CN101306464A - A process for preparing high-performance structural parts with high SiC particle volume fraction - Google Patents
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Abstract
本发明是一种制备高SiC颗粒体积分数高性能结构件工艺，在80℃－120℃对块状基体金属合金进行干燥处理后，在电阻炉中加热熔化，合金在完全熔化后保温静置20－30分钟；向保温静置后的合金液加入体积分数为10％－30％SiC颗粒，边加入边均匀搅拌，同时控制冷却到半固态温度区间，得到SiC体积分数为10％－30％的颗粒增强复合材料半固态浆料；高性能结构件的成形腔设计在挤压模具凹模腔的底部边缘水平方向；利用半固态挤压成形时液相和固相偏析和分离特点，用半固态挤压成形方法加工出高SiC体积分数颗粒增强金属基复合材料高性能结构件。本发明主要用于高性能结构件成形领域，可以实现高SiC颗粒体积分数高性能结构件的短流程、近终形的成形制造，还可以降低能源消耗，提高产品综合性能。The present invention is a process for preparing high-performance structural parts with high SiC particle volume fraction. After drying the bulk matrix metal alloy at 80°C-120°C, it is heated and melted in a resistance furnace, and the alloy is kept for 20 minutes after complete melting. -30 minutes; add SiC particles with a volume fraction of 10%-30% to the alloy liquid after heat preservation and standing still, stir evenly while adding, and control cooling to the semi-solid temperature range at the same time, to obtain SiC with a volume fraction of 10%-30% Particle-reinforced composite material semi-solid slurry; the forming cavity of high-performance structural parts is designed in the horizontal direction of the bottom edge of the die cavity of the extrusion die; utilizing the characteristics of segregation and separation of liquid and solid phases during semi-solid extrusion forming, semi-solid High-performance structural parts of metal matrix composites reinforced with high SiC volume fraction particles processed by extrusion molding. The invention is mainly used in the forming field of high-performance structural parts, and can realize short-process and near-net shape forming and manufacturing of high-performance structural parts with high SiC particle volume fraction, can also reduce energy consumption, and improve product comprehensive performance.
Description
技术领域 technical field
本发明属于高性能结构件成形领域，特别是提供了一种用半固态技术制备高SiC颗粒体积分数高性能结构件工艺。The invention belongs to the field of forming high-performance structural parts, and in particular provides a process for preparing high-performance structural parts with high SiC particle volume fraction by semi-solid technology.
背景技术 Background technique
现代科学技术的进步对材料科学与工程技术的要求日益提高，开发新型高性能复合材料以及其先进加工技术已经成为广大高科技企业需要迫切解决的问题，这一现象在电子封装领域体现得更为明显。航空航天、电子通信的飞速发展要求电子元器件能够具有更高的集成度、更快的运行速度和更大的容量，使电子器件和电子装置中元器件的复杂性和密集性日益提高，这必然会导致电路发热量提高、工作温度上升，而稳定性下降。据计算，在半导体器件中，温度每升高20℃，失效的可能性就增加3-4倍。目前，用于封装领域的高SiC颗粒体积分数复合材料结构件主要通过用粉末注射法(SiC预制坯+液态金属熔渗)制备加工。该方法的主要缺点是：①加工工艺流程长，成本高；②SiC与基体金属界面润湿性差，且易形成不利的中间相；③SiC颗粒体积分数上不去，热导率提高能力有限；④SiC预制坯在液态金属熔渗时易被压塌，且不易充满，制备加工的结构件气密性差；⑤只能做简单形状的零件；⑥规模化生产能力差。With the advancement of modern science and technology, the requirements for material science and engineering technology are increasing day by day. The development of new high-performance composite materials and their advanced processing technology has become an urgent problem for high-tech enterprises to solve. This phenomenon is more reflected in the field of electronic packaging. obvious. The rapid development of aerospace and electronic communication requires electronic components to have higher integration, faster operation speed and larger capacity, which makes the complexity and density of components in electronic devices and electronic devices increase day by day. It will inevitably lead to an increase in the heat generation of the circuit, an increase in the operating temperature, and a decrease in stability. According to calculations, in semiconductor devices, the probability of failure increases by 3-4 times for every 20°C increase in temperature. At present, high SiC particle volume fraction composite structural parts used in the packaging field are mainly prepared and processed by powder injection method (SiC preform + liquid metal infiltration). The main disadvantages of this method are: ①The processing process is long and the cost is high; ②SiC has poor wettability with the base metal interface, and it is easy to form an unfavorable intermediate phase; ③SiC particle volume fraction cannot increase, and the ability to improve thermal conductivity is limited; ④SiC prefabrication The billet is easy to be crushed and collapsed when the liquid metal is infiltrated, and it is not easy to be filled, and the airtightness of the prepared and processed structural parts is poor; ⑤ only parts with simple shapes can be made; ⑥ the large-scale production capacity is poor.
