WO2022110509A1 - Method for determining dislocation slip type - Google Patents

Method for determining dislocation slip type Download PDF

Info

Publication number
WO2022110509A1
WO2022110509A1 PCT/CN2021/000088 CN2021000088W WO2022110509A1 WO 2022110509 A1 WO2022110509 A1 WO 2022110509A1 CN 2021000088 W CN2021000088 W CN 2021000088W WO 2022110509 A1 WO2022110509 A1 WO 2022110509A1
Authority
WO
WIPO (PCT)
Prior art keywords
slip
sample
dislocation
different
type
Prior art date
Application number
PCT/CN2021/000088
Other languages
French (fr)
Chinese (zh)
Inventor
李阁平
张英东
袁福森
韩福洲
穆罕默德•阿里
郭文斌
任杰
刘承泽
顾恒飞
佟敏
Original Assignee
中国科学院金属研究所
Priority date (The priority date is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the date listed.)
Filing date
Publication date
Application filed by 中国科学院金属研究所 filed Critical 中国科学院金属研究所
Publication of WO2022110509A1 publication Critical patent/WO2022110509A1/en

Links

Images

Classifications

    • G—PHYSICS
    • G01—MEASURING; TESTING
    • G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
    • G01N3/00—Investigating strength properties of solid materials by application of mechanical stress
    • G01N3/40—Investigating hardness or rebound hardness
    • G01N3/42—Investigating hardness or rebound hardness by performing impressions under a steady load by indentors, e.g. sphere, pyramid
    • G—PHYSICS
    • G01—MEASURING; TESTING
    • G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
    • G01N23/00—Investigating or analysing materials by the use of wave or particle radiation, e.g. X-rays or neutrons, not covered by groups G01N3/00 – G01N17/00, G01N21/00 or G01N22/00
    • G01N23/20—Investigating or analysing materials by the use of wave or particle radiation, e.g. X-rays or neutrons, not covered by groups G01N3/00 – G01N17/00, G01N21/00 or G01N22/00 by using diffraction of the radiation by the materials, e.g. for investigating crystal structure; by using scattering of the radiation by the materials, e.g. for investigating non-crystalline materials; by using reflection of the radiation by the materials
    • G01N23/20008—Constructional details of analysers, e.g. characterised by X-ray source, detector or optical system; Accessories therefor; Preparing specimens therefor
    • G—PHYSICS
    • G01—MEASURING; TESTING
    • G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
    • G01N23/00—Investigating or analysing materials by the use of wave or particle radiation, e.g. X-rays or neutrons, not covered by groups G01N3/00 – G01N17/00, G01N21/00 or G01N22/00
    • G01N23/20—Investigating or analysing materials by the use of wave or particle radiation, e.g. X-rays or neutrons, not covered by groups G01N3/00 – G01N17/00, G01N21/00 or G01N22/00 by using diffraction of the radiation by the materials, e.g. for investigating crystal structure; by using scattering of the radiation by the materials, e.g. for investigating non-crystalline materials; by using reflection of the radiation by the materials
    • G01N23/20058—Measuring diffraction of electrons, e.g. low energy electron diffraction [LEED] method or reflection high energy electron diffraction [RHEED] method
    • G—PHYSICS
    • G01—MEASURING; TESTING
    • G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
    • G01N23/00—Investigating or analysing materials by the use of wave or particle radiation, e.g. X-rays or neutrons, not covered by groups G01N3/00 – G01N17/00, G01N21/00 or G01N22/00
    • G01N23/20—Investigating or analysing materials by the use of wave or particle radiation, e.g. X-rays or neutrons, not covered by groups G01N3/00 – G01N17/00, G01N21/00 or G01N22/00 by using diffraction of the radiation by the materials, e.g. for investigating crystal structure; by using scattering of the radiation by the materials, e.g. for investigating non-crystalline materials; by using reflection of the radiation by the materials
    • G01N23/20083—Investigating or analysing materials by the use of wave or particle radiation, e.g. X-rays or neutrons, not covered by groups G01N3/00 – G01N17/00, G01N21/00 or G01N22/00 by using diffraction of the radiation by the materials, e.g. for investigating crystal structure; by using scattering of the radiation by the materials, e.g. for investigating non-crystalline materials; by using reflection of the radiation by the materials by using a combination of at least two measurements at least one being a transmission measurement and one a scatter measurement
    • G—PHYSICS
    • G01—MEASURING; TESTING
    • G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
    • G01N23/00—Investigating or analysing materials by the use of wave or particle radiation, e.g. X-rays or neutrons, not covered by groups G01N3/00 – G01N17/00, G01N21/00 or G01N22/00
    • G01N23/20—Investigating or analysing materials by the use of wave or particle radiation, e.g. X-rays or neutrons, not covered by groups G01N3/00 – G01N17/00, G01N21/00 or G01N22/00 by using diffraction of the radiation by the materials, e.g. for investigating crystal structure; by using scattering of the radiation by the materials, e.g. for investigating non-crystalline materials; by using reflection of the radiation by the materials
    • G01N23/203—Measuring back scattering
    • G—PHYSICS
    • G01—MEASURING; TESTING
    • G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
    • G01N23/00—Investigating or analysing materials by the use of wave or particle radiation, e.g. X-rays or neutrons, not covered by groups G01N3/00 – G01N17/00, G01N21/00 or G01N22/00
    • G01N23/22—Investigating or analysing materials by the use of wave or particle radiation, e.g. X-rays or neutrons, not covered by groups G01N3/00 – G01N17/00, G01N21/00 or G01N22/00 by measuring secondary emission from the material
    • G01N23/225—Investigating or analysing materials by the use of wave or particle radiation, e.g. X-rays or neutrons, not covered by groups G01N3/00 – G01N17/00, G01N21/00 or G01N22/00 by measuring secondary emission from the material using electron or ion
    • G01N23/2251—Investigating or analysing materials by the use of wave or particle radiation, e.g. X-rays or neutrons, not covered by groups G01N3/00 – G01N17/00, G01N21/00 or G01N22/00 by measuring secondary emission from the material using electron or ion using incident electron beams, e.g. scanning electron microscopy [SEM]
    • G—PHYSICS
    • G01—MEASURING; TESTING
    • G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
    • G01N3/00—Investigating strength properties of solid materials by application of mechanical stress
    • G01N3/02—Details
    • G01N3/06—Special adaptations of indicating or recording means
    • G—PHYSICS
    • G01—MEASURING; TESTING
    • G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
    • G01N2203/00—Investigating strength properties of solid materials by application of mechanical stress
    • G01N2203/0001—Type of application of the stress
    • G01N2203/0003—Steady
    • G—PHYSICS
    • G01—MEASURING; TESTING
    • G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
    • G01N2203/00—Investigating strength properties of solid materials by application of mechanical stress
    • G01N2203/0014—Type of force applied
    • G01N2203/0016—Tensile or compressive
    • G01N2203/0019—Compressive
    • G—PHYSICS
    • G01—MEASURING; TESTING
    • G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
    • G01N2203/00—Investigating strength properties of solid materials by application of mechanical stress
    • G01N2203/0058—Kind of property studied
    • G01N2203/0069—Fatigue, creep, strain-stress relations or elastic constants
    • G01N2203/0075—Strain-stress relations or elastic constants
    • G—PHYSICS
    • G01—MEASURING; TESTING
    • G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
    • G01N2203/00—Investigating strength properties of solid materials by application of mechanical stress
    • G01N2203/0058—Kind of property studied
    • G01N2203/0076—Hardness, compressibility or resistance to crushing
    • G—PHYSICS
    • G01—MEASURING; TESTING
    • G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
    • G01N2203/00—Investigating strength properties of solid materials by application of mechanical stress
    • G01N2203/0098—Tests specified by its name, e.g. Charpy, Brinnel, Mullen
    • G—PHYSICS
    • G01—MEASURING; TESTING
    • G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
    • G01N2203/00—Investigating strength properties of solid materials by application of mechanical stress
    • G01N2203/02—Details not specific for a particular testing method
    • G01N2203/06—Indicating or recording means; Sensing means
    • G01N2203/0641—Indicating or recording means; Sensing means using optical, X-ray, ultraviolet, infrared or similar detectors
    • G—PHYSICS
    • G01—MEASURING; TESTING
    • G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
    • G01N2203/00—Investigating strength properties of solid materials by application of mechanical stress
    • G01N2203/02—Details not specific for a particular testing method
    • G01N2203/06—Indicating or recording means; Sensing means
    • G01N2203/067—Parameter measured for estimating the property
    • G01N2203/0682—Spatial dimension, e.g. length, area, angle

