CN100561175C - Method for Measuring Phase Transformation Properties of Shape Memory Alloys with Spherical Indenter - Google Patents
Method for Measuring Phase Transformation Properties of Shape Memory Alloys with Spherical Indenter Download PDFInfo
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Abstract
本发明公开了一种球形压头测量形状记忆合金(SMAs)相变特性的方法。它是利用球形压头压入形状记忆合金材料表面,使其发生应力诱发的相变,并通过传感器同时检测加卸载过程中的载荷和位移信号,得到载荷F-位移ht曲线,然后根据分析将试验获取的载荷-位移曲线转化为对应的名义应力σm-名义应变εm曲线,进而得到SMAs的相变应力和弹性模量等性能。该测试方法简单易行,可基本实现对材料的无损测量,不仅广泛适用于各种超弹和形状记忆SMAs相变特性的测量,而且特别适用于厚度低至数微米的SMAs薄膜或典型结构尺寸在微米量级的SMAs微器件相变特性的测试,测量值准确,精度高,能为SMAs在微机电系统的应用提供可靠的相变特性测试依据。
The invention discloses a method for measuring the phase transition characteristics of shape memory alloys (SMAs) with a spherical indenter. It uses a spherical indenter to press into the surface of the shape memory alloy material to cause a stress-induced phase transition, and simultaneously detects the load and displacement signals during the loading and unloading process through the sensor to obtain the load F-displacement ht curve, and then according to the analysis The load-displacement curve obtained from the test is converted into the corresponding nominal stress σ m - nominal strain ε m curve, and then the phase transformation stress and elastic modulus of SMAs are obtained. The test method is simple and easy, and can basically realize the non-destructive measurement of materials. It is not only widely applicable to the measurement of the phase transition characteristics of various hyperelastic and shape memory SMAs, but also especially suitable for SMAs films with a thickness as low as several microns or typical structural dimensions. The test of the phase change characteristics of SMAs micro-devices at the micron level has accurate measurement values and high precision, which can provide a reliable test basis for the phase change characteristics of SMAs in the application of micro-electromechanical systems.
Description
技术领域 technical field
本发明属于形状记忆合金材料机械性能测试技术领域。The invention belongs to the technical field of mechanical performance testing of shape memory alloy materials.
背景技术 Background technique
形状记忆合金(Shape Memory Alloys,简写SMAs)在不同温度下可表现出独特的形状记忆特性或者超弹特性。结合其高的功率密度(单位体积的输出功率)、大的输出力和输出位移等突出优点,SMAs已成为研制微机电系统驱动器和传感器的理想材料。在各种SMAs中,镍钛合金(NiTi)是实用化程度最高的形状记忆合金,其功密度高达2.5×107J/m3,比其它类型微驱动材料高两个数量级。高功率密度材料研制出的驱动器,输出功率不变但结构尺寸更小,或者结构尺寸不变但输出功率更大。Shape memory alloys (Shape Memory Alloys, SMAs for short) can exhibit unique shape memory properties or superelastic properties at different temperatures. Combined with its outstanding advantages such as high power density (output power per unit volume), large output force and output displacement, SMAs have become ideal materials for the development of MEMS drivers and sensors. Among various SMAs, nickel-titanium alloy (NiTi) is the most practical shape memory alloy, and its work density is as high as 2.5×10 7 J/m 3 , which is two orders of magnitude higher than other types of micro-actuation materials. The driver developed with high power density materials has the same output power but smaller structural size, or the same structural size but higher output power.
对镍钛合金(NiTi)微驱动器的研究已有20余年历史,已研制出微阀、微开关、微机器臂以及微泵等各种装置。由于上述NiTi微驱动器元件主要利用马氏体相变来完成微驱动的位移或应力驱动功能,NiTi合金的弹性模量和相变应力等特性就成为了决定微驱动器元件性能的主要参量。因此,在使用NiTi合金作为微驱动器元件时,首先必须明确元件的弹性模量和相变应力等性能,从而为NiTi合金微驱动器元件的设计和使用提供参考依据。然而,在这些微驱动器中,镍钛合金元件多为厚度仅几个微米的纳米多晶薄膜或典型结构尺寸在微米量级的微构件,无法用传统的拉伸试验方法来测试其弹性模量和相变应力等关键的相变特性,因而亟需开发出一种可测试镍钛合金及其他各种SMAs薄膜和SMAs微器件相变特性的测试方法。The research on nickel-titanium alloy (NiTi) micro-actuator has a history of more than 20 years, and various devices such as micro-valve, micro-switch, micro-machine arm and micro-pump have been developed. Since the above-mentioned NiTi micro-actuator components mainly use martensitic phase transformation to complete the displacement or stress driving function of the micro-drive, the elastic modulus and phase transformation stress of the NiTi alloy become the main parameters that determine the performance of the micro-drive components. Therefore, when using NiTi alloy as a micro-actuator element, the elastic modulus and phase transformation stress of the element must first be clarified, so as to provide a reference for the design and use of NiTi alloy micro-actuator elements. However, in these micro-actuators, the nickel-titanium alloy components are mostly nano-polycrystalline films with a thickness of only a few microns or micro-components with a typical structural size on the order of microns, and the traditional tensile test method cannot be used to test their elastic modulus. Therefore, there is an urgent need to develop a test method that can test the phase transition properties of nickel-titanium alloys and other various SMAs thin films and SMAs micro-devices.
