CN107881443A - A kind of high-entropy alloy squeezes pier composite modification technology - Google Patents
A kind of high-entropy alloy squeezes pier composite modification technology Download PDFInfo
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Abstract
本发明涉及一种专门针对高熵合金材料的热加工与晶粒细化的塑性改性技术制备组织均匀的高性能高熵合金材料的方法。本发明的目的主要在于:提供一种针对高熵合金服役要求的挤墩复合塑性改性方法。针对高熵合金的热加工特点,采用先墩再挤,挤完再墩,反复墩挤的方法,有效控制变形过程中高熵合金材料内部的应力状态,提高三向压缩应力,有效抑制晶格畸变诱发的微裂纹的萌生与扩展,细化晶粒,提高综合力学性,实现高熵合金的有效改性。挤墩复合工艺易于实现,成本低廉,能够获得组织性能均匀优良的高熵合金锭坯材料,有效提高其服役能力,采用该方法不仅能促进高熵合金的大批量使用,而且还可以有效改善以及控制高熵合金的力学性能。The invention relates to a method for preparing a high-performance high-entropy alloy material with uniform structure by a plastic modification technology specially aimed at thermal processing and grain refinement of the high-entropy alloy material. The main purpose of the present invention is to provide a composite plastic modification method for extruded piers aimed at the service requirements of high-entropy alloys. According to the thermal processing characteristics of high-entropy alloys, the method of pier first and then extrusion, extrusion and then pier, and repeated pier extrusion can effectively control the stress state inside the high-entropy alloy material during the deformation process, increase the three-dimensional compressive stress, and effectively suppress lattice distortion. The initiation and propagation of induced micro-cracks refine the grains, improve the comprehensive mechanical properties, and realize the effective modification of high-entropy alloys. The extrusion composite process is easy to implement and low in cost. It can obtain high-entropy alloy ingot materials with uniform and excellent structure properties, and effectively improve its service ability. This method can not only promote the large-scale use of high-entropy alloys, but also effectively improve and Controlling the mechanical properties of high-entropy alloys.
Description
技术领域technical field
本发明涉及一种专门针对高熵合金材料热加工与晶粒细化的塑性改性方法。The invention relates to a plastic modification method specially aimed at thermal processing and grain refinement of high-entropy alloy materials.
背景技术Background technique
高熵合金是近年来广受关注的新兴材料,具有高硬度、高强度、高耐磨性和高耐腐蚀性等良好的力学、物理及化学性能,在现代工程领域有着广泛的应用前景。但由于高熵合金晶格畸变严重,铸态组织为典型的枝晶结构,在高温变形条件下塑性较低,同时由于铸造缺陷的存在,经过高温锻造后易开裂,其优异的力学性能在工程应用中无法得到充分发挥,极大地限制了高熵合金的大规模工程应用。为了消除铸造缺陷,对高熵合金通常采用锻造改性。High-entropy alloys are emerging materials that have attracted widespread attention in recent years. They have good mechanical, physical and chemical properties such as high hardness, high strength, high wear resistance and high corrosion resistance, and have broad application prospects in modern engineering. However, due to the serious lattice distortion of high-entropy alloys, the as-cast structure is a typical dendrite structure, and the plasticity is low under high-temperature deformation conditions. At the same time, due to the existence of casting defects, it is easy to crack after high-temperature forging. It cannot be fully utilized in the application, which greatly limits the large-scale engineering application of high-entropy alloys. In order to eliminate casting defects, high-entropy alloys are usually modified by forging.
高温锻造是重要的材料加工技术,可以闭合微裂纹,打碎树枝晶,有效改善材料的组织性能,是金属材料的重要改性方法。但高熵合金由于晶格畸变严重,锻造过程中易形成裂纹,极大的阻碍了塑性加工锻造改性工艺的应用。High-temperature forging is an important material processing technology. It can close microcracks, break up dendrites, and effectively improve the structure and properties of materials. It is an important modification method for metal materials. However, due to the serious lattice distortion of high-entropy alloys, cracks are easy to form during forging, which greatly hinders the application of plastic processing forging modification technology.