所谓半固态加工是对具有一定液相组分的固液混合浆料进行压铸、挤压或模锻成形，是一种介于普通铸造(纯液态)和锻压(纯固态)之间的成形方法(M.C.Flemings.Behavior of Alloys in Semi-solidState.Metallurgical Transactions，1990，Vol.22B：269-293)。半固态浆料具有流变性和触变性，变形抗力非常小，因而可以成形断面十分复杂的零件，实现近净成形，并且缩短了加工周期，提高了材料利用率，有利于节能节材。半固态成形时，液相与固相容易偏析和分离。一般认为，半固态成形过程中液相与固相偏析和分离会导致成形件中成份组织分布不均，从而产生组织性能和力学性能分布不均，对使用性能产生不利影响。在SiC颗粒增强A356铝合金复合材料半固态触变挤压成形中，通过对成形件部分区域的显微组织观察发现，SiC增强颗粒分布密度随着半固态浆料充填行程的不断增加呈不断上升的趋势，与半固态成形中液相流动及分布规律一致。其根本的原因是由于在半固态浆料中SiC增强颗粒主要分布于以β-共晶相存在的液相中的缘故，在随后的半固态挤压成形中SiC增强颗粒随着液相流动到零件的边部或顶部，增加的幅度约为成形前复合材料中SiC颗粒体积分数的2-3倍。这表明，SiC颗粒体积分数的提高可以通过对液相分数分布规律进行控制来实现，也就是可用低SiC体积分数的颗粒增强复合材料通过半固态挤压成形得到高SiC体积分数的高性能结构零件，从而降低热膨胀系数。实现把半固态成形中液相与固相偏析和分离的不利因素转化为制备与成形高SiC颗粒体积分数复合材料结构件时的有利因素。The so-called semi-solid processing is to die-cast, extrude or die-forge a solid-liquid mixed slurry with a certain liquid phase component. It is a forming method between ordinary casting (pure liquid state) and forging (pure solid state). (M.C. Flemings. Behavior of Alloys in Semi-solid State. Metallurgical Transactions, 1990, Vol. 22B: 269-293). Semi-solid slurry has rheology and thixotropy, and the deformation resistance is very small, so it can form parts with very complex cross-sections, realize near-net shape, shorten the processing cycle, improve material utilization, and help save energy and materials. During semi-solid forming, liquid phase and solid phase are easy to segregate and separate. It is generally believed that the segregation and separation of liquid phase and solid phase in the semi-solid forming process will lead to uneven distribution of components in the formed part, resulting in uneven distribution of structural properties and mechanical properties, which will have an adverse effect on the performance. In the semi-solid thixotropic extrusion forming of SiC particle-reinforced A356 aluminum alloy composites, the observation of the microstructure of some areas of the formed parts shows that the distribution density of SiC-reinforced particles increases continuously with the increase of the filling stroke of the semi-solid slurry The trend is consistent with the liquid phase flow and distribution in semi-solid forming. The fundamental reason is that in the semi-solid slurry, the SiC-reinforced particles are mainly distributed in the liquid phase that exists in the β-eutectic phase, and in the subsequent semi-solid extrusion molding, the SiC-reinforced particles flow with the liquid phase to the The edge or top of the part increases by about 2-3 times the volume fraction of SiC particles in the composite material before forming. This shows that the increase of the SiC particle volume fraction can be achieved by controlling the distribution of the liquid phase fraction, that is, the particle-reinforced composite material with a low SiC volume fraction can be used to obtain high-performance structural parts with a high SiC volume fraction through semi-solid extrusion. , thereby reducing the coefficient of thermal expansion. Realize the conversion of unfavorable factors of liquid phase and solid phase segregation and separation in semi-solid forming into favorable factors when preparing and forming high SiC particle volume fraction composite material structural parts.
