CN114505497A - A method of using electric pulses to control the precipitation phase and properties of TiNi-based alloys by laser additive manufacturing - Google Patents
A method of using electric pulses to control the precipitation phase and properties of TiNi-based alloys by laser additive manufacturing Download PDFInfo
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Abstract
一种利用电脉冲调控激光增材制造TiNi基合金析出相和性能的方法,包括如下步骤:将激光增材制造的TiNi基合金两端夹持电极,通入脉冲电流,通过调节不同工艺参数,如电流和时间,在不改变晶粒尺寸的情况下,快速调控析出相分布,并可以实现局部加热,最终达到改善材料性能的目的;本发明工艺简单可控,具有实施快速、操作简便、适用范围广等特点,尤其适用于制备梯度功能材料。
A method for using electric pulses to control the precipitation phase and properties of TiNi-based alloys manufactured by laser additive materials, comprising the following steps: clamping electrodes at both ends of the TiNi-based alloys manufactured by laser additive materials, feeding pulse currents, and adjusting different process parameters, Such as current and time, without changing the grain size, the precipitation phase distribution can be quickly regulated, local heating can be achieved, and finally the purpose of improving the material properties can be achieved; Wide range and other characteristics, especially suitable for the preparation of gradient functional materials.
Description
技术领域technical field
本发明属于金属材料技术领域,涉及一种电脉冲调控激光增材制造合金析出相和性能的方法。The invention belongs to the technical field of metal materials, and relates to a method for controlling the precipitation phase and properties of an alloy by means of an electric pulse regulating laser additive manufacturing.
背景技术Background technique
TiNi基合金由于其特有的形状记忆效应和超弹性在航空航天和生物医学领域具有广泛的应用。传统的制备工艺如锻造、铸造等只能获得具有简单几何形状的合金,这极大地制约了TiNi合金的应用范围。激光增材制造是解决这一问题的有效手段之一,该技术可以通过计算机模拟CAD模型,直接构建出复杂结构的构件。TiNi-based alloys have a wide range of applications in aerospace and biomedicine due to their unique shape memory effect and superelasticity. Traditional preparation processes such as forging and casting can only obtain alloys with simple geometric shapes, which greatly restricts the application range of TiNi alloys. Laser additive manufacturing is one of the effective means to solve this problem. This technology can directly construct components of complex structures through computer simulation of CAD models.
激光增材制造TiNi基合金研究尚处于起步阶段,仍然面临诸多亟待解决的问题,如重复率低,缺陷较多,各向异性较明显,微观结构不均匀等。因此调控合金的微观组织,对于提高合金的性能至关重要。目前大部分研究集中在调整合金的制备工艺参数或传统的热处理等方法。虽然传统热处理工艺对合金的微观组织和性能有明显改进,但是所需要时间长,步骤复杂,包括固溶、时效等多个步骤,甚至加热时间较长会引起过热现象等。电流脉冲处理只需对试样通入脉冲电流,可以在较短时间内达到较高的温度。电脉冲处理通过热效应与非热效应耦合作用,对合金的晶粒、析出物等进行调控,改善合金性能。此外,由于电脉冲处理可以在局部进行,可以根据需求设计合金的微观组织,从而获得非匀质的梯度材料。The research on laser additive manufacturing of TiNi-based alloys is still in its infancy, and there are still many problems to be solved, such as low repetition rate, many defects, obvious anisotropy, and uneven microstructure. Therefore, controlling the microstructure of the alloy is very important to improve the performance of the alloy. Most of the current research focuses on adjusting the parameters of the alloy's preparation process or traditional heat treatment methods. Although the traditional heat treatment process can significantly improve the microstructure and properties of the alloy, it takes a long time and the steps are complex, including multiple steps such as solid solution and aging, and even a long heating time will cause overheating and so on. The current pulse treatment only needs to pass a pulse current to the sample, which can reach a higher temperature in a short time. The electric pulse treatment controls the grains and precipitates of the alloy through the coupling of thermal effect and non-thermal effect, and improves the properties of the alloy. In addition, since the electrical pulse treatment can be performed locally, the microstructure of the alloy can be designed according to requirements, thereby obtaining a heterogeneous gradient material.