如附图1的形状记忆合金进行单向拉伸实验时的拉伸应力σ-应变ε曲线示意图所示:不同于传统的材料,镍钛合金等形状记忆合金在单向拉伸或者压缩过程中会先后经历马氏体相变和马氏体屈服两个变形的应力平台,分别对应马氏体相变应力σt和马氏体屈服应力σn。因此,尽管基于Berkovich压头的纳米压痕法已被广泛应用于测量弹性或弹塑性材料的硬度和弹性模量,然而,由于SMAs变形过程中相变变形和塑性变形的耦合,无法用常规的Berkovich压痕技术来测量SMAs的相变特性:如图2所示,由于Berkovich压头的形状为尖端曲率半径很小的三棱锥形,在很小的载荷条件下,压痕区中心区域就会诱发马氏体屈服变形,并同时在边缘区域诱发马氏体相变变形。为此,所测得的硬度将是马氏体相变应力σt和马氏体屈服应力σn的综合反映,由于无法确知接触区中马氏体屈服区域的大小,也就无法进一步分析得到SMAs的马氏体相变应力等相变特性。As shown in the schematic diagram of the tensile stress σ-strain ε curve of the shape memory alloy in the uniaxial tensile test in Figure 1: different from traditional materials, shape memory alloys such as nickel-titanium alloys undergo uniaxial tension or compression It will successively experience two stress platforms of martensitic transformation and martensitic yield, corresponding to martensitic transformation stress σ t and martensitic yield stress σ n respectively. Therefore, although the nanoindentation method based on the Berkovich indenter has been widely used to measure the hardness and elastic modulus of elastic or elastoplastic materials, however, due to the coupling of phase change deformation and plastic deformation during the deformation of SMAs, it cannot be used with conventional Berkovich indentation technology to measure the phase transition characteristics of SMAs: as shown in Figure 2, since the shape of the Berkovich indenter is a triangular pyramid with a small radius of curvature at the tip, under a small load condition, the central area of the indentation area will be Induce martensitic yield deformation, and at the same time induce martensitic transformation deformation in the edge region. Therefore, the measured hardness will be a comprehensive reflection of the martensitic transformation stress σ t and the martensitic yield stress σ n . Since the size of the martensitic yield area in the contact zone cannot be determined, further analysis cannot be done. The transformation characteristics such as the martensitic transformation stress of SMAs are obtained.
发明内容 Contents of the invention
本发明的目的是提供一种球形压头测量形状记忆合金相变特性的方法,该种方法能对各种形状记忆合金的相变特性进行测量,尤其适合于形状记忆合金薄膜和形状记忆合金微器件相变特性的测试。The purpose of the present invention is to provide a method for measuring the phase transition characteristics of shape memory alloys with a spherical indenter, which can measure the phase transition characteristics of various shape memory alloys, and is especially suitable for shape memory alloy thin films and shape memory alloy microstructures. Testing of phase transition characteristics of devices.