Definitions

  • the invention belongs to the field of material analysis, in particular to a method for judging the type of dislocation slip through EBSD, Vickers hardness tester, tilt-scanning sample stage and Schmid theory.
  • deformation The deformation of the material when it is under load is called deformation, and the common deformation methods are mainly tension, compression, shear and torsion.
  • the two most common ways of deformation are dislocation slip and twinning.
  • dislocation slip often occurs in the vast majority of deformation processes, and is a particularly important deformation method. Slip in a crystal can only proceed along a certain crystal plane and a certain crystallographic direction on this plane, which we call the slip plane and the slip direction.
  • Common slips include cylinder slip, basal slip and cone slip.
  • dislocation slip is very important to study the formation mechanism of dislocation slip.
  • the most mainstream method for dislocation calibration is to calibrate by transmission, that is, to obtain different double-beam g-vectors by tilting the transmission sample rod, and then realize the calibration of dislocations.
  • this method requires high-end and expensive instruments (transmission electron microscope) to implement, the cost is high, and the popularity is not high.
  • transmission calibration is used, the operation is more complicated, and it is often difficult to calibrate complex dislocations, such as dislocation networks. Therefore, it is currently difficult to find an affordable, simple and convenient method to mark the type of misalignment slip. Therefore, it is very important to find a simple and convenient method to judge the type of dislocation slip.
  • the invention provides a method for judging the type of dislocation slip through EBSD, Vickers hardness tester, tilting scanning sample stage and Schmid theory, which is a simple, effective and accurate method for judging the type of dislocation slip.
  • a method for judging dislocation slip types characterized in that the specific steps are as follows:
  • the EBSD block sample is prepared by chemical light wiping corrosion method and slight mechanical vibration polishing method to ensure the flatness of the sample surface.
  • the preferred preparation method is: first mount the sample on the mounting machine, and then sequentially. Pre-grind with 150#, 320#, 800#, 2000# water sandpaper, after removing the deep scratches, perform mechanical polishing on the woolen cloth, the polishing liquid is SiO 2 nano-suspension, polishing for 6-10 minutes , to obtain a bright and traceless polished surface with a mirror effect; then etch, gently and quickly wipe the surface of the test sample with acid-stained cotton for 3-10 seconds, until the surface of the sample becomes bright; vibrate polishing on an automatic polishing machine , the polishing liquid is SiO 2 nano-suspension, polished for 10 minutes, and finally a bright and traceless polished surface with mirror effect was obtained.
  • the samples were rinsed with water and absolute ethanol in turn, and finally dried and stored.
  • step 2) the region to be measured is preferably marked with Vickers hardness on the surface of the sample, and the crystal orientation of the region is calibrated with EBSD technology.
  • step 3 a Vickers hardness tester is used to test the hardness of different crystal orientations in the region to be measured, and the diagonal size of the indentation and the hardness value are recorded.
  • the weight range of the Vickers hardness tester used is: 10-1000g.
  • different dislocation slip lines are obtained by applying weights of different weights, and at the same time, the propagation of slip lines between different crystal grains is obtained; and the quasi-in situ observation of dislocation slip can be realized by calibrating the crystal orientation function of EBSD.
  • the formation process of the line through the geometric force analysis of Vickers hardness indentation under different loads, the shear stress that forms the slip line is analyzed, and the Schmid factor of different dislocation slip is calculated based on the three-dimensional crystal structure calibrated by EBSD.
  • step 3 combined with the hardness test results, the geometric stress analysis of the indentation and the Schmid factor values at different slip starts, the first preliminary judgment of the dislocation slip types can be made, so as to exclude some dislocation slip types. .
  • the slip line comparison method is: matching and comparing the length direction of the slip line with the basal plane, cylindrical surface and cone surface of the three-dimensional crystal structure, combining the general direction of dislocation slip, the calculated The Schmid factor values of different slip systems and the angle of intersection between slip lines can preliminarily determine the type of dislocation slip.
  • step 5 after preliminarily judging the type of dislocation slip, set the sample rod on the scanning sample stage of the scanning electron microscope, then place the sample on the sample rod, first record the length direction of the slip line, and make the slip line
  • the length direction is perpendicular to the tilting direction of the scanning sample stage;
  • the sample rod is specially made, and its main body is a cylinder (the height is much larger than the radius of the bottom surface), and the lower end of the cylinder is provided with a threaded fastener that matches the scanning sample stage. It is used to install the sample rod on the scanning sample stage.
  • the upper end of the cylinder is provided with a sample stage.
  • the sample stage can be a plane or an inclined surface with a certain inclination. The inclination angle of the inclined surface ranges from -90° to 90°.
  • the tilt angle of the scanning sample stage of the SEM is only: -80 ⁇ 10°.
  • Installing a special sample rod on the scanning sample stage can increase the tilt angle range of the sample; that is, when the sample stage on the upper part of the sample rod is flat, The tilt angle of the sample is: -80 ⁇ 10°; when the sample stage on the upper part of the sample rod is inclined, the tilt direction of the sample can be tilted along the X-Y plane, the Y-Z plane and the X-Z plane or tilted simultaneously, which can increase the tilt of the scanned sample
  • the angle range is -90 ⁇ 90°.
  • the invention can also prepare transmission samples, and realize the determination of different dislocation types by TKD technology combined with dislocations observed by transmission electron microscope, combined with slip line comparison method, and tilted scanning electron microscope sample stage.
  • the inclination direction of the sample can be inclined along the X-Y plane, the Y-Z plane and the X-Z plane or inclined at the same time, which can increase the tilt angle range of the scanned sample (- 90 ⁇ 90°);
  • the determination of different dislocation types can also be realized by combining TKD technology with dislocations observed by transmission electron microscopy, combined with slip line comparison method.
  • ⁇ CRSS is the critical shear stress
  • ⁇ is the loading stress
  • m is the Schmidt factor.
  • Crystals with different orientations have different strengths, that is, their corresponding slip system activations are also different.
  • the easier the slip system is to be activated the larger the corresponding Schmid factor value, that is, the activation of the dislocation-slip system can be predicted by the Schmid factor theory.
  • the tilt angle range of the scanned sample can be increased (-90 ⁇ 90°).
  • ⁇ angle is the inclination of the X-Z plane direction
  • ⁇ angle is the inclination of the X-Y plane
  • ⁇ angle is the inclination of the Y-Z plane
  • Figure 5 is the actual picture of the sample rod with the top inclination of 70°, that is, when the sample is placed on the inclined plane
  • the tilt angles of the sample are: -90 to -60° and -10 to 80°.
  • Fig. 2 Schematic diagram of the change of the slip step when the sample stage is tilted and scanned.
  • Fig. 3 is a solid view of a flat sample rod.
  • Figure 4 is a schematic diagram of the sample rod with different angles of the top inclination.
  • Figure 5 is a solid view of the sample rod with a 70° inclination at the top.
  • Fig. 6 is a schematic diagram of the variation of the width of the slip step by theoretically judging.
  • FIG. 7 Schematic diagram of the principle of the slip line comparison method.
  • Fig. 9 The variation of the width of the slip line step and the theoretical comparison result when the SEM sample stage is tilted.
  • a method for judging the type of dislocation slip the specific steps are as follows:
  • the polishing liquid is SiO 2 nano-suspension, polish for 6-10 minutes to obtain a bright and traceless polished surface with mirror effect; then etch, gently and quickly wipe the surface of the test sample with acid-stained cotton for 3-10 seconds until the sample is The surface becomes brighter; vibration polishing is performed on an automatic polishing machine.
  • the polishing solution is a nano-suspension of SiO 2 , and polishing is performed for 10 minutes. Finally, a bright and trace-free polished surface with a mirror effect is obtained. Rinse the sample with water and anhydrous ethanol in turn. Finally dry and store.
  • the dislocation slip type is preliminarily determined, as shown in Figure 7;
  • the type of dislocation slip of the ⁇ 0001 ⁇ -oriented grains of the ⁇ -region as-quenched Zr-4 alloy was determined by the method described above.
  • Zr-4 alloy (Zr-1.5Sn-0.2Fe-0.1Cr) has very low thermal neutron absorption cross section, good mechanical properties and excellent corrosion resistance, mainly used in pressurized water reactor, boiling water reactor, heavy water reactor fuel cladding material.
  • the EBSD samples were prepared by wire-cutting samples, grinding, chemical light wiping corrosion and slight mechanical vibration polishing.
  • the morphology changes before and after the Vickers hardness indenter was observed by metallography and scanning electron microscope, and the crystal orientation was determined by EBSD and the calculation results of Schmid factor were shown in Figure 8. It can be seen from Figure 8 that the Schmid factor of base slip is greater than that of cone slip and cylinder slip.