发明内容SUMMARY OF THE INVENTION
本发明目的在于提供一种利用电脉冲处理调控激光增材制造合金析出相和性能的方法,电流脉冲技术是一种瞬时高能的处理方式,输入脉冲电流的过程中,电子风力与热效应耦合作用,加速构件的相变过程,可快速调控析出相分布,重构微观组织,且工艺简单可控。The purpose of the present invention is to provide a method for controlling the precipitation phase and properties of an alloy manufactured by laser additive manufacturing by using electric pulse treatment. The current pulse technology is an instantaneous high-energy treatment method. Accelerating the phase transformation process of the component can quickly control the distribution of the precipitation phase, reconstruct the microstructure, and the process is simple and controllable.
针对传统热处理在合金微观组织调控中存的不足,本发明提供了一种利用脉冲电流快速调控激光增材制造TiNi基合金析出相分布的工艺。采用本发明所述技术方案,在适当的工艺参数下,不仅可以调控合金的析出相,提升材料的综合力学性能,并且可以获得梯度功能材料。Aiming at the deficiencies of traditional heat treatment in the control of alloy microstructure, the present invention provides a process for rapidly regulating and controlling the distribution of precipitation phase of TiNi-based alloy manufactured by laser additive material by using pulse current. By adopting the technical solution of the present invention, under appropriate process parameters, not only can the precipitation phase of the alloy be regulated, the comprehensive mechanical properties of the material can be improved, but also gradient functional materials can be obtained.
本发明的目的是通过以下技术方案实现的:The purpose of this invention is to realize through the following technical solutions:
一种利用电脉冲调控激光增材制造合金析出相和性能的方法,具体步骤如下:A method for using electric pulses to regulate and control the precipitation phase and properties of an alloy by laser additive manufacturing, the specific steps are as follows:
(1)制备构件:通过激光增材制造制备TiNi合金,将初始沉积态材料进行超声清洗。(1) Preparation of components: TiNi alloys are prepared by laser additive manufacturing, and the initially deposited materials are ultrasonically cleaned.
(2)打磨构件表面,焊接温度测量用热电偶,将夹具两头夹持在构件两端约0.5cm处,通入脉冲电流。(2) Grind the surface of the component, weld a thermocouple for temperature measurement, clamp both ends of the fixture at about 0.5cm at both ends of the component, and apply a pulse current.
(3)设置参数,通过调节时间、电流等参数调控处理效果,一段时间后关闭电流,冷却至室温后取下合金构件。(3) Set parameters, adjust the treatment effect by adjusting time, current and other parameters, turn off the current after a period of time, and remove the alloy components after cooling to room temperature.
本发明中,所述通入电流时间为5-30s,通入电流为270-570A。In the present invention, the current passing time is 5-30s, and the passing current is 270-570A.
本发明中,所述激光增材制造包括激光选区熔化、激光直接沉积技术和选区激光烧结。In the present invention, the laser additive manufacturing includes laser selective melting, laser direct deposition technology and selective laser sintering.
本发明中,所述合金为含有Ti3Ni4析出相的TiNi合金,或含有TiCu析出相的TiNiCu合金,或含有H相的TiNiHf基合金。In the present invention, the alloy is a TiNi alloy containing a Ti 3 Ni 4 precipitation phase, or a TiNiCu alloy containing a TiCu precipitation phase, or a TiNiHf-based alloy containing an H phase.
本发明中,所述合金是在保护气氛下,通过激光增材制造技术制备。In the present invention, the alloy is prepared by a laser additive manufacturing technology under a protective atmosphere.
本发明中,所述电脉冲设备为高能脉冲电源,通过调节参数可以在外接示波器观测电流情况。In the present invention, the electrical pulse device is a high-energy pulse power supply, and current conditions can be observed on an external oscilloscope by adjusting parameters.
本发明中,所述构件点焊温度测量点,可以实时监测温度变化。In the present invention, the spot welding temperature measurement point of the component can monitor the temperature change in real time.