本发明为解决其发明目的所采用的技术方案是:一种球形压头测量形状记忆合金相变特性的方法,其步骤是:The technical scheme that the present invention adopts for solving the object of the invention is: a kind of spherical indenter measures the method for the phase change characteristic of shape memory alloy, and its steps are:
a、利用压痕设备,采用球形压头径向压入形状记忆合金材料表面,使其发生应力诱发的相变,并通过传感器同时检测加载和卸载过程中的载荷F和位移ht信号,得到形状记忆合金的载荷F-位移ht曲线;a. Using indentation equipment, a spherical indenter is used to press radially into the surface of the shape memory alloy material to cause a stress-induced phase transition, and the sensor simultaneously detects the load F and displacement h t signals in the loading and unloading process, and obtains Load F-displacement h t curve of shape memory alloy;
b、采用不同的峰值载荷,重复a步的步骤,得到不同峰值载荷下形状记忆合金的载荷F-位移ht曲线,这些载荷F-位移ht曲线的初始卸载斜率即为相应载荷下接触副的接触刚度S,从而拟合出接触刚度S随载荷F变化的曲线;b. Using different peak loads, repeat step a to obtain the load F-displacement ht curves of the shape memory alloy under different peak loads. The initial unloading slope of these load F-displacement ht curves is the contact pair under the corresponding load The contact stiffness S of , so as to fit the curve of the contact stiffness S changing with the load F;
c、在b步测量得到的形状记忆合金载荷F-位移ht曲线中,选定任意一条加载段和卸载段不重叠的载荷F-位移ht曲线,计算该选定曲线对应的加载和卸载过程中压痕接触区内的平均压力和代表性应变,分别定义为名义应力σm和名义应变εm,其计算过程为:先计算接触半径ac,
d、根据c步计算得出的名义应力σm和名义应变εm,得到待测形状记忆合金的名义应力σm-名义应变εm曲线;对于超弹状态的待测形状记忆合金,该名义应力σm-名义应变εm曲线加载段相变应力平台开始处的应力σf即对应待测形状记忆合金的正向相变应力,卸载段的回复应力平台结束处的应力σr即对应待测形状记忆合金的反向相变应力;对于形状记忆状态的待测形状记忆合金,该名义应力σm-名义应变εm曲线加载段相变应力平台开始处的应力σf即对应待测形状记忆合金的相变应力。d. According to the nominal stress σm and nominal strain εm calculated in step c, the nominal stress σm -nominal strain εm curve of the shape memory alloy to be tested is obtained; for the shape memory alloy to be tested in the hyperelastic state, the nominal The stress σ f at the beginning of the phase transition stress plateau in the loading section of the stress σ m - nominal strain ε m curve corresponds to the forward phase transition stress of the shape memory alloy to be tested, and the stress σ r at the end of the recovery stress plateau in the unloading section corresponds to the Measure the reverse phase transition stress of the shape memory alloy; for the shape memory alloy to be tested in the shape memory state, the stress σ f at the beginning of the phase transition stress plateau in the loading section of the nominal stress σ m - nominal strain ε m curve corresponds to the shape to be measured Phase transformation stress of memory alloy.
与现有技术相比,本发明的有益效果是:Compared with prior art, the beneficial effect of the present invention is:
一、常规的Berkovich尖椎形压头由于尖端曲率半径小,在压入过程中无法分离出相变变形和塑性变形的耦合,也即无法检测出仅有相变变形的相应载荷F-位移ht曲线,从而不能测试形状记忆合金的相变特性。不同于常规的Berkovich尖椎形压头,本发明的球形压头由于压头尖端曲率半径大,在能够施加并能测量的较小载荷下,它能仅在接触区内诱发形状记忆合金的马氏体相变变形,而在较大载荷下,才进一步诱发形状记忆合金的马氏体塑性变形。因此,它通过传感器检测到的加卸载过程中的载荷和位移数据中,有仅发生马氏体相变变形过程的载荷和相应的位移,从而能根据分析将试验获取的载荷F-位移ht曲线转化为对应的名义应力σm-名义应变εm曲线,进而得到形状记忆合金的相变应力。因此,本发明的测量方法能广泛适用于各种形状记忆合金相变特性的测量。特别是对于采用拉伸方法无法进行测试的形状记忆合金薄膜(厚度低至数微米)或形状记忆合金微器件(典型结构尺寸在微米量级),尤其适合采用本发明的方法,能达到现有测试方法所不能达到的测试效果和精度,数据的重现性好,能为SMAs在微机电系统的应用提供可靠的试验依据。1. Due to the small curvature radius of the tip of the conventional Berkovich cone-shaped indenter, it is impossible to separate the coupling of phase transformation deformation and plastic deformation during the indentation process, that is, it is impossible to detect the corresponding load F-displacement h of only phase transformation deformation t curve, so the phase transformation characteristics of shape memory alloys cannot be tested. Different from the conventional Berkovich cone-shaped indenter, the spherical indenter of the present invention has a large radius of curvature at the tip of the indenter, and it can induce the deformation of the shape memory alloy only in the contact area under a small load that can be applied and measured. The martensitic transformation deformation of the shape memory alloy is further induced under a larger load. Therefore, among the load and displacement data in the loading and unloading process detected by the sensor, there are loads and corresponding displacements that only occur in the martensitic transformation deformation process, so that the load F-displacement h t obtained from the test can be analyzed according to the analysis The curve is converted into the corresponding nominal stress σ m - nominal strain ε m curve, and then the phase transformation stress of the shape memory alloy is obtained. Therefore, the measurement method of the invention can be widely applied to the measurement of the phase transition characteristics of various shape memory alloys. Especially for shape memory alloy films (thickness as low as several microns) or shape memory alloy microdevices (typical structural size in micron order) that cannot be tested by stretching method, it is especially suitable to adopt the method of the present invention, which can reach the existing The test effect and accuracy that the test method cannot achieve, and the reproducibility of the data are good, which can provide a reliable test basis for the application of SMAs in micro-electromechanical systems.
