的制作:将FeCrNiMn四元高熵合金用线切割机切割成两块尺寸为10mm×10mm×10mm的热处理式样;(1) Production of heat treatment pattern of FeCrNiMn quaternary high-entropy alloy: cut FeCrNiMn quaternary high-entropy alloy into two heat-treatment patterns with a size of 10mm×10mm×10mm by a wire cutting machine;

(2)FeCrNiMn四元高熵合金热处理式样的热处理:取其中一块切割后的FeCrNiMn四元高熵合金热处理式样放置于马弗炉中升温煅烧,并控制马弗炉的升温速率为10℃/min,升温至900℃,升温完成后继续保温处理0.5小时;(2) Heat treatment of FeCrNiMn quaternary high-entropy alloy heat treatment pattern: take one of the cut FeCrNiMn quaternary high-entropy alloy heat treatment patterns and place it in a muffle furnace for heating and calcination, and control the heating rate of the muffle furnace to 10 °C/min , heat up to 900°C, and continue the heat preservation treatment for 0.5 hours after the temperature rise is completed;

(3)FeCrNiMn四元高熵合金热处理式样的冷却处理:将保温处理完成后的FeCrNiMn四元高熵合金热处理式样立即进行空气冷却处理(将FeCrNiMn四元高熵合金热处理式样冷却至室温即可)。(3) Cooling treatment of FeCrNiMn quaternary high-entropy alloy heat treatment pattern: air cooling the FeCrNiMn quaternary high-entropy alloy heat-treatment pattern after the heat preservation treatment is completed (the FeCrNiMn quaternary high-entropy alloy heat-treatment pattern can be cooled to room temperature) .

(4)FeCrNiMn四元高熵合金热处理式样的后处理:将冷却处理后的FeCrNiMn四元高熵合金热处理式样用二氧化硅砂纸对其进行研磨,将FeCrNiMn四元高熵合金热处理式样研磨至7000#为止,然后将研磨后的FeCrNiMn四元高熵合金热处理式样再用抛光膏在抛光机上进行手动抛光处理,抛光至FeCrNiMn四元高熵合金热处理式样的表面没有二氧化硅砂纸研磨的划痕为止;(4) Post-treatment of the FeCrNiMn quaternary high-entropy alloy heat treatment pattern: grind the FeCrNiMn quaternary high-entropy alloy heat-treatment pattern after cooling treatment with silica sandpaper, and grind the FeCrNiMn quaternary high-entropy alloy heat-treatment pattern to 7000 #, and then the ground FeCrNiMn quaternary high-entropy alloy heat-treated sample was manually polished with polishing paste on a polishing machine until the surface of the FeCrNiMn quaternary high-entropy alloy heat-treated sample had no scratches from silica sandpaper grinding. ;

(5)取上述步骤(1)中的另一块FeCrNiMn四元四元高熵合金热处理式样用二氧化硅砂纸对其进行研磨,将FeCrNiMn四元高熵合金热处理式样研磨至7000#为止,然后将研磨后的FeCrNiMn四元高熵合金热处理式样用抛光膏在抛光机上进行手动抛光处理,抛光至FeCrNiMn四元高熵合金热处理式样的表面没有二氧化硅砂纸研磨的划痕为止。(5) Take another FeCrNiMn quaternary high-entropy alloy heat treatment pattern in the above step (1) and grind it with silica sandpaper, and grind the FeCrNiMn quaternary high-entropy alloy heat treatment pattern to 7000#, then the The ground FeCrNiMn quaternary high-entropy alloy heat-treated sample was manually polished with a polishing paste on a polishing machine until the surface of the FeCrNiMn quaternary high-entropy alloy heat-treated sample had no scratches ground by silica sandpaper.

