阅读说明：本技术 基于ebsd技术的镁合金拉伸孪晶体积分数的计算方法 (EBSD technology-based calculation method for volume fraction of magnesium alloy stretching twin crystal ) 是由 吴懿萍 熊汉青 谢邵辉 于 2020-06-05 设计创作，主要内容包括：本发明公开了一种基于EBSD技术的镁合金拉伸孪晶体积分数的计算方法,根据晶界取向变化标示出拉伸孪晶晶界而获得所有发生拉伸孪晶的完整晶粒,再进行符合规定方向要求的晶粒的选取以及去除杂质处理来获得完全符合规定方向要求的晶粒,完全符合规定方向要求的晶粒中包括孪生部分和未发生孪生部分,将未发生孪生部分分离出,再对孪生部分进行拉伸孪晶体积分数的计算,排除了人为误差对计算精度产生的影响；该计算方法通过晶粒EBSD背散射衍射图和反极图能够更为准确地标定出样品中的拉伸孪晶,从而能够获得准确度更高的拉伸孪晶体积分数。(The invention discloses a calculation method of the volume fraction of a magnesium alloy stretching twin crystal based on an EBSD technology, which comprises the steps of marking a stretching twin crystal boundary according to the orientation change of the crystal boundary to obtain all complete crystal grains which generate stretching twin crystals, then selecting the crystal grains which meet the requirement of a specified direction and removing impurities to obtain the crystal grains which completely meet the requirement of the specified direction, separating the part which does not generate the twin crystals, and then calculating the volume fraction of the stretching twin crystals of the twin parts, thereby excluding the influence of human errors on the calculation precision; according to the calculation method, the stretching twin crystals in the sample can be more accurately marked through the grain EBSD back scattering diffraction pattern and the antipole pattern, so that the stretching twin crystal volume fraction with higher accuracy can be obtained.)

1. A method for calculating the volume fraction of a magnesium alloy stretching twin crystal based on an EBSD technology is characterized by comprising the following steps:

step 1: performing an EBSD test on the magnesium alloy with the tensile strain of N% to obtain an EBSD test chart, wherein the EBSD test chart comprises a test orientation chart and a corresponding test inverse pole chart;

step 2: in the test orientation graph, a tensile twin grain boundary is marked according to the orientation change of the grain boundary;

and step 3: selecting crystal grains meeting the requirement of a specified direction, and obtaining an EBSD orientation graph and a corresponding inverse pole graph of the crystal grains meeting the requirement of the specified direction, wherein the specified direction means that the c axis of the crystal grains is parallel to the stretching direction;

and 4, step 4: removing the crystal grains which do not meet the requirement of the specified direction in the EBSD orientation graph of the crystal grains which meet the requirement of the specified direction in the step 2 by combining the EBSD test graph in the step 1 to obtain the crystal grains which completely meet the requirement of the specified direction, thereby obtaining the orientation graph and the corresponding inverse pole graph of the crystal grains which completely meet the requirement of the specified direction;

and 5: in the inverse pole diagram of the crystal grain completely meeting the requirement of the specified direction in the step 4, separating the residual parent body without the stretching twin crystal from the stretching twin crystal to obtain an orientation diagram of the stretching twin crystal and a corresponding inverse pole diagram, and an orientation diagram of the residual parent body without the stretching twin crystal and a corresponding inverse pole diagram;

step 6: and calculating the volume fraction of the stretching twin crystals according to the inverse pole figure of the stretching twin crystals in the step 5 and the inverse pole figure of the matrix left without the stretching twin crystals.

2. The method for calculating the volume fraction of the magnesium alloy drawing twin crystal based on the EBSD technology as claimed in claim 1, wherein: in the step 2, after the tensile twin crystal is generated in the crystal grain, the c axis of the crystal grain is along

3. The method for calculating the volume fraction of the magnesium alloy drawing twin crystal based on the EBSD technology as claimed in claim 1 or 2, wherein: in step 3, the HKL Channel 5 software selects the die meeting the specified orientation requirement through the "Texture component" option.

4. The method for calculating the volume fraction of the magnesium alloy drawing twin crystal based on the EBSD technology as claimed in claim 1 or 2, wherein: in the step 6, the calculation expression of the volume fraction of the stretching twin crystal is as follows:

wherein f is_sTo stretch twin volume fraction, P_TwinNumber of mass points for stretching twins, P_FemaleIs the total mass point number of the parent crystal grains.