二、操作简单、方便,可在多台压痕设备上实现。仅需在压痕设备安装球形压头,对待测SMAs进行径向施压,同时检测加载及卸载过程中相应的载荷和位移信号,然后对数据进行分析计算即可。2. The operation is simple and convenient, and it can be realized on multiple indentation equipment. It is only necessary to install a spherical indenter on the indentation equipment, apply radial pressure on the SMAs to be tested, and simultaneously detect the corresponding load and displacement signals during the loading and unloading process, and then analyze and calculate the data.
三、试验区域小,对待测材料的损害小。仅在待测实验区中形成曲率半径大的球形凹陷,而较之拉伸实验对整个材料产生均匀变形、Berkovich压头产生集中的尖椎形凹陷,能够避免测试对材料造成的破坏,可基本实现对材料的无损测量。3. The test area is small, and the damage to the material to be tested is small. Only a spherical depression with a large radius of curvature is formed in the test area to be tested. Compared with the uniform deformation of the entire material in the tensile test and the concentrated pointed cone-shaped depression produced by the Berkovich indenter, it can avoid the damage caused by the test to the material, and can basically Realize non-destructive measurement of materials.
上述的d步得出待测形状记忆合金的相变应力后,还可以进一步计算得出形状记忆合金的弹性模量Em,
下面结合附图和具体实施方式对本发明作进一步详细的描述。The present invention will be further described in detail below in conjunction with the accompanying drawings and specific embodiments.
附图说明 Description of drawings
图1是形状记忆合金进行单向拉伸实验时的拉伸应力σ-应变ε曲线示意图。Fig. 1 is a schematic diagram of a tensile stress σ-strain ε curve when a shape memory alloy is subjected to a uniaxial tensile test.
图2是Berkovich压头压入形状记忆合金时的接触区示意图。Fig. 2 is a schematic diagram of the contact area when the Berkovich indenter presses into the shape memory alloy.
图3是本发明方法测试时,球形压头压入形状记忆合金材料的示意图。Fig. 3 is a schematic diagram of a spherical indenter pressing into a shape memory alloy material when the method of the present invention is tested.
图4是用本发明方法对长宽均为10mm、厚度为0.5mm的两个形状记忆镍钛合金多晶薄片样品进行测试,其中一个样品处于超弹状态SE,另一个样品处于形状记忆状态SME,从而分别得到同样形状的超弹状态的形状记忆合金样品SE和形状记忆状态的形状记忆合金样品SME的载荷F-位移ht曲线。Fig. 4 is to use the method of the present invention to test two shape-memory nickel-titanium alloy polycrystalline sheet samples whose length and width are 10mm and thickness 0.5mm, wherein one sample is in the superelastic state SE, and the other sample is in the shape-memory state SME , so that the load F-displacement h t curves of the shape memory alloy sample SE in the superelastic state and the shape memory alloy sample SME in the shape memory state of the same shape are respectively obtained.
图5是本发明方法是对图4的两个形状记忆合金样品,进行测试分析而分别得到的超弹状态的形状记忆样品SE接触刚度S随载荷F变化的曲线以及形状记忆合金状态的样品SME的接触刚度S随载荷F变化的曲线。Fig. 5 is the curve of the contact stiffness S of the shape memory sample SE in the superelastic state obtained by testing and analyzing the two shape memory alloy samples in Fig. 4 and the sample SME in the state of the shape memory alloy according to the load F. The contact stiffness S varies with the load F curve.
图6中的实线是本发明方法对图4的超弹状态的形状记忆样品SE测试分析得到的其名义应力σm-名义应变εm曲线;虚线为采用现有的拉伸方法测出的同一样品的单向拉伸应力σ-应变ε曲线。The solid line in Fig. 6 is its nominal stress σ m -nominal strain ε m curve obtained by the present invention method to the shape memory sample SE test analysis of hyperelastic state of Fig. 4; Dotted line is that adopts existing stretching method to measure Uniaxial tensile stress σ-strain ε curve of the same sample.