镦粗加工是锻造加工中使锻件坯料髙度减小,横截面积增大的成形工艺。镦粗时,由于材料上下两个端面与锻造设备砧板之间存在接触摩擦,引起材料不均匀流动,会导致材料不同区域的温度、受力情况、变形程度、组织转变等不均匀,而对于高熵合金镦粗来说,由于上述问题与晶格畸变问题的共同作用,常易在侧表面产生纵向或呈45°方向的裂纹。Upsetting is a forming process that reduces the height of the forging blank and increases the cross-sectional area in forging. When upsetting, due to the contact friction between the upper and lower end faces of the material and the cutting board of the forging equipment, the material will flow unevenly, which will lead to uneven temperature, stress, deformation degree, and tissue transformation in different regions of the material. For entropy alloy upsetting, due to the combined effect of the above problems and the lattice distortion problem, it is often easy to generate longitudinal or 45° direction cracks on the side surface.
挤压,是对置于模具模腔(或挤压筒)内的金属坯料施加外力,迫使金属从模孔中挤出,获得所需端面形状、尺寸并具有一定力学性能的挤压制件的塑性加工方法,其应力状态是典型的三向压应力,可以有效闭合微裂纹。Extrusion is the process of applying external force to the metal billet placed in the die cavity (or extrusion cylinder) to force the metal to extrude from the die hole to obtain the desired end face shape, size and extrusion parts with certain mechanical properties. The plastic processing method, whose stress state is a typical three-dimensional compressive stress, can effectively close microcracks.
鉴于此,本发明提出一种简单易实现的塑性加工技术,即挤墩复合改性技术,挤墩复合可以改善材料内部的应力状态,提高三向压应力,降低拉应力水平以提高材料成形性能的锻造方法,对于提高高熵合金塑性加工性能具有重要的作用和意义。通过对高熵合金锭坯施加充分多次挤墩复合加工,有效控制塑性加工过程中锭坯内部应力分布,形成针对变形过程特征的梯度三向压缩应力,有效抑制高熵合金变形过程中微裂纹的萌生与扩展,细化晶粒,完成对高熵合金微观组织的精细化有效控制,实现高效塑性改性,此过程可以在传统挤压筒及锻锤等加工设备上实现,简单易行,易推广应用。In view of this, the present invention proposes a simple and easy-to-implement plastic processing technology, that is, extruded pier composite modification technology. Extruded pier composite can improve the stress state inside the material, increase the three-dimensional compressive stress, and reduce the level of tensile stress to improve the forming performance of the material. The forging method has an important role and significance in improving the plastic processing performance of high-entropy alloys. By applying sufficient multi-extrusion compound processing to the high-entropy alloy ingot, the internal stress distribution of the ingot during the plastic processing process can be effectively controlled, and a gradient three-dimensional compressive stress specific to the characteristics of the deformation process can be formed to effectively suppress microcracks during the deformation process of the high-entropy alloy. The initiation and expansion of the microstructure, the refinement of the grains, the refinement and effective control of the microstructure of the high-entropy alloy, and the realization of high-efficiency plastic modification. This process can be realized on processing equipment such as traditional extrusion cylinders and forging hammers, which is simple and easy. Easy to promote and apply.
发明内容Contents of the invention
本发明的目的在于:提供一种针对高熵合金服役要求的挤墩复合塑性改性方法。针对高熵合金的热加工特点,采用先墩再挤,挤完再墩,反复墩挤的方法,有效控制变形过程中高熵合金材料内部的应力状态,提高三向压缩应力,有效抑制晶格畸变诱发的微裂纹的萌生与扩展,细化晶粒,提高综合力学性,实现高熵合金的有效改性。The purpose of the present invention is to provide a compound plastic modification method for extruded piers aimed at the service requirements of high-entropy alloys. According to the thermal processing characteristics of high-entropy alloys, the method of pier first and then extrusion, extrusion and then pier, and repeated pier extrusion can effectively control the stress state inside the high-entropy alloy material during the deformation process, increase the three-dimensional compressive stress, and effectively suppress lattice distortion. The initiation and propagation of induced micro-cracks refine the grains, improve the comprehensive mechanical properties, and realize the effective modification of high-entropy alloys.
挤墩复合工艺易于实现,成本低廉,能够获得组织性能均匀优良的高熵合金锭坯材料,有效提高其服役能力,采用该方法不仅能促进高熵合金的大批量使用,而且还可以有效改善以及控制高熵合金的力学性能。The extrusion composite process is easy to implement and low in cost. It can obtain high-entropy alloy ingot materials with uniform and excellent structure properties, and effectively improve its service ability. This method can not only promote the large-scale use of high-entropy alloys, but also effectively improve and Controlling the mechanical properties of high-entropy alloys.