Abstract

A method for determining a dislocation slip type, which is specifically as follows: first manufacturing an EBSD block sample, calibrating the crystal orientation by means of EBSD, and using Vickers hardness indenters having different loads to compress, in situ, grains measured by EBSD, wherein because the oriented grains are deformed after the compression deformation, slip lines are formed on the surfaces of the grains; performing hardness testing on different grains of a region to be measured, and in combination with geometric stress analysis for indentation, calculating Schmid factor values when different slip systems are activated; by comparing the slip lines with a three-dimensional crystal structure, in combination with a propagation direction of a dislocation slip line, the calculated Schmid factor values of the different slip systems, and angles formed by mutual intersection between the slip lines, preliminarily determining a slip type; and finally, scanning a sample table by tilting on a scanning electron microscope, recording a change in the width of a slip step during tilting at different angles, obtaining theoretical changes in the width of the step of different slip types in combination with the crystal orientation measured by EBSD, and then compared with the experimental result, comprehensively determining the slip type.

Description

一种判断位错滑移类型的方法A method for judging the type of dislocation slip 技术领域technical field
本发明属于材料分析领域，特别是指一种通过EBSD、维氏硬度计、倾转扫描样品台结合Schmid理论判断位错滑移类型的方法。The invention belongs to the field of material analysis, in particular to a method for judging the type of dislocation slip through EBSD, Vickers hardness tester, tilt-scanning sample stage and Schmid theory.
背景技术Background technique
材料零部件在实际应用之前，往往需要经过不同方式的机械加工(锻造、轧制、挤压以及成形等等)和热处理(淬火、退火等)。而材料在机械加工时就会发生严重的变形。那么在实际应用过程中，为了获得更好的材料力学性能以及更好的加工工艺，我们需要对材料的变形行为进行系统的基础研究。Before material parts are practically used, they often need to undergo different methods of machining (forging, rolling, extrusion, forming, etc.) and heat treatment (quenching, annealing, etc.). The material undergoes severe deformation during machining. Then in the actual application process, in order to obtain better mechanical properties of materials and better processing technology, we need to carry out systematic basic research on the deformation behavior of materials.
材料在承受载荷时发生的变形称为形变，而常见的变形方式主要有拉伸、压缩、剪切以及扭转等。发生变形最常见的2种方式是位错滑移和孪生。其中，位错滑移往往发生于绝大多数的变形过程中，是一种特别重要的变形方式。晶体中的滑移只能沿一定的晶面和该面上一定的晶体学方向进行，我们将其称为滑移面和滑移方向。常见的滑移有柱面滑移、基面滑移以及锥面滑移。The deformation of the material when it is under load is called deformation, and the common deformation methods are mainly tension, compression, shear and torsion. The two most common ways of deformation are dislocation slip and twinning. Among them, dislocation slip often occurs in the vast majority of deformation processes, and is a particularly important deformation method. Slip in a crystal can only proceed along a certain crystal plane and a certain crystallographic direction on this plane, which we call the slip plane and the slip direction. Common slips include cylinder slip, basal slip and cone slip.
位错滑移作为一种特别重要的变形方式，研究位错滑移的形成机制至关重要。在研究位错的形成机理时，我们需要对材料在发生某种变形时，滑移系开动的类型进行标定。目前，最主流的标定位错方法是通过透射进行标定，即通过倾转透射样品杆获得不同的双束g矢量，进而实现对位错的标定。但是该方法需要高端、昂贵的仪器(透射电子显微镜)去实现，成本很高，普及性不高。其次，通过透射标定时，操作较为复杂，往往很难标定出复杂的位错，如位错网。所以目前很难找到一种即实惠，又简单方便的方法去标定位错滑移的类型。因此，寻求一种能够简单方便判断位错滑移类型的方法至关重要。As a particularly important deformation method, dislocation slip is very important to study the formation mechanism of dislocation slip. When studying the formation mechanism of dislocations, we need to calibrate the type of slip system actuation when the material is deformed. At present, the most mainstream method for dislocation calibration is to calibrate by transmission, that is, to obtain different double-beam g-vectors by tilting the transmission sample rod, and then realize the calibration of dislocations. However, this method requires high-end and expensive instruments (transmission electron microscope) to implement, the cost is high, and the popularity is not high. Secondly, when the transmission calibration is used, the operation is more complicated, and it is often difficult to calibrate complex dislocations, such as dislocation networks. Therefore, it is currently difficult to find an affordable, simple and convenient method to mark the type of misalignment slip. Therefore, it is very important to find a simple and convenient method to judge the type of dislocation slip.
发明内容SUMMARY OF THE INVENTION
本发明提供了一种通过EBSD、维氏硬度计、倾转扫描样品台结合Schmid理论判断位错滑移类型的方法，是一种简单、有效、准确地判断位错滑移类型的方法。The invention provides a method for judging the type of dislocation slip through EBSD, Vickers hardness tester, tilting scanning sample stage and Schmid theory, which is a simple, effective and accurate method for judging the type of dislocation slip.
本发明通过以下技术方案获得：The present invention is obtained through the following technical solutions:
一种判断位错滑移类型的方法，其特征在于，具体步骤如下：A method for judging dislocation slip types, characterized in that the specific steps are as follows:
1)、制备EBSD块状样品；1), prepare EBSD block samples;
2)、在样品表面标记要测定的区域，并测定该区域的晶体取向；2), mark the area to be measured on the surface of the sample, and measure the crystal orientation of this area;
3)、对要测定的区域的不同晶粒进行硬度测试，结合压痕的几何应力分析，计算不同滑移开动时的Schmid因子值；3) Carry out the hardness test on different grains in the area to be measured, and calculate the Schmid factor value of different sliding movements in combination with the geometric stress analysis of the indentation;
4)、通过扫描电镜对压痕附近的变形部位进行观察，获得滑移线(滑移迹线)的形貌图；通过滑移线比对法初步判断位错滑移类型；4) Observing the deformed part near the indentation by scanning electron microscope to obtain the topography of the slip line (slip trace); preliminarily judge the type of dislocation slip by the slip line comparison method;
5)、记录滑移线的长度方向，使滑移线长度方向垂直扫描电镜的扫描样品台倾转方向，通过倾转扫描样品台，统计滑移台阶的宽度变化，通过EBSD测定的晶体取向，获得理论上不同滑移类型的台阶宽度变化，然后与实验结果相对比，最终判断出位错滑移类型。5), record the length direction of the slip line, make the length direction of the slip line perpendicular to the tilting direction of the scanning sample stage of the scanning electron microscope, scan the sample stage by tilting, count the width change of the slip step, and measure the crystal orientation by EBSD, The theoretical step width variation of different slip types is obtained, and then compared with the experimental results, the dislocation slip type is finally determined.
作为优选的技术方案：As the preferred technical solution:
步骤1)中，采用化学轻擦拭腐蚀法和轻微的机械振动抛光法制备EBSD块状样品，保证了样品表面的平整度，优选的制备方法为：先把样品在镶样机上镶样，然后依次用150#、320#、800#、2000#的水砂纸预磨，去除较深的划痕后，在洋绒布上进行机械抛光，抛光液为SiO 2的纳米悬浊液，抛光6-10分钟，得到镜面效果的光亮无痕的抛光面；然后进行蚀刻，用沾有酸的棉花轻轻快速擦拭试样品表面3-10秒钟，直至样品表面变亮；在自动抛磨机上进行振动抛光，抛光液为SiO 2的纳米悬浊液，抛光10分钟，最后得到镜面效果的光亮无痕的抛光 面，依次使用清水和无水乙醇冲洗样品，最后干燥保存。 In step 1), the EBSD block sample is prepared by chemical light wiping corrosion method and slight mechanical vibration polishing method to ensure the flatness of the sample surface. The preferred preparation method is: first mount the sample on the mounting machine, and then sequentially. Pre-grind with 150#, 320#, 800#, 2000# water sandpaper, after removing the deep scratches, perform mechanical polishing on the woolen cloth, the polishing liquid is SiO 2 nano-suspension, polishing for 6-10 minutes , to obtain a bright and traceless polished surface with a mirror effect; then etch, gently and quickly wipe the surface of the test sample with acid-stained cotton for 3-10 seconds, until the surface of the sample becomes bright; vibrate polishing on an automatic polishing machine , the polishing liquid is SiO 2 nano-suspension, polished for 10 minutes, and finally a bright and traceless polished surface with mirror effect was obtained. The samples were rinsed with water and absolute ethanol in turn, and finally dried and stored.
步骤2)中，在样品表面优选用维氏硬度标记要测定的区域，用EBSD技术对该区域的晶体取向进行标定。In step 2), the region to be measured is preferably marked with Vickers hardness on the surface of the sample, and the crystal orientation of the region is calibrated with EBSD technology.
步骤3)中，通过维氏硬度计对要测定的区域的不同晶体取向进行硬度测试，记录压痕的对角线大小以及硬度值，所用维氏硬度计的砝码范围为：10-1000g。In step 3), a Vickers hardness tester is used to test the hardness of different crystal orientations in the region to be measured, and the diagonal size of the indentation and the hardness value are recorded. The weight range of the Vickers hardness tester used is: 10-1000g.
本发明通过施加不同重量的砝码来获得不同位错滑移线，同时，获得滑移线在不同晶粒之间的传播；通过EBSD标定晶体取向功能，可以实现准原位观察位错滑移线的形成过程，通过对不同载荷的维氏硬度压痕几何受力分析，分析形成滑移线的剪切应力，结合EBSD标定出的三维晶体结构，计算出不同位错滑移的Schmid因子。In the present invention, different dislocation slip lines are obtained by applying weights of different weights, and at the same time, the propagation of slip lines between different crystal grains is obtained; and the quasi-in situ observation of dislocation slip can be realized by calibrating the crystal orientation function of EBSD. In the formation process of the line, through the geometric force analysis of Vickers hardness indentation under different loads, the shear stress that forms the slip line is analyzed, and the Schmid factor of different dislocation slip is calculated based on the three-dimensional crystal structure calibrated by EBSD.
步骤3)中，结合硬度测试结果、压痕的几何应力分析以及不同滑移开动时的Schmid因子值，可以对位错滑移类型进行第一次的初步判断，从而排除部分位错滑移类型。In step 3), combined with the hardness test results, the geometric stress analysis of the indentation and the Schmid factor values at different slip starts, the first preliminary judgment of the dislocation slip types can be made, so as to exclude some dislocation slip types. .
步骤4)中，所述滑移线比对法为：通过滑移线的长度方向与三维晶体结构的基面、柱面以及锥面进行匹配比对，结合位错滑移大体方向、所计算的不同滑移系的Schmid因子值以及滑移线之间相互交叉的角度，初步判断位错滑移类型。In step 4), the slip line comparison method is: matching and comparing the length direction of the slip line with the basal plane, cylindrical surface and cone surface of the three-dimensional crystal structure, combining the general direction of dislocation slip, the calculated The Schmid factor values of different slip systems and the angle of intersection between slip lines can preliminarily determine the type of dislocation slip.
步骤5)中，在初步判断位错滑移类型后，将样品杆设置于扫描电镜的扫描样品台上，然后将样品放置于样品杆上，先记录滑移线的长度方向，使滑移线长度方向垂直扫描样品台倾转方向；所述样品杆为特制的，其主体部分为圆柱体(高度远大于底面半径)，该圆柱体下端设有与扫描样品台相配合的螺纹紧固件，用于将样品杆安装在扫描样品台上，圆柱体上端设有样品台，该样品台可为平面状或具有一定倾斜度的斜面，该斜面的倾斜角度范围是-90～90°。In step 5), after preliminarily judging the type of dislocation slip, set the sample rod on the scanning sample stage of the scanning electron microscope, then place the sample on the sample rod, first record the length direction of the slip line, and make the slip line The length direction is perpendicular to the tilting direction of the scanning sample stage; the sample rod is specially made, and its main body is a cylinder (the height is much larger than the radius of the bottom surface), and the lower end of the cylinder is provided with a threaded fastener that matches the scanning sample stage. It is used to install the sample rod on the scanning sample stage. The upper end of the cylinder is provided with a sample stage. The sample stage can be a plane or an inclined surface with a certain inclination. The inclination angle of the inclined surface ranges from -90° to 90°.
扫描电镜的扫描样品台其倾转角度仅为：-80～10°，在扫描样品台上安装特制样品杆，可以增加样品的倾转角度范围；即当样品杆上部样品台为平面状时，样品的倾转角度为：-80～10°；当样品杆上部样品台为斜面时，样品的倾斜方向可以沿着X-Y平面、Y-Z平面以及X-Z平面倾斜或者同时倾斜，能够增加扫描样品的倾转角度范围至-90～90°。The tilt angle of the scanning sample stage of the SEM is only: -80~10°. Installing a special sample rod on the scanning sample stage can increase the tilt angle range of the sample; that is, when the sample stage on the upper part of the sample rod is flat, The tilt angle of the sample is: -80 ~ 10°; when the sample stage on the upper part of the sample rod is inclined, the tilt direction of the sample can be tilted along the X-Y plane, the Y-Z plane and the X-Z plane or tilted simultaneously, which can increase the tilt of the scanned sample The angle range is -90～90°.
本发明还可以制备透射样品，并通过TKD技术结合透射电镜观察的位错，结合滑移线比对法，倾转扫描电镜样品台实现对不同位错类型的判定。The invention can also prepare transmission samples, and realize the determination of different dislocation types by TKD technology combined with dislocations observed by transmission electron microscope, combined with slip line comparison method, and tilted scanning electron microscope sample stage.
本发明的特点如下所示：The characteristics of the present invention are as follows:
1、通过EBSD、维氏硬度计结合Schmid理论判断位错滑移类型的方法，维氏硬度计的砝码范围为：10-1000g，通过施加不同重量的砝码来获得不同位错滑移迹线，同时，能够获得滑移线在不同晶粒之间的传播；1. The method of judging the type of dislocation slip by EBSD, Vickers hardness tester combined with Schmid theory, the weight range of Vickers hardness tester is: 10-1000g, and different dislocation slip traces can be obtained by applying weights of different weights line, and at the same time, the propagation of slip lines between different grains can be obtained;
2、通过EBSD标定晶体取向功能，可以实现准原位观察位错滑移线的形成过程，通过维氏硬度压痕几何受力分析，分析形成滑移线的剪切应力，结合EBSD标定出的三维晶体结构，计算出位错滑移的Schmid因子；2. The function of calibrating the crystal orientation by EBSD can realize the quasi-in-situ observation of the formation process of the dislocation slip line. Through the geometric force analysis of Vickers hardness indentation, the shear stress forming the slip line can be analyzed. 3D crystal structure, calculated Schmid factor for dislocation slip;
3、通过位错滑移线的传播方向，结合维氏硬度形成的应力方向，大体判断位错滑移的方向；3. Through the propagation direction of the dislocation slip line, combined with the stress direction formed by the Vickers hardness, the direction of dislocation slip can be roughly judged;