图7中的实线是本发明方法对图4的形状记忆状态的形状记忆合金样品SME,测试分析得到的其名义应力σm-名义应变εm曲线;虚线为采用现有的拉伸方法测出的同一样品SME的单向拉伸应力σ-应变ε曲线。The solid line in Fig. 7 is the shape memory alloy sample SME of the shape memory state of Fig. 4 according to the present invention, and its nominal stress σm -nominal strain εm curve obtained by test and analysis; the dotted line is that adopts existing stretching method to measure The uniaxial tensile stress σ-strain ε curve of the same sample SME is obtained.
图8是本发明方法对图4的两个样品进行测试分析,得到的超弹状态的样品SE和形状记忆状态的样品SME的接触刚度S随接触半径ac变化的曲线,两条曲线的斜率为2Eeff(Eeff为球形压头和SMAs接触的复合弹性模量)。Fig. 8 is the curve that the contact stiffness S of the sample SE of the superelastic state obtained and the sample SME of the shape memory state are changed with the contact radius a c by testing and analyzing the two samples of Fig. 4 by the method of the present invention, the slopes of the two curves is 2E eff (E eff is the complex modulus of elasticity of the contact between the spherical indenter and the SMAs).
具体实施方式 Detailed ways
实施例Example
以长宽均为10mm、厚度为0.5mm的两个镍钛合金多晶薄片作为测试样品,其中一个为超弹状态的样品SE,另一个为形状记忆状态的样品SME。以该两个样品的测试为例,说明本发明方法的具体操作步骤。其步骤是:Two nickel-titanium alloy polycrystalline sheets with a length and width of 10 mm and a thickness of 0.5 mm were used as test samples, one of which was a sample SE in a superelastic state, and the other was a sample SME in a shape memory state. Taking the test of these two samples as an example, the specific operation steps of the method of the present invention are illustrated. The steps are:
a、利用压痕设备,采用球形压头径向压入形状记忆合金材料表面,使其发生应力诱发的相变,并通过传感器同时连续检测加载和卸载过程中的载荷F和位移ht信号,得到形状记忆合金的载荷F-位移ht曲线。图3即为测试时,球形压头压入形状记忆合金材料的示意图,其中R为球形压头的曲率半径,可由扫描电镜表征,本例中压头的曲率半径R=20μm;ac为接触半径,ht为样品受压后产生的位移,hc为压头样品接触边缘与样品凹陷最深处间的垂直距离。a. Using indentation equipment, a spherical indenter is used to radially press the surface of the shape memory alloy material to cause a stress-induced phase transition, and the load F and displacement h t signals during the loading and unloading process are continuously detected by the sensor at the same time, The load F-displacement h t curve of the shape memory alloy is obtained. Figure 3 is a schematic diagram of the spherical indenter pressing into the shape memory alloy material during the test, where R is the radius of curvature of the spherical indenter, which can be characterized by a scanning electron microscope. In this example, the radius of curvature of the indenter R=20 μm; a c is the contact Radius, h t is the displacement of the sample after being pressed, h c is the vertical distance between the contact edge of the indenter sample and the deepest part of the sample depression.
图4为采用峰值载荷为100mN对两个样品分别进行测试,得到的超弹状态的样品SE和形状记忆状态的样品SME的载荷F-位移ht曲线。可见,当压头曲率半径为20μm,试验峰值载荷为100mN时,超弹样品SE的载荷F-位移ht曲线在卸载后基本完全恢复,并在恢复前表现为一个较大滞后环,表明超弹样品SE的合金在发生塑性变形前已经发生了应力诱发的可逆相变。而形状记忆状态的样品SME的合金在试验过程中产生了较大的残余变形,说明其相变变形在卸载后基本没有恢复,具有形状记忆的特性。Figure 4 shows the load F-displacement h t curves of the sample SE in the hyperelastic state and the sample SME in the shape memory state obtained by testing two samples with a peak load of 100 mN. It can be seen that when the radius of curvature of the indenter is 20 μm and the test peak load is 100 mN, the load F-displacement h t curve of the hyperelastic sample SE is basically completely restored after unloading, and shows a large hysteresis loop before recovery, indicating that the hyperelastic sample SE The alloy of the elastic sample SE has undergone a stress-induced reversible phase transformation before undergoing plastic deformation. The SME alloy in the shape memory state produced a large residual deformation during the test, indicating that its phase transformation deformation basically did not recover after unloading, and it has the characteristics of shape memory.
b、采用不同的峰值载荷,重复a步的步骤,得到不同峰值载荷下形状记忆合金的载荷F-位移ht曲线,这些载荷F-位移ht曲线的初始卸载斜率即为相应载荷下接触副的接触刚度S,从而拟合出接触刚度S随载荷F变化的曲线。图5即为测试、拟合出的本例样品的接触刚度S随载荷F变化的曲线。利用这条拟合曲线可方便地得到不同载荷下的接触刚度数值。b. Using different peak loads, repeat step a to obtain the load F-displacement ht curves of the shape memory alloy under different peak loads. The initial unloading slope of these load F-displacement ht curves is the contact pair under the corresponding load The contact stiffness S, so as to fit the curve of the contact stiffness S changing with the load F. Figure 5 is the test and fitting curve of the contact stiffness S of the sample in this example changing with the load F. The contact stiffness values under different loads can be easily obtained by using this fitting curve.