Technical Field

The invention belongs to the technical field of plastic deformation and application of non-ferrous metal materials, and particularly relates to a calculation method of the volume fraction of a magnesium alloy stretching twin crystal based on an EBSD (electron back scattering) technology.

Background

The magnesium alloy has low strength and poor plasticity at room temperature, and is a key problem limiting the wide application of structural parts. The magnesium alloy extruded sheet is stretched along the direction vertical to the extrusion direction to preset stretching twin crystals, and the strength and the plasticity of the magnesium alloy sheet can be improved by means of the effects of the stretching twin crystals on grain refinement, texture weakening and coordinated deformation.

The most direct way to obtain The contribution of The tensile twins to The macroscopic strain is to calculate The volume fraction of The tensile twins according to The formula "roll of Deformation with The mechanical properties of metals" proposed by REED-HILL RE, The innovative of Plastic Deformation, ASM semi.1, 285-311,1973_t＝m_sf_sγ_tWherein, in the step (A),_tfor tensile axial strain due to twinning, m_sSchmidt (Schmid) factor (in general, the average value thereof is in the range of 0.4 to 0.45), f, which is a tensile twinning_sTo stretch the twin volume fraction, gamma_tShear (gamma) for tensile twinning in magnesium alloys_t＝0.13)。

Metallographic results show that the volume fraction of the tensile twin crystals of the AZ31magnesium alloy extruded pipe is almost negligible when the compressive strain is 2%; at a compressive strain of 4%, the integrated number of tensile twin crystals is about 35% (see JIANG LAN, JONAS JOHN J., LUO ALAN A., SACHDEV ANIL K., GODET ST PHANE. infiluence of {10-12} extension bending on the flow behavior of AZ31Mg alloy [ J ], Materials science and Engineering: A,2007, 445-one 446: 302-one 309.); at a compressive engineering strain of 1.5%, the tensile twin integral number in the AZ31magnesium alloy was about 25%, and the grain size did not greatly affect the twin integral number, and the axial strain was entirely attributed to the tensile twin (see ghadiri ALIREZA, BARNETT matrix r. sensitivity of deformation with respect to grain size in titanium and magnesium [ J ], ActaMaterialia,2011,59:7824 and 7839.). Neutron diffraction can be used to detect the twin volume fraction due to orientation changes caused by tensile twins, with an AZ31magnesium alloy having a tensile twin volume fraction of about 13% at an engineering strain of 1.5% (see CLAUSEN B., TOM C.N., BROWN D.W., AGEW S.R. Reoridation and stress release product to twisting: Modeling and experimental characterization for Mg [ J ], Acta Materialia,2008,56: 2456-. However, when the metallograph is adopted to calculate the volume fraction of the tensile twin crystal in the magnesium alloy, the accuracy of the result is poor; when the neutron diffraction test is adopted to obtain the volume fraction of the tensile twin crystal, the orientation requirement of the tensile twin crystal on the parent body is too perfect; when a crystal plasticity model is used to predict the stretching twin volume fraction, the strict twin Schmid factor rule is used, i.e. stretching twin with a larger Schmid factor is preferentially generated in a specific crystal grain (refer to WANG H., RAEISINIAB, WU P.D., AGNEW S.R., TOM C.N.evaluation of self-consistent polycrystalline silicon model for large alloy AZ31B sheet [ J ], International Journal of Solids and Structures,2010,47: 2905-2917.). In fact, EBSD (Electron Back scattered Diffraction) tests found that the generation of tensile twin does not completely conform to Schmid factor rule, that even though the Schmid factor is smaller in a certain crystal grain, tensile twin is generated within the crystal grain, and that tensile twin variants with small Schmid factor replace tensile twin variant generation with large Schmid factor (refer to BEYERLEIN I.J., CAPOLUNGO L., SHALL P.E., CABM R.J., TOMC.N. statistical analysis of deformation in magnesium J, physical Magazine,2010,90: 2161. 190.; HOU DEWEN, ZHUZHI, LIZHEN, LILIPO, NMO, WEN IMEI. E.10. 10. heavy alloy, and the statistical analysis of growth of magnesium in magnesium 31: 31 < AZE > and 31 < AZE > of growth of magnesium 31 > and 85twin < 12 > of magnesium, 2018,32.).