为解决上述技术问题,本发明挤墩复合改性方法采用以下技术方案来实现:In order to solve the above-mentioned technical problems, the compound modified method of extruded pier of the present invention adopts the following technical solutions to realize:
第一步:高熵合金原始毛坯的制作。按照锭坯尺寸下料高熵合金棒料,然后将根据高熵合金的组织成份的不同,加热到900℃-1200℃的起始温度,按照棒料厚度0.8-1min/mm进行保温处理,保温12-100h,促使其内部组织均匀。The first step: the production of the original blank of the high-entropy alloy. According to the size of the ingot, the high-entropy alloy bar is cut, and then according to the composition of the high-entropy alloy, it is heated to an initial temperature of 900°C-1200°C, and the heat preservation treatment is carried out according to the thickness of the bar 0.8-1min/mm. 12-100h, to promote the uniformity of its internal organization.
第二步:高熵合金棒料墩粗工艺分析及镦粗加工。结合所选用高熵合金的成份以及变形特点,通过软件计算与模拟仿真,获得墩粗变形过程中锭坯不同部位的应力特征与规律,尤其是三向压缩应力的分布规律与损伤分布。在此基础上,结合材料应力与损伤特征,分析高熵合金在不同墩粗条件下的变形以及三向压缩应力与损伤分布变化,获得最合适的墩粗高径比,进而优化墩粗方案,避免墩粗产生鼓形裂纹。在此基础上,依托优化的镦粗方案,对已经第一步均匀化的高熵合金锭坯进行镦粗加工,上下砧板采用平砧板,砧板预热至500度,应变速率0.01s-1-0.1s-1,首选0.05s-1。The second step: Analysis of high-entropy alloy bar pier roughing process and upsetting process. Combined with the composition and deformation characteristics of the selected high-entropy alloy, through software calculation and simulation, the stress characteristics and laws of different parts of the ingot during the thick deformation of the pier, especially the distribution of three-dimensional compressive stress and damage distribution, are obtained. On this basis, combined with the material stress and damage characteristics, the deformation of the high-entropy alloy under different pier thickness conditions and the change of three-dimensional compressive stress and damage distribution are analyzed to obtain the most suitable pier thickness height-to-diameter ratio, and then optimize the pier thickness scheme. Avoid pier thickening to produce drum-shaped cracks. On this basis, relying on the optimized upsetting scheme, the high-entropy alloy ingot that has been homogenized in the first step is upset. The upper and lower cutting boards are flat cutting boards. The cutting boards are preheated to 500 degrees and the strain rate is 0.01s -1 - 0.1s -1 , 0.05s -1 is preferred.
第三步:高熵合金挤压工艺分析及挤压加工。墩粗完成后,对已变形的高熵合金胚料进行高温挤压。通过软件计算与模拟仿真,分析挤压过程中高熵合金的材料流动特征,获得优化的挤压工艺方案。在此基础上,结合分析结果,开展高熵合金挤压加工,减小坯料直径,增加材料长度。挤压温度900-1100度,挤压比小于2。The third step: high-entropy alloy extrusion process analysis and extrusion processing. After the pier is thickened, high-temperature extrusion is performed on the deformed high-entropy alloy billet. Through software calculation and simulation, the material flow characteristics of the high-entropy alloy in the extrusion process are analyzed, and the optimized extrusion process scheme is obtained. On this basis, combined with the analysis results, high-entropy alloy extrusion processing was carried out to reduce the diameter of the billet and increase the length of the material. The extrusion temperature is 900-1100 degrees, and the extrusion ratio is less than 2.
第四步:循环墩粗。将挤压完成后的高熵合金棒料再放入加热炉升温、保温。当达到变形温度后,将高熵合金取出进行再次高温墩粗加工改性。变形温度900℃-1200℃,优选1100℃,应变速率0.01s-1-0.1s-1,首选0.05s-1。The fourth step: thick loop pier. Put the extruded high-entropy alloy bar into the heating furnace to raise the temperature and keep it warm. When the deformation temperature is reached, the high-entropy alloy is taken out for another high-temperature pier rough machining modification. The deformation temperature is 900°C-1200°C, preferably 1100°C, and the strain rate is 0.01s -1 -0.1s -1 , preferably 0.05s -1 .
第五步:循环挤压。对经过再次镦粗的高熵合金坯料进行再次挤压加工,挤压温度900-1100度,挤压比小于2。Step 5: Loop Extrusion. Re-extrude the high-entropy alloy billet after re-upsetting, the extrusion temperature is 900-1100 degrees, and the extrusion ratio is less than 2.