c、在b步测量得到的形状记忆合金载荷F-位移ht曲线中,选定任意一条加载段和卸载段不重叠的载荷F-位移ht曲线。本例在实测中选用峰值载荷为100mN时超弹状态的形状记忆合金样品SE和形状记忆状态的样品SME的载荷F-位移ht曲线,如图4所示。c. From the load F-displacement h t curves of the shape memory alloy measured in step b, select any load F-displacement h t curve in which the loading section and the unloading section do not overlap. In this example, the load F-displacement ht curves of the shape memory alloy sample SE in the superelastic state and the sample SME in the shape memory state when the peak load is 100mN are selected in the actual measurement, as shown in Figure 4.
计算选定的100mN峰值载荷下,压痕接触区在加载及卸载过程中的平均压力和代表性应变,分别定义为名义应力σm和名义应变εm。其计算过程为:先计算接触半径ac,
接触半径ac公式的推导过程为:根据Oliver-Pharr理论,
d、根据c步计算得出的名义应力σm和名义应变εm,得到待测形状记忆合金的名义应力σm-名义应变εm曲线;对于超弹状态的待测形状记忆合金,该名义应力σm-名义应变εm曲线加载段相变应力平台开始处的应力σf即对应待测形状记忆合金的正向相变应力,卸载段的回复应力平台结束处的应力σr即对应待测形状记忆合金的反向相变应力;对于形状记忆状态的待测形状记忆合金,该名义应力σm-名义应变εm曲线加载段相变应力平台开始处的应力σf即对应待测形状记忆合金的相变应力。d. According to the nominal stress σm and nominal strain εm calculated in step c, the nominal stress σm -nominal strain εm curve of the shape memory alloy to be tested is obtained; for the shape memory alloy to be tested in the hyperelastic state, the nominal The stress σ f at the beginning of the phase transition stress plateau in the loading section of the stress σ m - nominal strain ε m curve corresponds to the forward phase transition stress of the shape memory alloy to be tested, and the stress σ r at the end of the recovery stress plateau in the unloading section corresponds to the Measure the reverse phase transition stress of the shape memory alloy; for the shape memory alloy to be tested in the shape memory state, the stress σ f at the beginning of the phase transition stress plateau in the loading section of the nominal stress σ m - nominal strain ε m curve corresponds to the shape to be measured Phase transformation stress of memory alloy.
图6中的实线即为实测出的超弹状态样品SE的名义应力σm-名义应变εm曲线;为了便于本发明方法与拉伸实验方法的比较,同时对该样品SE采用拉伸实验方法测试得到了其单向拉伸应力σ-应变ε曲线,即图6中的虚线。图7中的实线即为实测出的形状记忆状态的样品SME的名义应力σm-名义应变εm曲线;同样为便于比较,也给出了该样品采用拉伸实验方法测试得到的单向拉伸应力σ-应变ε曲线,即图7中的虚线。The solid line in Fig. 6 is the nominal stress σ m -nominal strain ε m curve of the measured hyperelastic state sample SE; in order to facilitate the comparison between the method of the present invention and the tensile test method, the tensile test is adopted for the sample SE at the same time The method test obtained its uniaxial tensile stress σ-strain ε curve, which is the dotted line in Figure 6. The solid line in Figure 7 is the measured nominal stress σ m - nominal strain ε m curve of the sample SME in the shape memory state; also for the convenience of comparison, the unidirectional Tensile stress σ-strain ε curve, namely the dotted line in Fig. 7.
从图6、图7中可以看出,本发明方法得到的名义应力σm-名义应变εm曲线与拉伸试验得到的应力σ-应变ε曲线形状非常一致。在加载过程中,由于应力诱发的马氏体相变,NiTi形状记忆合金分别在图6、图7中的两种应力-应变曲线都出现了应力平台。卸载过程中:图6中由于超弹(SE)NiTi合金的超弹性能,其相变均得到了很好的恢复,而图7中形状记忆(SME)NiTi合金在两种测试方法下,均只有较小的弹性恢复。It can be seen from Fig. 6 and Fig. 7 that the nominal stress σ m -nominal strain ε m curve obtained by the method of the present invention is very consistent with the shape of the stress σ-strain ε curve obtained by the tensile test. During the loading process, due to the stress-induced martensitic transformation, stress plateaus appeared in the two stress-strain curves of NiTi shape memory alloy in Fig. 6 and Fig. 7 respectively. During the unloading process: due to the superelastic properties of the superelastic (SE) NiTi alloy in Figure 6, its phase transformation has been well recovered, while the shape memory (SME) NiTi alloy in Figure 7 has both Only minor elastic recovery.