Disclosure of Invention

Aiming at the defects of the prior art, the invention provides a method for calculating the volume fraction of a magnesium alloy stretching twin crystal based on an EBSD technology, so as to improve the calculation accuracy of the volume fraction of the stretching twin crystal.

The invention solves the technical problems through the following technical scheme: a method for calculating the volume fraction of a magnesium alloy stretching twin crystal based on an EBSD technology comprises the following steps:

step 1: performing an EBSD test on the magnesium alloy with the tensile strain of N% to obtain an EBSD test chart, wherein the EBSD test chart comprises a test orientation chart and a corresponding test inverse pole chart;

step 2: in the test orientation graph, a tensile twin grain boundary is marked according to the orientation change of the grain boundary;

and step 3: selecting crystal grains meeting the requirement of a specified direction, and obtaining an EBSD orientation graph and a corresponding inverse pole graph of the crystal grains meeting the requirement of the specified direction, wherein the specified direction means that the c axis of the crystal grains is parallel to the stretching direction;

and 4, step 4: removing the crystal grains which do not meet the requirement of the specified direction in the EBSD orientation graph of the crystal grains which meet the requirement of the specified direction in the step 2 by combining the EBSD test graph in the step 1 to obtain the crystal grains which completely meet the requirement of the specified direction, thereby obtaining the orientation graph and the corresponding inverse pole graph of the crystal grains which completely meet the requirement of the specified direction;

and 5: in the inverse pole diagram of the crystal grain completely meeting the requirement of the specified direction in the step 4, separating the residual parent body without the stretching twin crystal from the stretching twin crystal to obtain an orientation diagram of the stretching twin crystal and a corresponding inverse pole diagram, and an orientation diagram of the residual parent body without the stretching twin crystal and a corresponding inverse pole diagram;

step 6: and calculating the volume fraction of the stretching twin crystals according to the inverse pole figure of the stretching twin crystals in the step 5 and the inverse pole figure of the matrix left without the stretching twin crystals.

Therefore, by the calculation method, the stretching twin crystal boundary is marked according to the stretching orientation change to obtain all complete crystal grains which generate stretching twin crystals, then crystal grains which meet the requirement of the specified direction are selected and impurity removal treatment is carried out to obtain crystal grains which completely meet the requirement of the specified direction, the crystal grains which completely meet the requirement of the specified direction comprise twin crystal parts and twin crystal non-generating parts, the twin crystal non-generating parts are separated, then the stretching twin crystal volume fraction of the twin crystal parts is calculated, and the influence of artificial errors on the calculation precision is eliminated; according to the calculation method, the stretching twin crystals in the sample can be more accurately marked through the EBSD back scattering diffraction pattern and the antipole pattern, so that the stretching twin crystal volume fraction with higher accuracy can be obtained.

Go toStep 2, after the tensile twin crystal is generated in the crystal grain, the c axis of the crystal grain is along<11^_20>The direction was subjected to an orientation change of 86.3 °, from which the tensile twin boundaries were identified.

Further, in step 3, the HKL Channel 5 software selects the grains meeting the specified orientation requirement through the "Texture component" option.

Further, in the step 6, the calculation expression of the volume fraction of the tensile twin crystals is as follows:

wherein f is_sTo stretch twin volume fraction, P_TwinNumber of mass points for stretching twins, P_FemaleIs the total mass point number of the parent crystal grains.

Advantageous effects

Compared with the prior art, the calculation method of the volume fraction of the magnesium alloy stretching twin crystals based on the EBSD technology provided by the invention has the advantages that the stretching twin crystal boundary is marked according to the orientation change of the crystal boundary to obtain all complete crystal grains which generate the stretching twin crystals, then the crystal grains which meet the requirement of the specified direction are selected and the impurities are removed to obtain the crystal grains which completely meet the requirement of the specified direction, the crystal grains which completely meet the requirement of the specified direction comprise a twin part and a non-twin part, the non-twin part is separated out, the volume fraction of the stretching twin crystals of the twin part is calculated, and the influence of human errors on the calculation precision is eliminated; the calculation method can more accurately mark the stretching twin crystals in the sample through the EBSD back scattering diffraction pattern and the antipole pattern, so that the stretching twin crystal volume fraction with higher accuracy can be obtained.