实际上，金属(复合)材料以及超导材料的导热、导电性能除了与(复合)材料本身成份结构相关外，与其加工过程中形成的形变织构有很重要的关系。目前国内外用SiC预制坯的Al液或Cu液润浸法制备高性能封装用结构件仍是走传统铸造成型的道路，所得到的复合材料结构件显微组织中无明显形变织构，也就是说，所制备加工的封装用结构件是各向同性。在半固态挤压成形过程中，浆料是在一定的压力下由模具挤入模腔，其中的α-相在充填过程中会被拉长，形成与充填方向相一致的有利织构。In fact, the thermal conductivity and electrical conductivity of metal (composite) materials and superconducting materials are not only related to the composition and structure of the (composite) materials themselves, but also have a very important relationship with the deformation texture formed during processing. At present, the preparation of structural parts for high-performance packaging by Al or Cu liquid infiltration of SiC preforms at home and abroad still follows the traditional casting method, and the obtained composite structural parts have no obvious deformation texture in the microstructure, that is, In other words, the prepared and processed structural members for packaging are isotropic. In the semi-solid extrusion process, the slurry is extruded from the mold into the cavity under a certain pressure, and the α-phase in it will be elongated during the filling process, forming a favorable texture consistent with the filling direction.
发明内容 Contents of the invention
本发明的目的在于提供一种用半固态技术制备高SiC颗粒体积分数颗粒增强复合材料高性能结构件工艺，克服了用粉末注射法制备高SiC体积分数复合材料结构件时存在的SiC体积分数‘上不去’、加工路线长、生产成本高等问题，利用半固态挤压成形中液相与固相偏析和分离的特征，制备加工高SiC颗粒体积分数颗粒增强复合材料高性能结构件。The purpose of the present invention is to provide a process for preparing high-performance structural parts of high-SiC particle volume fraction particle-reinforced composite materials with semi-solid technology, which overcomes the SiC volume fraction that exists when preparing high-SiC volume fraction composite material structural parts by powder injection method. In order to solve the problems of "can't go up", long processing route, high production cost, etc., the characteristics of segregation and separation of liquid phase and solid phase in semi-solid extrusion forming are used to prepare and process high-performance structural parts of particle-reinforced composite materials with high SiC particle volume fraction.
具体工艺步骤如下：The specific process steps are as follows:
(1)在80℃-120℃对块状基体金属合金进行干燥处理后，在电阻炉中加热熔化，合金在完全熔化后保温静置20-30分钟；(1) After drying the bulk matrix metal alloy at 80°C-120°C, heat and melt in a resistance furnace, and keep the alloy for 20-30 minutes after it is completely melted;
(2)向保温静置后的合金液加入体积分数为10％-30％SiC颗粒，边加入边均匀搅拌，同时控制冷却到半固态温度区间，得到SiC体积分数为10％-30％的颗粒增强复合材料半固态浆料；(2) Add SiC particles with a volume fraction of 10%-30% to the alloy liquid after heat preservation and standing, stir evenly while adding, and control cooling to the semi-solid temperature range at the same time, to obtain particles with a SiC volume fraction of 10%-30% Reinforced composite material semi-solid slurry;
(3)所述的SiC颗粒增强金属基复合材料半固态浆料在成形模具中挤压成形得到SiC颗粒体积分数为40％-60％的结构件：成形速度控制在80mm/s-140mm/s，模具预热温度设为200℃-300℃，成形压力设为400KN-600KN，保压时间设为5-10秒。(3) The SiC particle reinforced metal matrix composite semi-solid slurry is extruded in a forming die to obtain a structural part with a SiC particle volume fraction of 40%-60%: the forming speed is controlled at 80mm/s-140mm/s , The mold preheating temperature is set at 200°C-300°C, the forming pressure is set at 400KN-600KN, and the holding time is set at 5-10 seconds.