测试与分析:分别取上述步骤(5)中的FeCrNiMn四元高熵合金热处理式样(经过研磨和抛光处理但未经过热处理和冷却处理)和上述步骤(4)中经过热处理及空气冷却处理后的FeCrNiMn四元高熵合金热处理式样,然后通过扫描电镜(SEM)分别进行观察:得到如图1所示的未经过热处理(锻态)的FeCrNiMn四元高熵合金热处理式样的显微组织图和如图2所示的经过900℃热处理、保温0.5小时及空气冷却处理后的FeCrNiMn四元高熵合金热处理式样的显微组织图,从图1中可以看出锻态式样下(即未经过热处理的FeCrNiMn四元高熵合金热处理式样)FeCrNiMn四元高熵合金中存在大量的调幅组织(即FeCrNiMn四元高熵合金中细小、硬脆的FeCr相与基体BCC相构成的组织),从图2中可以看出经过本实施例1的热处理及空气冷却处理后的FeCrNiMn四元高熵合金中没有发现调幅组织的存在,证实了本发明方案的有效性及可靠性。Test and analysis: respectively take the FeCrNiMn quaternary high-entropy alloy heat treatment pattern in the above step (5) (after grinding and polishing but not heat treatment and cooling treatment) and the heat treatment and air cooling treatment in the above step (4) respectively. The heat treatment pattern of FeCrNiMn quaternary high-entropy alloy was then observed by scanning electron microscope (SEM): the microstructure of the heat-treated pattern of FeCrNiMn quaternary high-entropy alloy without heat treatment (forging state) as shown in Figure 1 and as shown in Figure 1 were obtained. Figure 2 shows the microstructure of the FeCrNiMn quaternary high-entropy alloy heat treatment style after heat treatment at 900 °C, heat preservation for 0.5 hours and air cooling treatment. FeCrNiMn quaternary high-entropy alloy heat treatment pattern) FeCrNiMn quaternary high-entropy alloy has a large number of amplitude-modulated structures (that is, the structure composed of fine, hard and brittle FeCr phase and matrix BCC phase in FeCrNiMn quaternary high-entropy alloy), from Figure 2 It can be seen that there is no AM structure in the FeCrNiMn quaternary high-entropy alloy after the heat treatment and air cooling treatment in Example 1, which confirms the effectiveness and reliability of the solution of the present invention.

实施例2Example 2

本实施例中2所述的FeCrNiMn四元高熵合金为等原子比的FeCrNiMn高熵合金。The FeCrNiMn quaternary high-entropy alloy described in 2 in this embodiment is a FeCrNiMn high-entropy alloy with an equal atomic ratio.

(1)FeCrNiMn四元高熵合金热处理式样的制作:将FeCrNiMn四元高熵合金用线切割机切割成两块尺寸为10mm×10mm×10mm的热处理式样;(1) Production of heat treatment pattern of FeCrNiMn quaternary high-entropy alloy: cut FeCrNiMn quaternary high-entropy alloy into two heat-treatment patterns with a size of 10mm×10mm×10mm by a wire cutting machine;

(2)FeCrNiMn四元高熵合金热处理式样的热处理:取其中一块切割后的FeCrNiMn四元高熵合金热处理式样放置于马弗炉中升温煅烧,并控制马弗炉的升温速率为20℃/min,升温至1100℃,升温完成后继续保温处理24小时;(2) Heat treatment of FeCrNiMn quaternary high-entropy alloy heat treatment pattern: take one of the cut FeCrNiMn quaternary high-entropy alloy heat treatment patterns and place it in a muffle furnace for heating and calcination, and control the heating rate of the muffle furnace to 20 °C/min , heat up to 1100°C, and continue to keep heat for 24 hours after the temperature rise is completed;

(3)FeCrNiMn四元高熵合金热处理式样的冷却处理:将保温处理完成后的FeCrNiMn四元高熵合金热处理式样立即进行淬火处理(淬火所使用的溶液为盐水)。(3) Cooling treatment of the FeCrNiMn quaternary high-entropy alloy heat treatment pattern: The FeCrNiMn quaternary high-entropy alloy heat-treatment pattern after the heat preservation treatment was completed immediately quenched (the solution used for quenching was brine).