继续反复第四步及第五步流程,镦粗挤压复合循环,直至获得晶粒细小组织均匀,具有优良服役能力的高熵合金锭坯,所加工高熵合金组织性能满足服役要求。Continue to repeat the process of the fourth and fifth steps, upsetting and extruding compound cycle, until a high-entropy alloy ingot with fine grain structure and uniform structure and excellent service ability is obtained, and the structure and performance of the processed high-entropy alloy meet the service requirements.
与现有技术相比,本发明的有益效果如下:Compared with the prior art, the beneficial effects of the present invention are as follows:
高熵合金由多元素组元组成,其铸态组织多以粗大的枝晶为主,这种组织结构会严重的影响高熵合金的综合性能。通过塑性加工可以破碎枝晶、细化晶粒,但是由于高熵合金中大原子半径组元的存在,导致其存在严重的晶格畸变,在塑性变形过程中容易导致开裂,裂纹的形成会严重影响材料的应用。通过挤墩复合加工可以有效提高压缩应力,控制变形过程中高熵合金材料内部的应力状态,提高三向压缩应力,完成破碎粗大枝晶的同时抑制晶格畸变诱发的微裂纹的萌生与扩展,细化晶粒,提高综合力学性,改善材料的微观组织与力学性能,实现加工改性。High-entropy alloys are composed of multi-element components, and their as-cast structures are mostly coarse dendrites, which will seriously affect the comprehensive properties of high-entropy alloys. Plastic processing can break dendrites and refine grains, but due to the existence of large atomic radius components in high-entropy alloys, there are serious lattice distortions, which can easily lead to cracks during plastic deformation, and the formation of cracks will be serious. affect the application of the material. The compressive stress can be effectively increased by the composite processing of piers, the stress state inside the high-entropy alloy material can be controlled during the deformation process, the three-dimensional compressive stress can be increased, and the coarse dendrites can be broken while inhibiting the initiation and expansion of micro-cracks induced by lattice distortion. Crystallization, improve comprehensive mechanical properties, improve the microstructure and mechanical properties of materials, and realize processing modification.
附图说明Description of drawings
图1是高熵合金锭坯制备的工艺流程见说明书附图。Fig. 1 is the process flow of high entropy alloy ingot preparation, see the accompanying drawings.
具体实施方式Detailed ways
以AlCrFeNiCuMu为例,本实施方式是一种通过墩挤复合技术制备组织均匀并且力学性能显著提高的AlCrFeNiCuMu0.5高熵合金锭坯的方法,具体时按以下步骤完成:Taking AlCrFeNiCuMu as an example, this embodiment is a method for preparing an AlCrFeNiCuMu 0.5 high-entropy alloy ingot with a uniform structure and significantly improved mechanical properties through pier extrusion composite technology. Specifically, it is completed according to the following steps:
(1)准备高熵合金:AlCrFeNiCuMu0.5铸锭:选取成分为AlCrFeNiCuMu0.5的高熵合金的铸锭,5种元素的摩尔比分别为Al:Cr:Fe:Ni:Cu:Mu=1:1:1:1:1:0.5。(1) Prepare a high-entropy alloy: AlCrFeNiCuMu 0.5 ingot: Select an ingot of a high-entropy alloy with a composition of AlCrFeNiCuMu 0.5 , and the molar ratios of the five elements are Al:Cr:Fe:Ni:Cu:Mu=1:1: 1:1:1:0.5.
(2)均匀化热处理:将步骤(1)选取的AlCrFeNiCuMu 0.5高熵合金铸锭进行均匀化热处理,均匀化热处理的温度为1000℃-1100℃,然后按照铸锭厚度 0.8-1min/mm进行保温处理,均匀化热处理的保温时间为12h-100h,得到内部组织成分均匀化的高熵合金铸锭。(2) Homogenization heat treatment: perform homogenization heat treatment on the AlCrFeNiCuMu 0.5 high-entropy alloy ingot selected in step (1), the temperature of the homogenization heat treatment is 1000°C-1100°C, and then heat preservation according to the thickness of the ingot 0.8-1min/mm Treatment, the heat preservation time of homogenization heat treatment is 12h-100h, and the high-entropy alloy ingot with homogenized internal structure components is obtained.