本发明中,电脉冲处理是在室温条件、无保护气体条件下进行的。In the present invention, the electric pulse treatment is carried out at room temperature without protective gas.
本发明中,电脉冲电流方向垂直于构件沉积方向。In the present invention, the direction of the electric pulse current is perpendicular to the deposition direction of the component.
本发明中,构件截面的温度被认为是均匀的。In the present invention, the temperature of the cross section of the member is considered to be uniform.
本发明中,工艺不仅适用于激光增材制造TiNi二元合金,而且适用于其他含有析出相的TiNi基多元合金,如TiNiCu、TiNiHf、TiNiHfPd等合金。In the present invention, the process is not only applicable to laser additive manufacturing of TiNi binary alloys, but also applicable to other TiNi-based multi-element alloys containing precipitation phases, such as TiNiCu, TiNiHf, TiNiHfPd and other alloys.
本发明的优点在于:The advantages of the present invention are:
(1)通过简单可控的工艺,即主要通过直接对激光增材制造的TiNi基合金进行电脉冲,进行瞬时高效的微观组织调控。(1) Through a simple and controllable process, that is, mainly by directly applying electrical pulses to the TiNi-based alloys fabricated by laser additive manufacturing, instantaneous and efficient microstructure control is performed.
(2)经电脉冲处理的样品,合金析出相具有明显的变化,析出相会出现回溶和再析出的现象。根据电流脉冲参数设置的不同,析出相的大小、分布形式均有所不同,且这种不同是可控的。电流脉冲是一种快速加热的过程,通常这种外部提供的能量会转化为焦耳热,在金属材料中,电子激发转到热的耗散非常快,升温速率很高。电脉冲的快速加热过程将在动态热膨胀前产生温升的非同步变化。因此形成了瞬态热应力,有利于原子的扩散。焦耳热引起的热效应在很短的时间内以纳秒量级结束,电子和原子之间周期性的剧烈碰撞力可以提供非热效应。电脉冲过程中的相变可以可归因于脉冲电流引起的第二相相变势垒的降低。电脉冲可以促进第二相的析出,提高其体积分数。在电脉冲通过过程中,高速漂移电子对原子产生强大的冲击力。合金析出相的体积百分比会因高频的周期性性冲击而增加,进而导致原子进入高能状态。原子与相邻原子断开键并跳过能垒所需的最小能量减少。原子扩散的活化能随原子跃迁能垒的减小而减小。因此通过电流脉冲可以达到在不改变其他微观组织状态的情况下,只对析出相分布的调控。由于本技术可以实现局部加热,因而可以更容易地获得梯度功能材料。(2) For the samples treated by electric pulse, the alloy precipitation phase has obvious changes, and the precipitation phase will appear back-dissolution and re-precipitation. According to the different settings of the current pulse parameters, the size and distribution of the precipitates are different, and this difference is controllable. The current pulse is a rapid heating process. Usually this externally provided energy is converted into Joule heat. In metallic materials, the dissipation of electron excitation to heat is very fast and the heating rate is very high. The rapid heating process of the electrical pulse will produce an asynchronous change in temperature rise before dynamic thermal expansion. Therefore, a transient thermal stress is formed, which is conducive to the diffusion of atoms. The thermal effect caused by Joule heating ends in nanoseconds in a very short time, and the periodic violent collision force between electrons and atoms can provide non-thermal effects. The phase transition during the electrical pulse can be attributed to the lowering of the barrier to the second phase transition induced by the pulsed current. Electric pulses can promote the precipitation of the second phase and increase its volume fraction. During the passage of the electric pulse, the high-speed drifting electrons produce a powerful impact on the atoms. The volume percentage of the alloy precipitates increases due to periodic shocks at high frequencies, which in turn cause the atoms to enter a high-energy state. The minimum energy required for an atom to break bonds with neighboring atoms and jump over the energy barrier is reduced. The activation energy of atomic diffusion decreases as the atomic transition energy barrier decreases. Therefore, only the precipitation phase distribution can be regulated by the current pulse without changing other microstructural states. Gradient functional materials can be more easily obtained due to the localized heating that can be achieved with the present technology.