同拉伸应力σ-应变ε曲线类似,图6和图7中名义应力σm和名义应变εm曲线的平台也反映了镍钛合金在本发明的压痕过程中的相变流动:根据Tabor的理论,相变流动时的名义应力σm约为单向压缩时相变应力的三倍。另外,由于镍钛合金在拉伸和压缩时的各向异性,其压缩时的相变应力约为拉伸时的1.5倍。因此,镍钛合金压缩时相变流动的名义应力σm约为其单向拉伸相变应力σ的4.5倍。Similar to the tensile stress σ-strain ε curve, the platforms of the nominal stress σ m and nominal strain ε m curves in Fig. 6 and Fig. 7 also reflect the phase change flow of nickel-titanium alloy in the indentation process of the present invention: according to Tabor According to the theory of phase change flow, the nominal stress σ m is about three times of the phase change stress in unidirectional compression. In addition, due to the anisotropy of nickel-titanium alloy in tension and compression, the phase transformation stress in compression is about 1.5 times that in tension. Therefore, the nominal stress σ m of phase transition flow of NiTi alloy in compression is about 4.5 times of its uniaxial tensile phase transition stress σ.
图6中超弹状态的样品SE的名义应力σm-名义应变εm曲线加载段相变应力平台开始处的应力σf为1780MPa,对应超弹状态的样品SE压缩时相变流动时的正向相变应力,计算出对应的拉伸相变应力σ为395MPa。该值与图6中单向拉伸试验直接测量(表征)的相变应力σ值370MPa非常接近。图6中名义应力σm-名义应变εm曲线卸载段的回复应力平台结束处的应力σr=666MPa,对应超弹状态的的样品SE回弹时的反向相变应力,计算出对应的拉伸相变应力σ为148MPa,也与图6中的拉伸试验直接测量值137MPa较好地吻合。In Fig. 6, the nominal stress σ m - nominal strain ε m curve of the sample SE in the hyperelastic state, the stress σ f at the beginning of the phase transition stress plateau in the loading section is 1780 MPa, which corresponds to the positive direction of the phase change flow when the sample SE in the hyperelastic state is compressed Phase transition stress, the calculated corresponding tensile phase transition stress σ is 395MPa. This value is very close to the phase transformation stress σ value of 370MPa directly measured (characterized) by the uniaxial tensile test in Fig. 6 . The stress at the end of the recovery stress plateau in the unloading section of the nominal stress σ m -nominal strain ε m curve in Figure 6 is σ r = 666MPa, which corresponds to the reverse phase transition stress of the sample SE in the hyperelastic state when it rebounds, and the corresponding The tensile phase transition stress σ is 148MPa, which is also in good agreement with the direct measurement value of 137MPa in the tensile test in Figure 6.
图7中形状记忆状态的样品SE的名义应力σm-名义应变εm曲线加载段相变应力平台开始处的应力σf为750MPa,对应形状记忆状态的样品SE压缩时相变流动时的相变应力,计算出对应的拉伸相变应力σ为167MPa。该值与图7中单向拉伸试验直接测量(表征)的相变应力σ值162MPa非常接近。The nominal stress σ m -nominal strain ε m curve of the sample SE in the shape memory state in Fig. 7, the stress σ f at the beginning of the phase transition stress plateau in the loading section is 750 MPa, which corresponds to the phase change flow when the sample SE in the shape memory state is compressed The corresponding tensile phase transition stress σ is calculated to be 167MPa. This value is very close to the phase transformation stress σ value of 162 MPa directly measured (characterized) by the uniaxial tensile test in Fig. 7 .
需要说明的是:在b步测量得到的形状记忆合金载荷F-位移ht曲线中,峰值载荷小于其产生马氏体相变的最小载荷时,形状记忆合金将只产生弹性变形,而不产生马氏体相变,其载荷F-位移ht曲线的加载段和卸载段则完全重叠。显然,c、d两步选择没有产生相变的这些测试所得到的载荷F-位移ht曲线进行分析计算,无法得出其相变应力。It should be noted that: in the shape memory alloy load F-displacement h t curve measured in step b, when the peak load is less than the minimum load for martensitic transformation, the shape memory alloy will only produce elastic deformation without For martensitic transformation, the loading section and unloading section of the load F-displacement h t curve overlap completely. Obviously, the load F-displacement h t curves obtained from these tests without phase transition are selected in steps c and d for analysis and calculation, and the phase transition stress cannot be obtained.