本发明的另一个技术方案是：所述的基体合金为A356铝合金、AZ91镁合金或CuZn31Al2黄铜合金。Another technical solution of the present invention is: the base alloy is A356 aluminum alloy, AZ91 magnesium alloy or CuZn31Al2 brass alloy.
本发明的又一个技术方案是：所述的成形模具的成形腔应开设在挤压模具凹模的底部位置，并与挤压方向垂直。Yet another technical solution of the present invention is: the forming cavity of the forming die should be set at the bottom of the die of the extrusion die and perpendicular to the extrusion direction.
半固态挤压成形高SiC颗粒体积分数高性能结构件分为触变挤压成形和流变挤压成形两种方法。当使用流变挤压成形方法制备高SiC颗粒体积分数高性能结构件时，直接将半固态浆料输送到模具中挤压成形；对于用触变挤压成形方法制备高SiC颗粒体积分数高性能结构件，需要进行半固态坯料二次感应加热，将感应加热后半固态坯料放入挤压模具中挤压成形得到高SiC颗粒体积分数高性能结构件。Semi-solid extrusion forming of high-performance structural parts with high SiC particle volume fraction can be divided into two methods: thixotropic extrusion and rheological extrusion. When using the rheological extrusion forming method to prepare high-performance structural parts with high SiC particle volume fraction, the semi-solid slurry is directly conveyed to the mold for extrusion molding; For structural parts, secondary induction heating of the semi-solid billet is required, and the semi-solid billet after induction heating is put into an extrusion die for extrusion molding to obtain a high-performance structural part with a high SiC particle volume fraction.
本发明的优点Advantages of the invention
利用半固态成形过程中液相与固相偏析和分离特征，将半固态成形工艺应用于SiC颗粒增强复合材料高性能结构件的制备。所得到的技术原型和通用性核心技术可同样运用于其它(SiC)颗粒增强复合材料成形高颗粒体积分数的复杂形状结构零件，如Al2O3/Cu合金和Si3N4/Cu合金等。Utilizing the segregation and separation characteristics of liquid and solid phases in the semi-solid forming process, the semi-solid forming process was applied to the preparation of high-performance structural parts of SiC particle-reinforced composites. The obtained technical prototype and general core technology can also be applied to other (SiC) particle-reinforced composite materials to form complex shape structural parts with high particle volume fraction, such as Al2O3/Cu alloy and Si3N4/Cu alloy.
用低SiC颗粒体积分数复合材料制备高SiC颗粒体积分数复合材料结构零件。Fabrication of high SiC particle volume fraction composite structural parts with low SiC particle volume fraction composites.
目前，用于封装领域的高SiC颗粒体积分数复合材料结构件主要通过用粉末注射法(SiC预制坯+液态金属熔渗)制备加工。该方法的主要缺点是：①加工工艺流程长，成本高；②SiC与基体金属界面润湿性差，且易形成不利的中间相；③SiC颗粒体积分数上不去，热导率提高能力有限；④SiC预制坯在液态金属熔渗时易被压塌，且不易充满，制备加工的结构件气密性差；⑤只能做简单形状的零件；⑥规模化生产能力差。At present, high SiC particle volume fraction composite structural parts used in the packaging field are mainly prepared and processed by powder injection method (SiC preform + liquid metal infiltration). The main disadvantages of this method are: ①The processing process is long and the cost is high; ②SiC has poor wettability with the base metal interface, and it is easy to form an unfavorable intermediate phase; ③SiC particle volume fraction cannot increase, and the ability to improve thermal conductivity is limited; ④SiC prefabrication The billet is easy to be crushed and collapsed when the liquid metal is infiltrated, and it is not easy to be filled, and the airtightness of the prepared and processed structural parts is poor; ⑤ only parts with simple shapes can be made; ⑥ the large-scale production capacity is poor.