(4)FeCrNiMn四元高熵合金热处理式样的后处理:将冷却处理后的FeCrNiMn四元高熵合金热处理式样用二氧化硅砂纸对其进行研磨,将FeCrNiMn四元高熵合金热处理式样研磨至7000#为止,然后将研磨后的FeCrNiMn四元高熵合金热处理式样再用抛光膏在抛光机上进行手动抛光处理,抛光至FeCrNiMn四元高熵合金热处理式样的表面没有二氧化硅砂纸研磨的划痕为止;(4) Post-treatment of the FeCrNiMn quaternary high-entropy alloy heat treatment pattern: grind the FeCrNiMn quaternary high-entropy alloy heat-treatment pattern after cooling treatment with silica sandpaper, and grind the FeCrNiMn quaternary high-entropy alloy heat-treatment pattern to 7000 #, and then the ground FeCrNiMn quaternary high-entropy alloy heat-treated sample was manually polished with polishing paste on a polishing machine until the surface of the FeCrNiMn quaternary high-entropy alloy heat-treated sample had no scratches from silica sandpaper grinding. ;

(5)取上述步骤(1)中的另一块FeCrNiMn四元四元高熵合金热处理式样用二氧化硅砂纸对其进行研磨,将FeCrNiMn四元高熵合金热处理式样研磨至7000#为止,然后将研磨后的FeCrNiMn四元高熵合金热处理式样用抛光膏在抛光机上进行手动抛光处理,抛光至FeCrNiMn四元高熵合金热处理式样的表面没有二氧化硅砂纸研磨的划痕为止。(5) Take another FeCrNiMn quaternary high-entropy alloy heat treatment pattern in the above step (1) and grind it with silica sandpaper, and grind the FeCrNiMn quaternary high-entropy alloy heat treatment pattern to 7000#, then the The ground FeCrNiMn quaternary high-entropy alloy heat-treated sample was manually polished with a polishing paste on a polishing machine until the surface of the FeCrNiMn quaternary high-entropy alloy heat-treated sample had no scratches ground by silica sandpaper.

测试与分析:分别取上述步骤(5)中的FeCrNiMn四元高熵合金热处理式样(经过研磨和抛光处理但未经过热处理和冷却处理)和上述步骤(4)中经过热处理及淬火处理(淬火用溶液为盐水)过后的FeCrNiMn四元高熵合金热处理式样,然后通过扫描电镜(SEM)分别进行观察:得到如图1所示的未经过热处理(锻态)的FeCrNiMn四元高熵合金锻态式样的显微组织图和如图3所示的经过1100℃热处理、保温24小时及淬火处理后的FeCrNiMn四元高熵合金热处理式样的显微组织图,从图1中可以看出锻态式样下(未经过热处理)FeCrNiMn四元高熵合金中存在大量的调幅组织(细小、硬脆的FeCr相与基体BCC相构成的组织),从图3中可以看出经过本实施例2的热处理及淬火处理后的FeCrNiMn四元高熵合金中没有发现调幅组织的存在,证实了本发明方案的有效性及可靠性。Test and analysis: Take the FeCrNiMn quaternary high-entropy alloy heat treatment pattern in the above step (5) (after grinding and polishing but not heat treatment and cooling treatment) and the heat treatment and quenching treatment in the above step (4) (for quenching), respectively. The heat treatment pattern of FeCrNiMn quaternary high-entropy alloy after the solution is brine), and then observed by scanning electron microscope (SEM) respectively: the forged pattern of FeCrNiMn quaternary high-entropy alloy without heat treatment (forging state) is obtained as shown in Figure 1 The microstructure of the FeCrNiMn quaternary high-entropy alloy after heat treatment at 1100 °C, holding for 24 hours and quenching as shown in Figure 3. It can be seen from Figure 1 that under the forging style (without heat treatment) FeCrNiMn quaternary high-entropy alloy has a large amount of amplitude modulation structure (structure composed of fine, hard and brittle FeCr phase and matrix BCC phase), it can be seen from Figure 3 that after heat treatment and quenching in Example 2 The existence of amplitude modulation structure is not found in the treated FeCrNiMn quaternary high-entropy alloy, which confirms the validity and reliability of the solution of the present invention.