Drawings

In order to more clearly illustrate the technical solution of the present invention, the drawings needed to be used in the description of the embodiments are briefly introduced below, and it is obvious that the drawings in the following description are only one embodiment of the present invention, and it is obvious for those skilled in the art to obtain other drawings based on the drawings without creative efforts.

FIG. 1(a) is an EBSD test orientation of an extruded AZ31magnesium alloy in a state of being extruded in an embodiment of the present invention, when the magnesium alloy is stretched in a direction perpendicular to the extrusion direction and the tensile strain is 4%;

FIG. 1(b) is an EBSD test inverse plot of an extruded AZ31magnesium alloy at 4% tensile strain drawn perpendicular to the extrusion direction in an example of the invention;

FIG. 2(a) is an EBSD orientation of grains meeting the specified orientation requirements (meaning that grains <0001> are parallel to the direction of stretching) in an embodiment of the present invention;

FIG. 2(b) is an EBSD antipole diagram of the grains meeting the specified orientation requirement in the embodiment of the present invention;

FIG. 3(a) is an orientation diagram of a process for removing grains that do not meet the specified orientation requirements in an embodiment of the present invention;

FIG. 3(b) is an inverse view of the removal process of grains that do not meet the specified orientation requirements in an embodiment of the present invention;

FIG. 4(a) is an orientation diagram of a grain fully meeting the specified orientation requirement in an embodiment of the present invention;

FIG. 4(b) is an inverse view of a die fully meeting the specified orientation requirements in an embodiment of the present invention;

FIG. 5(a) is an orientation diagram of the remaining matrix in which no stretching twins occur in the example of the present invention;

FIG. 5(b) is a reverse polarity diagram of the remaining matrix in which no stretching twins occur in the example of the present invention;

FIG. 6(a) is an orientation diagram of a drawing twin in the example of the invention;

FIG. 6(b) is a reverse polarity diagram of a tensile twin crystal in the embodiment of the invention.

Detailed Description

The technical solutions in the present invention are clearly and completely described below with reference to the drawings in the embodiments of the present invention, and it is obvious that the described embodiments are only a part of the embodiments of the present invention, and not all of the embodiments. All other embodiments, which can be derived by a person skilled in the art from the embodiments given herein without making any creative effort, shall fall within the protection scope of the present invention.

The invention provides a method for calculating the volume fraction of a magnesium alloy stretching twin crystal based on an EBSD technology, which comprises the following steps:

1. and performing an EBSD test on the AZ31magnesium alloy with the tensile strain of 4% to obtain an EBSD test chart, wherein the EBSD test chart comprises a test orientation chart and a corresponding test inverse pole chart.

The EBSD test was performed on a scanning electron microscope of LEO1530 to obtain EBSD test patterns of AZ31magnesium alloy at 4% tensile strain, as shown in fig. 1(a) and 1 (b). In fig. 1(a) and 1(b), the dark gray portion and the middle gray portion constitute a complete crystal grain that meets the requirement of the prescribed direction, and in this complete crystal grain, the dark gray indicates a parent body in which no stretching twin occurs, and the middle gray indicates a stretching twin; the light gray portion is the grains that do not meet the specified orientation requirement (i.e., the grains that are not of interest); the lines indicate the tensile twin boundaries. Since the drawings in the specification can only be represented in black and white, and cannot be colored, the drawings are not easily distinguished by dark gray, middle gray and light gray, but can be represented by different colors in actual operation, and the implementation of the scheme of the application is not influenced.

The inverse polar diagram shows the distribution of the characteristic appearance direction in the crystal space by marking the crystal orientation of each crystal grain in the polycrystalline material parallel to the characteristic appearance direction of the material with the crystallographic direction < uvw > as a reference coordinate system, particularly with the important low-index crystal orientation of the crystal as three coordinate axes of the coordinate system. The spatial distribution is projected by taking a plane vertical to the main crystal axis of the crystal as a projection plane and taking a polar-ray equatorial plane projection, namely a reverse polar diagram of the characteristic direction of the polycrystalline material. In all the inverse pole figures of the present application, rd (radial direction of bar) indicates the radial direction of the bar, and ed (extrusion direction) indicates the extrusion direction of the bar.