4、通过滑移线的长度方向与三维晶体结构的基面、柱面以及锥面进行匹配比对，结合位错滑移大体方向，所计算的不同滑移系的Schmid因子值以及滑移线之间相互交叉的角度，初步判断位错滑移类型；4. By matching and comparing the length direction of the slip line with the basal plane, cylindrical plane and cone plane of the three-dimensional crystal structure, combined with the general direction of dislocation slip, the calculated Schmid factor values and slip lines of different slip systems The angle of intersection between them is used to preliminarily determine the type of dislocation slip;
5、放置样品时，先记录滑移线的长度方向，使滑移线长度方向垂直扫描样品台倾转方向，记录不同倾转角度时，滑移台阶的宽度变化；5. When placing the sample, first record the length direction of the slip line, make the length direction of the slip line vertically scan the tilting direction of the sample stage, and record the width change of the slip step at different tilt angles;
6、通过设置具有不同倾斜度(-90～90°)的样品杆，使样品倾斜方向可以沿着X-Y平面、Y-Z平面以及X-Z平面倾斜或者同时倾斜，能够增加扫描样品 的倾转角度范围(-90～90°)；6. By setting the sample rods with different inclinations (-90~90°), the inclination direction of the sample can be inclined along the X-Y plane, the Y-Z plane and the X-Z plane or inclined at the same time, which can increase the tilt angle range of the scanned sample (- 90～90°);
7、通过倾转扫描样品台，统计滑移台阶的宽度变化，通过EBSD测定的晶体取向，获得理论上不同滑移类型的台阶宽度变化，然后与实验结果相对比，最终判断出位错滑移类型；7. Scan the sample stage by tilting, count the width changes of the slip steps, and obtain the theoretical step width changes of different slip types through the crystal orientation determined by EBSD, and then compare with the experimental results to finally judge the dislocation slip. type;
8、基于本发明所述方法，还可以通过TKD技术结合透射电镜观察的位错，结合滑移线比对法，实现对不同位错类型的判定。8. Based on the method of the present invention, the determination of different dislocation types can also be realized by combining TKD technology with dislocations observed by transmission electron microscopy, combined with slip line comparison method.
相关技术原理：Related technical principles:
通过维氏硬度压痕的几何受力分析原理如图1所示：The principle of geometric force analysis through Vickers hardness indentation is shown in Figure 1:
从图1可知：维氏硬度压头为136°，当载荷P加于其上时，垂直于压头棱锥体侧表面的压力为P n，即P n＝Psin(136°/2)。那么棱锥体压入金属的表面积为：A＝d^2/(2sin(136°/2))，即压头所导致的压力为σ HV＝P n/A。维氏硬度的计算公式为：HV＝2Psin(136°/2)/d^2。综上，可得维氏硬度与应力的相互关系推导公式：σ HV＝0.9272HV。 It can be seen from Figure 1 that the Vickers hardness indenter is 136°, when the load P is applied to it, the pressure perpendicular to the pyramidal side surface of the indenter is Pn , that is, Pn =Psin(136°/2). Then the surface area of the pyramid pressed into the metal is: A=d^2/(2sin(136°/2)), that is, the pressure caused by the indenter is σ HV =P n /A. The calculation formula of Vickers hardness is: HV=2Psin(136°/2)/d^2. To sum up, the derivation formula of the relationship between Vickers hardness and stress can be obtained: σ HV =0.9272HV.
Schmid因子理论：Schmid factor theory:
当滑移面上沿滑移方向的切应力达到临界分切应力值τ CRSS时，滑移就发生了，即如公式(1)所示： When the shear stress along the slip direction on the slip surface reaches the critical shear stress value τ CRSS , slip occurs, as shown in formula (1):
τ CRSS＝σm    (1) τ CRSS = σm (1)
式中τ CRSS为临界剪切应力；σ为加载应力；m为施密特因数。不同取向的晶体的强度不同，即其对应的滑移系开动情况也不同。此外，滑移系越容易开动，其对应的Schmid因子值越大，即可以通过Schmid因子理论来预判位错滑移系的开动情况。 where τ CRSS is the critical shear stress; σ is the loading stress; m is the Schmidt factor. Crystals with different orientations have different strengths, that is, their corresponding slip system activations are also different. In addition, the easier the slip system is to be activated, the larger the corresponding Schmid factor value, that is, the activation of the dislocation-slip system can be predicted by the Schmid factor theory.
倾转扫描样品台时滑移台阶变化的原理如图2所示：The principle of the change of the slip step when the sample stage is tilted and scanned is shown in Figure 2:
放置样品时，先记录滑移线的长度方向，使滑移线长度方向垂直扫描样品 台倾转方向，记录不同角度时，滑移台阶的宽度变化。When placing the sample, first record the length direction of the slip line, make the length direction of the slip line perpendicular to the tilting direction of the sample stage, and record the change of the width of the slip step at different angles.
通过在扫描样品台上安装样品杆，可以增加扫描样品的倾转角度范围(-90～90°)，平面状样品杆如图3所示，倾斜度为不同角度的样品杆示意图如图4所示(β角为X-Z平面方向的倾斜，γ角为X-Y平面的倾斜，σ角为Y-Z平面的倾斜)，图5为顶部倾斜度为70°的样品杆实物图，即当样品放在倾斜度为70°的样品杆时，其样品的倾转角度为：-90～-60°和-10～80°。By installing the sample rod on the scanning sample stage, the tilt angle range of the scanned sample can be increased (-90~90°). (β angle is the inclination of the X-Z plane direction, γ angle is the inclination of the X-Y plane, and σ angle is the inclination of the Y-Z plane), Figure 5 is the actual picture of the sample rod with the top inclination of 70°, that is, when the sample is placed on the inclined plane When the sample holder is 70°, the tilt angles of the sample are: -90 to -60° and -10 to 80°.
理论判断滑移台阶宽度变化方法的原理：Theoretical judgment of the principle of the method for changing the width of the slip step:
已知晶体取向，那么可以理论上判断出该晶体内部不同滑移线形成时的台阶宽度变化，如{0001}取向晶粒的基面滑移台阶宽度变化如图6所示。{0001}取向的晶粒的基面滑移，当样品旋转角度为0°时，观察到的台阶为一条直线，随着旋转角度β的增大，台阶宽度也增大，当倾转到90°时，台阶的宽度为最大，那么可以获得基面滑移时，台阶宽度变化的理论变化趋势。Knowing the crystal orientation, it is possible to theoretically determine the variation of the step width when different slip lines are formed inside the crystal. The basal plane slip of {0001} oriented grains, when the sample rotation angle is 0°, the observed step is a straight line, with the increase of the rotation angle β, the step width also increases. When °, the width of the step is the largest, then the theoretical variation trend of the step width change when the base surface slips can be obtained.
附图说明Description of drawings
为了更清楚地说明本发明的技术方案，下面将对本申请中所需要使用的附图作简单地介绍。In order to illustrate the technical solutions of the present invention more clearly, the following briefly introduces the accompanying drawings used in this application.
图1通过维氏硬度压痕几何受力分析原理。Figure 1. Principle of geometric force analysis through Vickers hardness indentation.
图2倾转扫描样品台时滑移台阶变化的原理示意图。Fig. 2 Schematic diagram of the change of the slip step when the sample stage is tilted and scanned.
图3顶部为平面状的样品杆实体图。The top of Fig. 3 is a solid view of a flat sample rod.
图4顶部倾斜度为不同角度的样品杆示意图。Figure 4 is a schematic diagram of the sample rod with different angles of the top inclination.
图5顶部倾斜度为70°的样品杆实体图。Figure 5 is a solid view of the sample rod with a 70° inclination at the top.
图6通过理论判断滑移台阶宽度变化示意图。Fig. 6 is a schematic diagram of the variation of the width of the slip step by theoretically judging.
图7滑移线比对法原理示意图。Figure 7 Schematic diagram of the principle of the slip line comparison method.
图8 Zr-4合金原位维氏硬度压缩前后金相、扫描形貌和EBSD测定的晶体取向图。Fig.8 Metallographic, scanning morphologies and crystallographic orientations of Zr-4 alloy before and after compression with in-situ Vickers hardness.
图9倾转扫描电镜样品台时，滑移线台阶的宽度变化与理论对比结果。Fig. 9 The variation of the width of the slip line step and the theoretical comparison result when the SEM sample stage is tilted.
具体实施方式Detailed ways