实施例3Example 3

本实施例中3所述的FeCrNiMn四元高熵合金为等原子比的FeCrNiMn高熵合金。The FeCrNiMn quaternary high-entropy alloy described in 3 in this embodiment is a FeCrNiMn high-entropy alloy with an equal atomic ratio.

(1)FeCrNiMn四元高熵合金热处理式样的制作:将FeCrNiMn四元高熵合金用线切割机切割成两块尺寸为10mm×10mm×10mm的热处理式样;(1) Production of heat treatment pattern of FeCrNiMn quaternary high-entropy alloy: cut FeCrNiMn quaternary high-entropy alloy into two heat-treatment patterns with a size of 10mm×10mm×10mm by a wire cutting machine;

(2)FeCrNiMn四元高熵合金热处理式样的热处理:取其中一块切割后的FeCrNiMn四元高熵合金热处理式样放置于马弗炉中升温煅烧,并控制马弗炉的升温速率为15℃/min,升温至1200℃,升温完成后继续保温处理12小时;(2) Heat treatment of FeCrNiMn quaternary high-entropy alloy heat treatment pattern: take one of the cut FeCrNiMn quaternary high-entropy alloy heat treatment patterns and place it in a muffle furnace for heating and calcination, and control the heating rate of the muffle furnace to be 15℃/min , heat up to 1200 ° C, and continue to keep heat for 12 hours after the temperature rise is completed;

(3)FeCrNiMn四元高熵合金热处理式样的冷却处理:将保温处理完成后的FeCrNiMn四元高熵合金热处理式样立即进行淬火处理(淬火所使用的溶液为机油)。(3) Cooling treatment of the FeCrNiMn quaternary high-entropy alloy heat treatment pattern: The FeCrNiMn quaternary high-entropy alloy heat-treatment pattern after the heat preservation treatment was completed immediately quenched (the solution used for quenching was engine oil).

(4)FeCrNiMn四元高熵合金热处理式样的后处理:将冷却处理后的FeCrNiMn四元高熵合金热处理式样用二氧化硅砂纸对其进行研磨,将FeCrNiMn四元高熵合金热处理式样研磨至7000#为止,然后将研磨后的FeCrNiMn四元高熵合金热处理式样再用抛光膏在抛光机上进行手动抛光处理,抛光至FeCrNiMn四元高熵合金热处理式样的表面没有二氧化硅砂纸研磨的划痕为止;(4) Post-treatment of the FeCrNiMn quaternary high-entropy alloy heat treatment pattern: grind the FeCrNiMn quaternary high-entropy alloy heat-treatment pattern after cooling treatment with silica sandpaper, and grind the FeCrNiMn quaternary high-entropy alloy heat-treatment pattern to 7000 #, and then the ground FeCrNiMn quaternary high-entropy alloy heat-treated sample was manually polished with polishing paste on a polishing machine until the surface of the FeCrNiMn quaternary high-entropy alloy heat-treated sample had no scratches from silica sandpaper grinding. ;

(5)取上述步骤(1)中的另一块FeCrNiMn四元四元高熵合金热处理式样用二氧化硅砂纸对其进行研磨,将FeCrNiMn四元高熵合金热处理式样研磨至7000#为止,然后将研磨后的FeCrNiMn四元高熵合金热处理式样用抛光膏在抛光机上进行手动抛光处理,抛光至FeCrNiMn四元高熵合金热处理式样的表面没有二氧化硅砂纸研磨的划痕为止。(5) Take another FeCrNiMn quaternary high-entropy alloy heat treatment pattern in the above step (1) and grind it with silica sandpaper, and grind the FeCrNiMn quaternary high-entropy alloy heat treatment pattern to 7000#, then the The ground FeCrNiMn quaternary high-entropy alloy heat-treated sample was manually polished with a polishing paste on a polishing machine until the surface of the FeCrNiMn quaternary high-entropy alloy heat-treated sample had no scratches ground by silica sandpaper.