本发明正是针对高SiC颗粒体积分数高性能结构件加工的市场需求，用低SiC颗粒体积分数复合材料通过半固态挤压成形工艺来制备高SiC颗粒体积分数复合材料高性能结构件，扩大了半固态技术的应用领域，拓展了高SiC颗粒体积分数高性能结构件的制造途径，是一种完成崭新的原创性技术和工艺。使用该工艺，不但可以实现高SiC颗粒体积分数高性能结构件的短流程、近终形的成形制造，而且可以降低能源消耗，提高产品质量。完成后将使我国在高强度、超高热导率和低热膨胀系数等高性能复合材料结构件的制备与成形技术上一个大台阶，为其高性能化和低成本生产提供有力保证。The present invention is aimed at the market demand for processing high-performance structural parts with high SiC particle volume fraction, and uses low SiC particle volume fraction composite materials to prepare high-performance structural parts with high SiC particle volume fraction composite materials through a semi-solid extrusion molding process, which expands The application field of semi-solid technology has expanded the manufacturing method of high-performance structural parts with high SiC particle volume fraction, and is a completely new and original technology and process. Using this process, not only can realize the short-process and near-net shape forming and manufacturing of high-performance structural parts with high SiC particle volume fraction, but also can reduce energy consumption and improve product quality. After completion, it will make my country a big step forward in the preparation and forming technology of high-performance composite material structural parts such as high strength, ultra-high thermal conductivity and low thermal expansion coefficient, and provide a strong guarantee for its high-performance and low-cost production.
具体实施方式 Detailed ways
实施例1：使用半固态触变挤压成形方法制备高SiC体积分数颗粒增强A356铝合金复合材料结构件。Example 1: A semi-solid thixotropic extrusion method was used to prepare a high SiC volume fraction particle-reinforced A356 aluminum alloy composite structure.
从Duralcan公司(Duralcan company)购买直径为φ56mm的SiC颗粒(10％体积分数)增强A356铝合金复合材料。距切加工后，首先用感应加热炉将坯料快速均匀加热到半固态温度：577℃。设计结构形式为反挤压成形杯形件的模具，并在凹模腔的底部边缘水平方向加工出高性能结构件的成形腔。将感应加热后的半固态坯料迅速用夹具放入到挤压模具的凹模中(模具预热温度设为200℃)。压力机的挤压速度调整为80mm/s、使用石墨脱模剂，成形压力设为400KN，保压时间设为5秒。使用以上参数可挤压成形得到高SiC颗粒体积分数A356铝合金复合材料结构零件(SiC体积分数40％)。SiC particle (10% volume fraction) reinforced A356 aluminum alloy composite material with a diameter of φ56mm was purchased from Duralcan company (Duralcan company). After the distance cutting process, the billet is firstly heated to the semi-solid temperature quickly and uniformly with an induction heating furnace: 577°C. The structure is designed as a mold for back-extruding cup-shaped parts, and a forming cavity for high-performance structural parts is processed horizontally at the bottom edge of the die cavity. The induction heated semi-solid billet is quickly put into the die of the extrusion die with a clamp (the preheating temperature of the die is set to 200° C.). The extrusion speed of the press is adjusted to 80mm/s, a graphite release agent is used, the forming pressure is set to 400KN, and the holding time is set to 5 seconds. Using the above parameters can be extruded to obtain high SiC particle volume fraction A356 aluminum alloy composite structural parts (SiC volume fraction 40%).
实施例2：使用半固态流变挤压成形方法制备高SiC体积分数颗粒增强A356铝合金复合材料结构件。Example 2: A semi-solid rheological extrusion molding method was used to prepare a high SiC volume fraction particle-reinforced A356 aluminum alloy composite structural part.