为使本发明实施例的目的、技术方案和优点更加清楚，下面将对本发明实施例中的技术方案进行清楚、完整地描述。实施例中未注明具体条件者，按照常规条件或制造商建议的条件进行。In order to make the objectives, technical solutions and advantages of the embodiments of the present invention clearer, the technical solutions in the embodiments of the present invention will be described clearly and completely below. If the specific conditions are not indicated in the examples, it is carried out according to the conventional conditions or the conditions suggested by the manufacturer.
实施例1Example 1
一种判断位错滑移类型的方法，具体步骤如下：A method for judging the type of dislocation slip, the specific steps are as follows:
1)、制备EBSD块状样品(保证样品的平整度)：1), prepare EBSD block samples (to ensure the flatness of the samples):
先把样品在镶样机上镶样，然后依次用150#、320#、800#、2000#的水砂纸预磨，去除较深的划痕后，在洋绒布上进行机械抛光，抛光液为SiO 2的纳米悬浊液，抛光6-10分钟，得到镜面效果的光亮无痕的抛光面；然后进行蚀刻，用沾有酸的棉花轻轻快速擦拭试样品表面3-10秒钟，直至样品表面变亮；在自动抛磨机上进行振动抛光，抛光液为SiO 2的纳米悬浊液，抛光10分钟，最后得到镜面效果的光亮无痕的抛光面，依次使用清水和无水乙醇冲洗样品，最后干燥保存。 First mount the sample on the mounting machine, and then pre-grind it with 150#, 320#, 800#, 2000# water sandpaper in turn, remove the deep scratches, and perform mechanical polishing on the woolen cloth. The polishing liquid is SiO 2 nano-suspension, polish for 6-10 minutes to obtain a bright and traceless polished surface with mirror effect; then etch, gently and quickly wipe the surface of the test sample with acid-stained cotton for 3-10 seconds until the sample is The surface becomes brighter; vibration polishing is performed on an automatic polishing machine. The polishing solution is a nano-suspension of SiO 2 , and polishing is performed for 10 minutes. Finally, a bright and trace-free polished surface with a mirror effect is obtained. Rinse the sample with water and anhydrous ethanol in turn. Finally dry and store.
2)、通过金相显微镜观察块状样品表面，并用维氏硬度标记试样表面某一要测定的位置，用EBSD技术对该区域的晶体取向进行标定；2) Observe the surface of the bulk sample through a metallographic microscope, mark a certain position on the surface of the sample to be measured with Vickers hardness, and use EBSD technology to demarcate the crystal orientation of this area;
3)、通过维氏硬度计(载荷：10-1000g)对该区域已知的晶体取向进行硬度测定(记录压痕的对角线大小以及硬度值)，结合维氏压痕的几何应力分析，计算不同滑移开动时的Schmid因子值；3) Carry out hardness measurement (record the diagonal size of the indentation and the hardness value) with a Vickers hardness tester (load: 10-1000g) for the known crystal orientation in this area, combined with the geometric stress analysis of the Vickers indentation, Calculate the Schmid factor value for different slip starts;
4)、通过扫描电镜对维氏硬度压痕附近的变形部位进行观察，获得滑移线 的形貌图；通过滑移线的长度方向与三维晶体结构的基面、柱面以及锥面进行匹配比对，结合位错滑移线的传播方向，所计算的不同滑移系的Schmid因子值以及滑移线之间相互交叉的角度，初步判断位错滑移类型，如图7所示；4) Observing the deformed part near the Vickers hardness indentation by scanning electron microscope to obtain the topography of the slip line; the length direction of the slip line is matched with the basal plane, cylindrical surface and cone surface of the three-dimensional crystal structure By comparison, combined with the propagation direction of the dislocation slip line, the calculated Schmid factor values of different slip systems, and the angle of intersection between the slip lines, the dislocation slip type is preliminarily determined, as shown in Figure 7;
5)、将样品杆设置于扫描电镜的扫描样品台上，然后将样品放置于样品杆上，先记录滑移线的长度方向，使滑移线长度方向垂直扫描电镜的扫描样品台倾转方向，通过倾转扫描样品台，统计滑移台阶的宽度变化，通过EBSD测定的晶体取向，获得理论上不同滑移类型的台阶宽度变化，然后与实验结果相对比，最终判断位错滑移类型。5) Set the sample rod on the scanning sample stage of the SEM, then place the sample on the sample rod, record the length direction of the slip line first, and make the length direction of the slip line perpendicular to the tilt direction of the scanning sample stage of the SEM , by tilting and scanning the sample stage, counting the width changes of the slip steps, and obtaining the theoretical step width changes of different slip types through the crystal orientation determined by EBSD, and then comparing with the experimental results to finally determine the dislocation slip type.
下述的实施例2是在实施例1的基础上具体展开实施的，特此说明。The following embodiment 2 is specifically developed and implemented on the basis of the embodiment 1, and is hereby described.
实施例2Example 2
通过以上描述的方法对β相区淬火态的Zr-4合金的{0001}取向的晶粒的位错滑移类型进行判定。The type of dislocation slip of the {0001}-oriented grains of the β-region as-quenched Zr-4 alloy was determined by the method described above.
Zr-4合金(Zr-1.5Sn-0.2Fe-0.1Cr)具有非常低的热中子吸收截面，良好的力学性能和优良的耐腐蚀性，主要用于压水堆，沸水堆，重水堆中的燃料包壳材料。Zr-4 alloy (Zr-1.5Sn-0.2Fe-0.1Cr) has very low thermal neutron absorption cross section, good mechanical properties and excellent corrosion resistance, mainly used in pressurized water reactor, boiling water reactor, heavy water reactor fuel cladding material.
首先通过线切割样品、研磨，化学轻微擦拭腐蚀和轻微的机械振动抛光等过程后制备出EBSD样品。其次，通过金相、扫描电子显微镜观察维氏硬度压头压入前后的形貌变化，EBSD测定晶体取向以及Schmid因子计算结果，如图8所示。从图8可以看出，基面滑移的Schmid因子大于锥面滑移大于柱面滑移，由于锥面的临界剪切应力很大以及柱面滑移的Schmid因子较小，所以基面滑移更容易开启；然后，结合滑移线的增值方向、维氏硬度压痕的受力方向、滑移方向和不同滑移线的交角(120°)综合判断，初步判断该滑移为基面滑移；并且通过倾转扫描样品台发现，滑移线台阶的宽度随着倾转角α增大而减小，与理 论的基面滑移台阶宽度变化相一致，最终判断该滑移类型为基面滑移，如图9。First, the EBSD samples were prepared by wire-cutting samples, grinding, chemical light wiping corrosion and slight mechanical vibration polishing. Secondly, the morphology changes before and after the Vickers hardness indenter was observed by metallography and scanning electron microscope, and the crystal orientation was determined by EBSD and the calculation results of Schmid factor were shown in Figure 8. It can be seen from Figure 8 that the Schmid factor of base slip is greater than that of cone slip and cylinder slip. Because the critical shear stress of cone is large and the Schmid factor of cylinder slip is small, base slip Then, combined with the increment direction of the slip line, the force direction of the Vickers hardness indentation, the slip direction and the intersection angle (120°) of different slip lines, it is preliminarily judged that the slip is the base surface And by tilting and scanning the sample stage, it is found that the width of the slip line step decreases with the increase of the tilt angle α, which is consistent with the variation of the theoretical base plane slip step width. surface slip, as shown in Figure 9.
本发明未尽事宜为公知技术。Matters not addressed in the present invention are known in the art.
上述实施例只为说明本发明的技术构思及特点，其目的在于让熟悉此项技术的人士能够了解本发明的内容并据以实施，并不能以此限制本发明的保护范围。凡根据本发明精神实质所作的等效变化或修饰，都应涵盖在本发明的保护范围之内。The above-mentioned embodiments are only intended to illustrate the technical concept and characteristics of the present invention, and the purpose thereof is to enable those who are familiar with the art to understand the content of the present invention and implement them accordingly, and cannot limit the protection scope of the present invention. All equivalent changes or modifications made according to the spirit of the present invention should be included within the protection scope of the present invention.