(3)墩粗变形过程模拟仿真:通过数值模拟软件对变形过程进行计算机仿真,获得变形过程锭坯不同部位的应力特征与规律,尤其是三向压缩应力的分布规律与损伤分布。在此基础上,结合材料应力与损伤特征,分析高熵合金在不同墩粗条件下的变形以及三向压缩应力与损伤分布变化,优化墩粗方案和墩粗比,避免墩粗产生鼓肚裂纹。监测高熵合金组织变化及晶粒度变化。(3) Simulation of pier coarse deformation process: Computer simulation of the deformation process is carried out through numerical simulation software to obtain the stress characteristics and laws of different parts of the ingot during the deformation process, especially the distribution of three-dimensional compressive stress and damage distribution. On this basis, combined with the material stress and damage characteristics, the deformation of the high-entropy alloy under different pier thickness conditions and the change of three-dimensional compressive stress and damage distribution are analyzed, and the pier thickness scheme and pier thickness ratio are optimized to avoid belly cracks due to pier thickness . Monitor the structure change and grain size change of high entropy alloy.
在此基础上,依托优化的镦粗方案,对已经第一步均匀化的AlCrFeNiCuMu0.5高熵合金锭坯进行镦粗加工,上下砧板采用平砧板,砧板预热至500度,应变速率0.01s-1-0.1s-1,首选0.05s-1。On this basis, relying on the optimized upsetting scheme, the AlCrFeNiCuMu 0.5 high-entropy alloy ingot that has been homogenized in the first step is subjected to upsetting processing. The upper and lower cutting boards are flat cutting boards . 1 -0.1s -1 , preferably 0.05s -1 .
(4)挤压加工设计及模拟仿真:通过软件计算与模拟仿真,分析挤压过程中AlCrFeNiCuMu0.5高熵合金的材料流动特征,获得优化的挤压工艺方案。在此基础上,结合分析结果,开展AlCrFeNiCuMu0.5高熵合金挤压加工。挤压温度 900-1200度,挤压比小于2。(4) Extrusion processing design and simulation: Through software calculation and simulation, the material flow characteristics of AlCrFeNiCuMu 0.5 high-entropy alloy during extrusion were analyzed, and an optimized extrusion process plan was obtained. On this basis, combined with the analysis results, the extrusion processing of AlCrFeNiCuMu 0.5 high-entropy alloy was carried out. The extrusion temperature is 900-1200 degrees, and the extrusion ratio is less than 2.
(5)再次墩粗、挤压加工:将经挤压加工后的AlCrFeNiCuMu0.5放入加热炉加热,并重复第3步及第4步流程,反复墩挤细化AlCrFeNiCuMu0.5高熵合金组织,同时通过墩挤工艺的复合,抑制由于高熵合金严重晶格畸变所引起的微裂纹的萌生与扩展,结合金相分析及力学性能测试,最终得到晶粒更为细小且组织均匀,具有优良服役能力的高熵合金锭坯。(5) Thickening and extrusion processing again: Put the AlCrFeNiCuMu 0.5 after extrusion processing into the heating furnace for heating, and repeat the process of step 3 and step 4, repeatedly pier extrusion to refine the AlCrFeNiCuMu 0.5 high-entropy alloy structure, and at the same time Through the combination of piercing process, the initiation and propagation of micro-cracks caused by the severe lattice distortion of high-entropy alloys are suppressed, combined with metallographic analysis and mechanical performance testing, the final grain size is finer and the structure is uniform, with excellent serviceability high-entropy alloy ingots.
本实施方式的优点:The advantage of this implementation mode:
(1)本实施方式通过挤墩复合改性方法制备出的高熵合金构件,由于在加工过程中始终对高熵合金坯料实施反复挤压及墩粗,能够很好地抑制高熵合金严重晶格畸变所引起的微裂纹的萌生与扩展,得到晶粒更为细小且组织均匀,具有优良服役能力的高熵合金锭坯。(1) In this embodiment, the high-entropy alloy component prepared by the extruding pier composite modification method can well suppress the serious crystallization of the high-entropy alloy due to repeated extrusion and pier thickening of the high-entropy alloy blank during the processing process. The initiation and propagation of micro-cracks caused by lattice distortion can obtain a high-entropy alloy ingot with finer grains, uniform structure, and excellent serviceability.
(2)本实施方式可以制备出较大尺寸的高熵合金构件,并且加工过程可以在传统液压机或锻锤等加工设备上实现,简单易行,易于推广应用。(2) This embodiment can prepare larger-sized high-entropy alloy components, and the processing process can be realized on processing equipment such as traditional hydraulic presses or forging hammers, which is simple and easy to popularize and apply.
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