在100℃对块状基体金属铝合金A356进行干燥处理后，在电阻炉中加热熔化。熔化温度设为640℃，合金在完全熔化后保温静置30分钟。向保温静置后的合金液加入体积分数为30％的细SiC颗粒。为防止SiC颗粒聚集，在加入过程中要分多次逐步加入，边加入边均匀搅拌，同时控制冷却到半固态温度582℃。设计结构形式为反挤压成形杯形件的模具，并在凹模腔的底部边缘水平方向加工出高性能结构件的成形腔。使用简易浆料输送装置将半固态浆料迅速放入挤压模具的凹模中(模具预热温度设为300℃)。压力机的挤压速度调整为140mm/s、使用石墨脱模剂，成形压力设为600KN，保压时间设为10秒。使用以上参数可挤压成形得到高SiC颗粒体积分数A356铝合金复合材料结构零件(SiC体积分数60％)。After drying the bulk base metal aluminum alloy A356 at 100°C, it was heated and melted in a resistance furnace. The melting temperature was set at 640° C., and the alloy was kept for 30 minutes after it was completely melted. Add fine SiC particles with a volume fraction of 30% to the alloy liquid after heat preservation and standing. In order to prevent SiC particles from aggregating, the addition process should be divided into several times and gradually added, stirring evenly while adding, and controlled cooling to a semi-solid temperature of 582°C. The structure is designed as a mold for back-extruding cup-shaped parts, and a forming cavity for high-performance structural parts is processed horizontally at the bottom edge of the die cavity. The semi-solid slurry was quickly put into the die of the extrusion die using a simple slurry delivery device (the mold preheating temperature was set to 300°C). The extrusion speed of the press is adjusted to 140mm/s, a graphite release agent is used, the forming pressure is set to 600KN, and the holding time is set to 10 seconds. Using the above parameters can be extruded to obtain high SiC particle volume fraction A356 aluminum alloy composite structural parts (SiC volume fraction 60%).
实施例3：使用半固态触变挤压成形方法制备高SiC体积分数颗粒增强黄铜合金CuZn31Al2复合材料结构零件。Example 3: A semi-solid thixotropic extrusion forming method was used to prepare a high SiC volume fraction particle reinforced brass alloy CuZn31Al2 composite structural part.
在100℃对块状基体金属黄铜合金CuZn31Al2进行干燥处理后，在电阻炉中加热熔化。熔化温度设为970℃，合金在完全熔化后保温静置30分钟。向保温静置后的合金液加入体积分数为10％的细SiC颗粒。为防止SiC颗粒聚集，在加入过程中要分多次逐步加入，边加入边均匀搅拌，并使用制坯模制备SiC颗粒增强黄铜合金CuZn31Al2复合材料坯料。设计结构形式为反挤压成形杯形件的模具，并在凹模腔的底部边缘水平方向加工出高性能结构件的成形腔。使用感应加热炉将用制坯模制备的黄铜合金复合材料坯料快速均匀加热到半固态温度：960℃。使用夹具将感应加热后半固态坯料迅速放入挤压模具的凹模中(模具预热温度设为220℃)。压力机的挤压速度调整为90mm/s、使用石墨脱模剂，成形压力设为450KN，保压时间设为7秒。使用以上参数可挤压成形得到高SiC颗粒体积分数黄铜合金CuZn31Al2复合材料结构零件(SiC体积分数45％)。After the bulk matrix metal brass alloy CuZn31Al2 is dried at 100°C, it is heated and melted in a resistance furnace. The melting temperature was set at 970°C, and the alloy was kept for 30 minutes after it was completely melted. Add fine SiC particles with a volume fraction of 10% to the alloy liquid after heat preservation and standing. In order to prevent SiC particles from agglomerating, the addition process should be divided into several times and gradually added, and evenly stirred while adding, and the SiC particle-reinforced brass alloy CuZn31Al2 composite material blank is prepared by using the billet mold. The structure is designed as a mold for back-extruding cup-shaped parts, and a forming cavity for high-performance structural parts is processed horizontally at the bottom edge of the die cavity. The brass alloy composite billet prepared by the billet mold was rapidly and uniformly heated to the semi-solid temperature: 960 °C using an induction heating furnace. The semi-solid billet after induction heating was quickly put into the concave die of the extrusion die (the die preheating temperature was set to 220° C.) using a clamp. The extrusion speed of the press is adjusted to 90mm/s, a graphite release agent is used, the forming pressure is set to 450KN, and the holding time is set to 7 seconds. Using the above parameters, the brass alloy CuZn31Al2 composite structure parts with high SiC particle volume fraction (SiC volume fraction 45%) can be obtained by extrusion.
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