Claims (8)

  1. 一种判断位错滑移类型的方法，其特征在于，具体步骤如下：A method for judging dislocation slip types, characterized in that the specific steps are as follows:
    1)、制备EBSD块状样品；1), prepare EBSD block samples;
    2)、在样品表面标记要测定的区域，并测定该区域的晶体取向；2), mark the area to be measured on the surface of the sample, and measure the crystal orientation of this area;
    3)、对要测定的区域的不同晶粒进行硬度测试，结合维氏压痕的几何应力分析，计算不同滑移开动时的Schmid因子值；3) Carry out the hardness test on different grains in the area to be measured, and calculate the Schmid factor value of different slip starts in combination with the geometric stress analysis of Vickers indentation;
    4)、通过扫描电镜对压痕附近的变形部位进行观察，获得滑移线的形貌图；通过滑移线比对法初步判断位错滑移类型；4) Observing the deformed part near the indentation by scanning electron microscope to obtain the topography of the slip line; preliminarily judge the type of dislocation slip by the slip line comparison method;
    5)、记录滑移线的长度方向，使滑移线长度方向垂直扫描样品台倾转方向，通过倾转扫描样品台，统计滑移台阶的宽度变化，通过EBSD测定的晶体取向，获得理论上不同滑移类型的台阶宽度变化，然后与实验结果相对比，最终判断出位错滑移类型。5), record the length direction of the slip line, make the length direction of the slip line vertically scan the tilting direction of the sample stage, scan the sample stage by tilting, count the width change of the slip step, and obtain the theoretical crystal orientation determined by EBSD. The step widths of different slip types are changed, and then compared with the experimental results to finally determine the dislocation slip type.
  2. 按照权利要求1所述判断位错滑移类型的方法，其特征在于：步骤1)中，EBSD块状样品的制备方法为：先把样品在镶样机上镶样，然后依次用150#、320#、800#、2000#的水砂纸预磨，去除较深的划痕后，在洋绒布上进行机械抛光，抛光液为SiO 2的纳米悬浊液，抛光6-10分钟，得到镜面效果的光亮无痕的抛光面；然后进行蚀刻，用沾有酸的棉花擦拭试样品表面3-10秒钟，直至样品表面变亮；在自动抛磨机上进行振动抛光，抛光液为SiO 2的纳米悬浊液，抛光10分钟，最后得到镜面效果的光亮无痕的抛光面，依次使用清水和无水乙醇冲洗样品，最后干燥保存。 According to the method for judging the type of dislocation slip according to claim 1, it is characterized in that: in step 1), the preparation method of the EBSD bulk sample is: first mount the sample on a mounting machine, and then use 150#, 320 #, 800#, 2000# water sandpaper pre-grinding, after removing deep scratches, perform mechanical polishing on velvet cloth, polishing liquid is SiO 2 nano-suspension, polishing for 6-10 minutes, to get mirror effect Bright and scratch-free polished surface; then etch, wipe the surface of the test sample with acid-stained cotton for 3-10 seconds, until the surface of the sample becomes bright; perform vibration polishing on an automatic polishing machine, and the polishing solution is nanometer SiO 2 The suspension liquid was polished for 10 minutes, and finally a bright and traceless polished surface with a mirror effect was obtained. The samples were rinsed with water and absolute ethanol in turn, and finally dried and stored.
  3. 按照权利要求1所述判断位错滑移类型的方法，其特征在于：步骤2)中，在样品表面用维氏硬度标记要测定的区域，并用EBSD测定该区域的晶体取向。The method for judging the type of dislocation slip according to claim 1, characterized in that: in step 2), the region to be measured is marked with Vickers hardness on the surface of the sample, and the crystal orientation of the region is measured with EBSD.
  4. 按照权利要求1所述判断位错滑移类型的方法，其特征在于：步骤3) 中，通过维氏硬度计对要测定的区域的不同晶体取向进行硬度测试，记录压痕的对角线大小以及硬度值，所用维氏硬度计的砝码范围为：10-1000g。The method for judging the type of dislocation slip according to claim 1, characterized in that: in step 3), hardness testing is performed on different crystal orientations of the region to be measured by a Vickers hardness tester, and the diagonal size of the indentation is recorded. As well as the hardness value, the weight range of the Vickers hardness tester used is: 10-1000g.
  5. 按照权利要求1所述判断位错滑移类型的方法，其特征在于：步骤3)中，结合硬度测试结果、压痕的几何应力分析以及不同滑移开动时的Schmid因子值，对位错滑移类型进行第一次的初步判断，从而排除部分位错滑移类型。According to the method for judging the type of dislocation slip according to claim 1, it is characterized in that: in step 3), in combination with the hardness test result, the geometric stress analysis of the indentation and the Schmid factor value when different slip starts, the dislocation slip The first preliminary judgment is made on the slip type, so as to exclude some dislocation slip types.
  6. 按照权利要求1所述判断位错滑移类型的方法，其特征在于：步骤4)中，所述滑移线比对法为：通过滑移线的长度方向与三维晶体结构的基面、柱面以及锥面进行匹配比对，结合位错滑移线的传播方向、所计算的不同滑移系的Schmid因子值以及滑移线之间相互交叉的角度，初步判断位错滑移类型。According to the method for judging the type of dislocation slip according to claim 1, it is characterized in that: in step 4), the slip line comparison method is: by comparing the length direction of the slip line with the basal plane and column of the three-dimensional crystal structure The dislocation slip line is preliminarily judged based on the propagation direction of the dislocation slip line, the calculated Schmid factor value of different slip systems, and the cross angle between the slip lines.
  7. 按照权利要求1所述判断位错滑移类型的方法，其特征在于：步骤5)中，在初步判断位错滑移类型后，将样品杆设置于扫描电镜的扫描样品台上，然后将样品放置于样品杆上，先记录滑移线的长度方向，使滑移线长度方向垂直扫描样品台倾转方向；所述样品杆的主体部分为圆柱体，该圆柱体下端设有与扫描样品台相配合的螺纹紧固件，圆柱体上端设有样品台，该样品台可为平面状或具有一定倾斜度的斜面。According to the method for judging the type of dislocation slip according to claim 1, it is characterized in that: in step 5), after preliminarily judging the type of dislocation slip, the sample rod is set on the scanning sample stage of the scanning electron microscope, and then the sample Place it on the sample rod, first record the length direction of the slip line, so that the length direction of the slip line is perpendicular to the tilting direction of the scanning sample stage; the main part of the sample rod is a cylinder, and the lower end of the cylinder is provided with the scanning sample stage. The upper end of the cylindrical body is provided with a sample stage for the matched threaded fastener, and the sample stage can be a plane shape or an inclined surface with a certain inclination.
  8. 按照权利要求7所述判断位错滑移类型的方法，其特征在于：所述样品台为不同角度的斜面时，可以增加扫描样品的倾转角度范围，使样品的倾斜角度范围是-90～90°，倾斜方向可以沿着X-Y平面和Y-Z以及X-Z平面倾斜或者同时倾斜。The method for judging the type of dislocation slip according to claim 7, wherein when the sample stage is inclined with different angles, the tilt angle range of the scanned sample can be increased, so that the tilt angle range of the sample is -90～ 90°, the tilt direction can be tilted along the X-Y plane and the Y-Z and X-Z planes or both.
PCT/CN2021/000088 2020-11-30 2021-04-14 Method for determining dislocation slip type WO2022110509A1 (en)