测试与分析:分别取上述步骤(5)中的FeCrNiMn四元高熵合金热处理式样(经过研磨和抛光处理但未经过热处理和冷却处理)和上述步骤(4)中经过热处理及淬火处理(淬火用溶液为机油)过后的FeCrNiMn四元高熵合金热处理式样,然后通过扫描电镜(SEM)分别进行观察:得到如图1所示的未经过热处理(锻态)的FeCrNiMn四元高熵合金锻态式样的显微组织图和如图4所示的经过1200℃热处理、保温12小时及淬火处理后的FeCrNiMn四元高熵合金热处理式样的显微组织图,从图1中可以看出锻态式样下(未经过热处理)FeCrNiMn四元高熵合金中存在大量的调幅组织(细小、硬脆的FeCr相与基体BCC相构成的组织),从图4中可以看出经过本实施例3的热处理及淬火处理后的FeCrNiMn四元高熵合金中没有发现调幅组织的存在,证实了本发明方案的有效性及可靠性。Test and analysis: Take the FeCrNiMn quaternary high-entropy alloy heat treatment pattern in the above step (5) (after grinding and polishing but not heat treatment and cooling treatment) and the heat treatment and quenching treatment in the above step (4) (for quenching), respectively. The heat treatment pattern of FeCrNiMn quaternary high-entropy alloy after the solution is engine oil), and then observed by scanning electron microscope (SEM) respectively: the forged pattern of FeCrNiMn quaternary high-entropy alloy without heat treatment (forging) is obtained as shown in Figure 1. The microstructure of the FeCrNiMn quaternary high-entropy alloy after heat treatment at 1200 °C, holding for 12 hours and quenching as shown in Figure 4. It can be seen from Figure 1 that under the forging style (without heat treatment) FeCrNiMn quaternary high-entropy alloy has a large amount of amplitude modulation structure (structure composed of fine, hard and brittle FeCr phase and matrix BCC phase), it can be seen from Figure 4 that after the heat treatment and quenching of Example 3 The existence of amplitude modulation structure is not found in the treated FeCrNiMn quaternary high-entropy alloy, which confirms the validity and reliability of the solution of the present invention.

上述为本发明的较佳实施例仅用于解释本发明,并不用于限定本发明。凡由本发明的技术方案所引伸出的显而易见的变化或变动仍处于本发明的保护范围之中。The above-mentioned preferred embodiments of the present invention are only used to explain the present invention, and are not intended to limit the present invention. Any obvious changes or changes derived from the technical solutions of the present invention are still within the protection scope of the present invention.

Claims (6)