附图说明Description of drawings
图1沉积态和不同脉冲电流参数处理后激光增材制造TiNi合金的显微硬度;Fig.1 Microhardness of laser additively fabricated TiNi alloy as deposited and treated with different pulse current parameters;
图2激光增材制造TiNi合金的显微组织;Fig. 2 Microstructure of TiNi alloy fabricated by laser additive manufacturing;
图3分别为经过272A(a)和477A(b)电脉冲处理后激光增材制造TiNi合金的显微组织。Figure 3 shows the microstructures of laser additively fabricated TiNi alloys after 272A (a) and 477A (b) electrical pulse treatments, respectively.
具体实施方式Detailed ways
下面结合实施例与附图对本发明的技术方案作进一步介绍的说明。本发明技术方案不局限于下列技术方案,此处所描述的具体实施例仅用于解释本发明而非限定。对本发明进行修改或替换而不脱离本发明精神的,均涵盖在本发明的保护范围中。The technical solutions of the present invention will be further described below with reference to the embodiments and the accompanying drawings. The technical solutions of the present invention are not limited to the following technical solutions, and the specific embodiments described herein are only used to explain the present invention and not limit it. Modifications or substitutions of the present invention without departing from the spirit of the present invention are all included in the protection scope of the present invention.
实施例1Example 1
以激光选区熔化TiNi合金为例,利用电脉冲调控激光增材制造TiNi合金析出相与性能的方法,包括如下步骤:Taking laser selective melting of TiNi alloy as an example, the method of using electric pulses to control the precipitation phase and properties of TiNi alloy by laser additive manufacturing includes the following steps:
(1)利用激光选区熔化制备TiNi合金构件。利用线切割切下构建,超声清洗表面,去除表面上黏附的金属粉末。(1) Preparation of TiNi alloy components by laser selective melting. The build is cut by wire cutting, and the surface is ultrasonically cleaned to remove the metal powder adhering to the surface.
(2)将上述构件氧化皮与切割痕打磨去掉,便于焊接温度测量点。(2) Grind and remove the oxide scale and cutting marks of the above components, so as to facilitate the welding temperature measurement point.
(3)将上述构件放置于脉冲电流发生装置中,通过纯铜夹具固定,保证两个电极处于一条直线上,且与构件完全接触,再用铜导线接入脉冲电源两端。(3) The above components are placed in the pulse current generating device, and fixed by pure copper clamps to ensure that the two electrodes are in a straight line and are in complete contact with the components, and then copper wires are connected to both ends of the pulse power supply.
(4)设置参数,对上述构件分别施加272A、330A、376A、420A、477A、528A、575A的电流。通电开始7s后,切断电源,待冷却到室温后,将构件取下。(4) Set parameters, and apply currents of 272A, 330A, 376A, 420A, 477A, 528A, and 575A to the above components, respectively. 7s after the start of power-on, cut off the power supply, and remove the component after cooling to room temperature.
(5)测试上述构件的力学性能及微观组织。(5) Test the mechanical properties and microstructure of the above components.
图1为沉积态及不同参数电脉冲处理后的构件的显微硬度。从图中可以看到,电脉冲处理后硬度比沉积态显著增高,在420A时,显微硬度到达最大值。Figure 1 shows the microhardness of the components in the as-deposited state and after electric pulse treatment with different parameters. It can be seen from the figure that the hardness after electric pulse treatment is significantly higher than that of the as-deposited state, and the microhardness reaches the maximum value at 420A.
图2为沉积态合金的透射电子显微相,在图中可以看到呈透镜状的Ti3Ni4相,长度大约为几十到一百纳米,宽度为10nm左右。Figure 2 shows the transmission electron microphase of the as-deposited alloy. In the figure, a lenticular Ti 3 Ni 4 phase can be seen, with a length of about tens to one hundred nanometers and a width of about 10 nm.