而加载段和卸载段不重叠的任意一条载荷F-位移ht曲线,其加载的峰值载荷均大于其产生马氏体相变的最小载荷,测试过程中均发生了马氏体相变,对于超弹状态的形状记忆合金,d步分析得出的名义应力σm-名义应变εm曲线就必然有加载段的相变应力平台和卸载段的回复应力平台,最终对应的正向相变应力为加载段相变应力平台初始处的应力,最终对应的反向相变应力为卸载段回复应力平台结束处的应力。而对于形状记忆状态的形状记忆合金,d步分析得出的名义应力σm-名义应变εm曲线就必然有加载段的相变应力平台,最终对应的相变应力为加载段相变应力平台初始处的应力。因此,选择任意一条加载段和卸载段不重叠的载荷F-位移ht曲线,均可通过c、d两步的步骤得到对应的相变应力,而与具体选择哪一条载荷F-位移ht曲线无关。在加载段和卸载段不重叠的载荷F-位移ht曲线中选择不同的曲线,只是d步的名义应力σm-名义应变εm曲线中,应力平台长短有差别而已(峰值载荷大的名义应力σm-名义应变εm曲线,应力平台更长;相反,应力平台更短)。However, for any load F-displacement h t curve that does not overlap between the loading section and the unloading section, the peak load of the load is greater than the minimum load for martensitic transformation, and martensitic transformation occurs during the test. For a shape memory alloy in a hyperelastic state, the nominal stress σ m -nominal strain ε m curve obtained from the d-step analysis must have a phase transition stress platform in the loading section and a recovery stress platform in the unloading section, and the final corresponding positive phase transition stress is the stress at the beginning of the phase change stress platform in the loading section, and the final corresponding reverse phase transition stress is the stress at the end of the recovery stress platform in the unloading section. For shape memory alloys in the shape memory state, the nominal stress σ m -nominal strain ε m curve obtained from the d-step analysis must have a phase transition stress plateau in the loading section, and the final corresponding phase transition stress is the phase transition stress plateau in the loading section initial stress. Therefore, choosing any load F-displacement h t curve that does not overlap between the loading section and the unloading section, the corresponding phase change stress can be obtained through steps c and d, and which load F-displacement h t curve is selected specifically Curves are irrelevant. Choose different curves in the load F-displacement h t curves that do not overlap between the loading section and the unloading section, but the length of the stress plateau is different in the nominal stress σ m -nominal strain ε m curve of step d (nominal with a large peak load Stress σ m - nominal strain ε m curve, the stress plateau is longer; conversely, the stress plateau is shorter).
本例d步得出待测形状记忆合金的相变应力后,还进一步计算得出形状记忆合金的弹性模量Em,
由于球形压头和SMAs接触的复合弹性模量Eeff与接触刚度S、接触半径ac之间存在如下关系:Eeff=0.5S/ac,其中:
根据以上公式和图8的接触半径-刚度曲线,实测得到本例超弹(SE)和形状记忆(SME)NiTi合金的弹性模量分别为42GPa和48GPa,与拉伸试验得到的41GPa和42GPa基本一致。According to the above formula and the contact radius-stiffness curve in Figure 8, the elastic modulus of the superelastic (SE) and shape memory (SME) NiTi alloys in this example are measured to be 42GPa and 48GPa, respectively, which are basically the same as the 41GPa and 42GPa obtained by the tensile test. unanimous.
综上所述,利用球形压头压入法可以方便地测得形状记忆材料的载荷F-位移ht曲线,并根据分析可将其转化为对应的名义应力σm和-名义应变εm曲线,进而得到形状记忆材料的相变应力和弹性模量等性能。该测试方法简单易行,可基本实现对材料的无损测量,适用于各种形状记忆合金(SMAs)材料在超弹状态下或形状记忆状态下的相变特性测试,而且特别适用于SMAs薄膜或SMAs微器件相变特性的测试与研究。In summary, the load F-displacement h t curve of shape memory materials can be easily measured by using the spherical indenter indentation method, and can be converted into corresponding nominal stress σ m and -nominal strain ε m curves according to the analysis , and then the phase transition stress and elastic modulus of the shape memory material are obtained. The test method is simple and easy, and can basically realize the non-destructive measurement of the material. It is suitable for the phase change characteristics test of various shape memory alloy (SMAs) materials in the superelastic state or shape memory state, and is especially suitable for SMAs thin films or Testing and research on phase transition characteristics of SMAs micro-devices.
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