1.一种消除FeCrNiMn四元高熵合金中调幅组织的方法,其特征在于,该方法包括如下步骤:1. a method for eliminating amplitude modulation structure in FeCrNiMn quaternary high-entropy alloy, is characterized in that, this method comprises the steps: (1)高熵合金热处理式样的制作:将FeCrNiMn四元高熵合金切割成热处理式样;(1) Production of high-entropy alloy heat treatment patterns: cutting FeCrNiMn quaternary high-entropy alloys into heat-treatment patterns; (2)高熵合金热处理式样的热处理:将高熵合金热处理式样升温煅烧,升温完成后进行保温处理;(2) Heat treatment of the high-entropy alloy heat treatment sample: the high-entropy alloy heat treatment sample is heated and calcined, and the heat preservation treatment is performed after the heating is completed; (3)高熵合金热处理式样的冷却处理:将保温处理后的高熵合金热处理式样立刻采取冷却处理;(3) Cooling treatment of the high-entropy alloy heat treatment pattern: immediately take the cooling treatment of the high-entropy alloy heat treatment pattern after the heat preservation treatment; (4)高熵合金热处理式样的后处理:将冷却处理后的高熵合金热处理式样先进行研磨,然后再进行抛光处理。(4) Post-treatment of the high-entropy alloy heat-treatment pattern: the cooling-treated high-entropy alloy heat-treatment pattern is first ground, and then polished. 2.根据权利要求1所述的一种消除FeCrNiMn四元高熵合金中调幅组织的方法,其特征在于,步骤(1)中所述高熵合金热处理式样的制作:采用线切割机将FeCrNiMn四元高熵合金切割成尺寸为10mm×10mm×10mm的热处理式样。2. a kind of method that eliminates AM structure in FeCrNiMn quaternary high-entropy alloy according to claim 1, it is characterized in that, the making of high-entropy alloy heat treatment pattern described in step (1): adopt wire cutting machine to make FeCrNiMn four. The high-entropy alloy was cut into a heat-treated pattern with a size of 10mm×10mm×10mm. 3.根据权利要求1所述的一种消除FeCrNiMn四元高熵合金中调幅组织的方法,其特征在于,步骤(2)中所述高熵合金热处理式样的热处理:将FeCrNiMn四元高熵合金热处理式样放入马弗炉中升温煅烧,控制升温速率为10-20℃/min、升温至900-1200℃,升温完成后进行0.5-24小时的保温处理。3. a kind of method that eliminates AM structure in FeCrNiMn quaternary high-entropy alloy according to claim 1, it is characterized in that, the heat treatment of the high-entropy alloy heat treatment pattern described in step (2): FeCrNiMn quaternary high-entropy alloy The heat treatment sample is placed in a muffle furnace for heating and calcination, and the heating rate is controlled to be 10-20°C/min, and the temperature is raised to 900-1200°C. 4.根据权利要求1所述的一种消除FeCrNiMn四元高熵合金中调幅组织的方法,其特征在于,步骤(3)中所述高熵合金热处理式样的冷却处理:将保温处理后的FeCrNiMn四元高熵合金热处理式样立即进行空气冷却处理或淬火处理。4. a kind of method that eliminates the amplitude modulation structure in FeCrNiMn quaternary high-entropy alloy according to claim 1, it is characterized in that, the cooling treatment of the high-entropy alloy heat treatment pattern described in step (3): the FeCrNiMn after the heat preservation treatment The quaternary high-entropy alloy heat-treated samples were immediately air-cooled or quenched. 5.根据权利要求4所述的一种消除FeCrNiMn四元高熵合金中调幅组织的方法,其特征在于,所述淬火处理过程中所使用的溶液为水、盐水或机油中任一种。5. a kind of method for eliminating amplitude modulation structure in FeCrNiMn quaternary high-entropy alloy according to claim 4, is characterized in that, the solution used in described quenching treatment process is any in water, salt water or engine oil. 6.根据权利要求1所述的一种消FeCrNiMn四元高熵合金中调幅组织的方法,其特征在于,步骤(4)中所述高熵合金热处理式样的后处理:采用二氧化硅砂纸对冷却处理后的FeCrNiMn四元高熵合金热处理式样进行研磨,将研磨后的FeCrNiMn四元高熵合金热处理式样再用抛光膏在抛光机上进行手动抛光。6. a kind of method of eliminating AM structure in FeCrNiMn quaternary high-entropy alloy according to claim 1, is characterized in that, the post-processing of the high-entropy alloy heat treatment pattern described in step (4): adopt silica sandpaper to The FeCrNiMn quaternary high-entropy alloy heat-treated sample after cooling treatment was ground, and the ground FeCrNiMn quaternary high-entropy alloy heat-treated sample was manually polished with polishing paste on a polishing machine.
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CN110983146A (en) * 2019-12-31 2020-04-10 苏州热工研究院有限公司 A kind of preparation method of large-scale manganese-containing high-entropy alloy ingot

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Application publication date: 20201023