图3(a),(b)分别为经过脉冲电流272A和477A处理后合金的透射电子显微像。在电流为272A时,Ti3Ni4析出相尺寸明显减小,呈椭球状,长度减少至20nm左右,宽度约为几纳米。电流为477A时,Ti3Ni4析出相尺寸更小,呈现出弥散分布的点状。Figure 3(a), (b) are the transmission electron micrographs of the alloys treated with pulse current 272A and 477A, respectively. When the current is 272A, the size of the Ti 3 Ni 4 precipitates is obviously reduced, and it is ellipsoid, the length is reduced to about 20 nm, and the width is about a few nanometers. When the current is 477A, the size of the Ti 3 Ni 4 precipitates is smaller, showing the dispersed distribution of dots.
施加脉冲电流后,析出相的分布由脉冲电流和热效应的共同作用,与热处理相比,脉冲电流可以瞬时快速地调控微观组织。After the pulse current is applied, the distribution of the precipitates is caused by the combined action of the pulse current and the thermal effect. Compared with the heat treatment, the pulse current can control the microstructure instantaneously and rapidly.
由于合金两端夹具材料为纯铜,散热较快,根据检测的温度曲线,中间产生了更高的温度,因此主要关注的为脉冲电流处理的合金中心高温部分内的组织变化和析出相分布。Since the material of the clamps at both ends of the alloy is pure copper, the heat dissipation is fast, and according to the detected temperature curve, a higher temperature is generated in the middle, so the main concern is the microstructure change and the distribution of precipitation in the high temperature part of the alloy center treated by pulse current.
由于本发明中的技术方法通过电效应和热效应的共同作用,可以在较短时间内达成析出相调控的目的,同时由于其可以局部加热的特点,更适于做梯度材料。相比于传统的热处理方法,本发明消耗时间、能源更少,效率更高。Because the technical method in the present invention can achieve the purpose of regulating and controlling the precipitation phase in a relatively short time through the combined action of the electrical effect and the thermal effect, and at the same time, it is more suitable for the gradient material due to the characteristic of local heating. Compared with the traditional heat treatment method, the present invention consumes less time and energy and has higher efficiency.
实施例2:Example 2:
本实施例与例1的区别在于步骤一中采用激光熔化沉积制备TiNi合金。The difference between this example and Example 1 is that in step 1, the TiNi alloy is prepared by laser melting deposition.
实施例3:Example 3:
本实施例与例1的区别在于步骤一种采用选区激光烧结制备TiNi合金。The difference between this example and Example 1 is that in step one, selective laser sintering is used to prepare TiNi alloy.
实施例4:Example 4:
本实施例与例1的区别在于选用含有H析出相的TiNiHf基合金进行电脉冲处理。The difference between this example and Example 1 is that a TiNiHf-based alloy containing H precipitation is selected for electric pulse treatment.
实施例5:Example 5:
本实施例与例1的区别在于选用含有TiCu析出相的TiNiCu合金进行电脉冲处理。The difference between this example and Example 1 is that a TiNiCu alloy containing a TiCu precipitation phase is selected for electric pulse treatment.
一种利用电脉冲调控激光增材制造TiNi基合金析出相和性能的方法,包括如下步骤:将激光增材制造的TiNi基合金两端夹持电极,通入脉冲电流。通过调节不同工艺参数,如电流和时间,在不改变晶粒尺寸的情况下,快速调控析出相分布,并可以实现局部加热,最终达到改善材料性能的目的。本发明工艺简单可控,具有实施快速、操作简便、适用范围广等特点,尤其适用于制备梯度功能材料。A method for controlling the precipitation phase and properties of a TiNi-based alloy manufactured by laser additive manufacturing by means of electric pulses comprises the following steps: clamping electrodes at both ends of the TiNi-based alloy manufactured by laser additive manufacturing, and feeding a pulse current. By adjusting different process parameters, such as current and time, the precipitation phase distribution can be rapidly regulated without changing the grain size, and local heating can be achieved, ultimately achieving the purpose of improving the material properties. The process of the invention is simple and controllable, and has the characteristics of fast implementation, simple operation, wide application range and the like, and is especially suitable for preparing gradient functional materials.
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