Applications Claiming Priority (2)

Application Number Priority Date Filing Date Title
CN202011370476.6A CN112611661B (en) 2020-11-30 2020-11-30 Method for judging dislocation slippage type
CN202011370476.6 2020-11-30

Publications (1)

Publication Number Publication Date
WO2022110509A1 true WO2022110509A1 (en) 2022-06-02

Family

ID=75228007

Family Applications (1)

Application Number Title Priority Date Filing Date
PCT/CN2021/000088 WO2022110509A1 (en) 2020-11-30 2021-04-14 Method for determining dislocation slip type

Country Status (2)

Country Link
CN (1) CN112611661B (en)
WO (1) WO2022110509A1 (en)

Families Citing this family (4)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN112611661B (en) * 2020-11-30 2022-04-12 中国科学院金属研究所 Method for judging dislocation slippage type
CN113203763B (en) * 2021-06-04 2023-07-04 哈尔滨工业大学 Rapid and accurate calibration method for sliding line by utilizing pole figure analysis
CN113484351A (en) * 2021-07-07 2021-10-08 中国航发北京航空材料研究院 Method for representing yield strength anisotropy of beta forging titanium alloy forging
CN115183726B (en) * 2022-09-13 2022-11-22 太原理工大学 Device and method for measuring relative rotation angle and horizontal frictional slip between wood members

Citations (7)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
JP5000424B2 (en) * 2007-08-10 2012-08-15 一般財団法人電力中央研究所 Defect detection method for silicon carbide single crystal wafer and method for manufacturing silicon carbide semiconductor element
CN103175856A (en) * 2013-03-17 2013-06-26 中国科学院苏州纳米技术与纳米仿生研究所 Scanning transmission electron microscope imaging method for sample dislocation
CN104569012A (en) * 2015-01-19 2015-04-29 大连理工大学 Method for determining polycrystalline metal deformation activation slippage system
CN108333203A (en) * 2018-02-09 2018-07-27 中国科学院地球化学研究所 A kind of method of in situ detection mineral microcell EBSD images
CN109142402A (en) * 2018-09-28 2019-01-04 中国科学院金属研究所 A kind of TKD of the single crystal grain stress state of polycrystalline material determines method
CN110940686A (en) * 2019-11-18 2020-03-31 中国科学院金属研究所 Method for calculating critical splitting stress of twin crystal through EBSD technology and Vickers hardness tester
CN112611661A (en) * 2020-11-30 2021-04-06 中国科学院金属研究所 Method for judging dislocation slippage type

Family Cites Families (4)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US10784076B2 (en) * 2018-07-05 2020-09-22 Fei Company 3D defect characterization of crystalline samples in a scanning type electron microscope
CN110133022B (en) * 2019-04-12 2021-12-21 中国科学院金属研究所 Method for calculating orientation of bottom crystal face of oxide film of material by EBSD technology
CN110940683A (en) * 2019-11-18 2020-03-31 中国科学院金属研究所 Method for realizing in-situ compression observation by combination of Vickers hardness tester and transmission electron microscope
CN111999323A (en) * 2020-08-13 2020-11-27 中国科学院金属研究所 In-situ EBSD observation method for microscopic orientation evolution of magnesium alloy recrystallized grains

Patent Citations (7)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
JP5000424B2 (en) * 2007-08-10 2012-08-15 一般財団法人電力中央研究所 Defect detection method for silicon carbide single crystal wafer and method for manufacturing silicon carbide semiconductor element
CN103175856A (en) * 2013-03-17 2013-06-26 中国科学院苏州纳米技术与纳米仿生研究所 Scanning transmission electron microscope imaging method for sample dislocation
CN104569012A (en) * 2015-01-19 2015-04-29 大连理工大学 Method for determining polycrystalline metal deformation activation slippage system
CN108333203A (en) * 2018-02-09 2018-07-27 中国科学院地球化学研究所 A kind of method of in situ detection mineral microcell EBSD images
CN109142402A (en) * 2018-09-28 2019-01-04 中国科学院金属研究所 A kind of TKD of the single crystal grain stress state of polycrystalline material determines method
CN110940686A (en) * 2019-11-18 2020-03-31 中国科学院金属研究所 Method for calculating critical splitting stress of twin crystal through EBSD technology and Vickers hardness tester
CN112611661A (en) * 2020-11-30 2021-04-06 中国科学院金属研究所 Method for judging dislocation slippage type

Also Published As

Publication number Publication date
CN112611661B (en) 2022-04-12
CN112611661A (en) 2021-04-06

Similar Documents

Publication Publication Date Title
WO2022110509A1 (en) Method for determining dislocation slip type
Andersson et al. In-situ SEM study of fatigue crack growth behaviour in IN718
Hay et al. Instrumented indentation testing
Uchic et al. Exploring specimen size effects in plastic deformation of Ni3 (Al, Ta)
Sneddon et al. Sensitivity of material failure to surface roughness: A study on titanium alloys Ti64 and Ti407
CN110940686B (en) Method for calculating critical splitting stress of twin crystal through EBSD technology and Vickers hardness tester
EP2118635A1 (en) Estimation of non-equibiaxial stress using instrumented indentation technique
JP2844181B2 (en) Material testing device, material testing apparatus and material testing method
Sagadevan et al. Novel Analysis on the Influence of Tip Radius and Shape of the Nanoindenter on the Hardness of Materials
CN108931544B (en) Sample clamping device and test method for in-situ electron back scattering diffraction research
Useinov et al. Mutual consistency of hardness testing at micro-and nanometer scales
Ridgway et al. The hardness and elastic modulus of some crystalline pharmaceutical materials
Yeung et al. Assessment of backside processes through die strength evaluation
Fischer-Cripps Factors affecting nanoindentation test data
Ma et al. Effect of the spherical indenter tip assumption on the initial plastic yield stress
Wang Influences of sample preparation on the indentation size effect and nanoindentation pop-in on nickel
Lee et al. Fracture strength measurement of silicon chips
Popelar An investigation into the fracture of silicon die used in flip chip applications
Göken et al. Atomic force microscopy investigations of loaded crack tips in NiAl
CN115047216A (en) Method for testing abrasion performance of particle reinforced metal matrix composite
Huang et al. Anisotropic elastic recovery behavior of AlN ceramic during nanoindentation and scratching
US3435668A (en) Method of determining preferred orientation in metals
Tsai et al. Determination of silicon die strength
Shen et al. Prediction of residual stress components and their directions from pile-up morphology: An experimental study
Soifer et al. Investigation of the local mechanical properties of potassium chloride single crystals by atomic force microscopy

Legal Events

Date Code Title Description
121 Ep: the epo has been informed by wipo that ep was designated in this application

Ref document number: 21896029

Country of ref document: EP

Kind code of ref document: A1

NENP Non-entry into the national phase

Ref country code: DE

122 Ep: pct application non-entry in european phase

Ref document number: 21896029

Country of ref document: EP

Kind code of ref document: A1