2. In the test orientation chart, the tensile twin boundaries are marked according to the variation in the orientation of the grain boundaries.

Twinning is uniformShearing, the sheared portion undergoes lattice rotation, forming mirror symmetry with the unsheared portion. With magnesium alloys

Twinning, e.g. the interface of a sheared and unswept zoneCalled twin plane, denoted by K1,

for the shear direction, indicated at η 1,is a second non-distorted noodle, denoted by K2, {12^_10 comprises η 1 and is perpendicular to both K1 and K2, denoted by P, the intersection of the K2 plane and PFor the purpose of not distorting the shear direction, expression η 2, K1, K2, η 1, η 2 is used as twin element or twin parameter, and "study of twin in magnesium alloy plastic deformation" proposed by Cheng shui et al can be referred to]Material reporting, 2006.

The magnesium alloy is a close-packed hexagonal structure, and the tensile twin system is {0001}

Twin planes according to the stretching of twin crystals are Shear direction ofAfter the tensile twin is generated in the crystal grains, the c-axis of the crystal grains (i.e., the<0001>Direction) will be along

The orientation was changed by 86.3 ° in direction, and the orientation was changed by 86.3 ° in misoniationangle "using HKL Channel 5 software, representing that the c-axis of the crystal grain was rotated by 86.3 °, and the tensile twin grain boundary was marked in the test orientation chart of fig. 1(a), as indicated by the line in fig. 1 (a).

3. And selecting the crystal grains meeting the requirement of the specified direction, and obtaining the orientation diagram and the corresponding inverse pole diagram of the crystal grains meeting the requirement of the specified direction.

Since the crystal grains of interest are crystal grains having <0001> orientation parallel to the stretching direction (i.e., the prescribed direction), crystal grains having c-axes (i.e., <0001> direction) oriented parallel to the stretching direction, which are crystal grains satisfying the prescribed direction requirements, are selected by the "Texture component" option in the HKL Channel 5 software. The selected grains are saved as an EBSD subfile for individual analysis, i.e. an EBSD orientation map and a corresponding inverse map of the grains meeting the requirements of the specified orientation, as shown in fig. 2(a) and 2(b), the dark gray and medium gray portions constitute the complete grains meeting the requirements of the specified orientation, and the light gray portions are the grains not meeting the requirements of the specified orientation.

4. And (4) combining the EBSD test pattern, removing the crystal grains which do not meet the requirement of the specified direction in the EBSD orientation pattern of the crystal grains meeting the requirement of the specified direction, and obtaining the crystal grains which completely meet the requirement of the specified direction, namely obtaining the orientation pattern and the corresponding inverse pole pattern of the crystal grains which completely meet the requirement of the specified direction.

As can be seen from fig. 2(a) and 2(b), there are some crystal grains (shown in light gray) that do not meet the requirement of the specified direction, and these crystal grains that do not meet the requirement of the specified direction need to be removed, so as to avoid the influence on the calculation accuracy, the process of removing the light gray crystal grains is shown in fig. 3(a) and 3(b), and finally, an orientation diagram and a corresponding inverse pole diagram of the crystal grains that completely meet the requirement of the specified direction are obtained, as shown in fig. 4(a) and 4(b), respectively. In fig. 4(a) and 4(b) only grains that meet the requirements of the specified orientation (shown in dark grey and medium grey portions) remain, the light grey grains being removed. In actual operation with HKL Channel 5 software, comparing fig. 1(a) and 2(a), the light gray part in fig. 2(a) is deleted to obtain fig. 4(a), and the corresponding fig. 4(b) is obtained.

5. In the inverse pole figure (fig. 4(b)) of crystal grains completely meeting the requirement of the specified direction, the matrix which is not stretched and the stretched twin crystal are separated, and the orientation figure of the stretched twin crystal and the corresponding inverse pole figure are obtained, and the orientation figure of the matrix crystal grains which are not stretched and the corresponding inverse pole figure are obtained.

As can be seen from fig. 4(a), the stretching twin crystal is middle gray, the matrix left without stretching twin crystal is deep gray, and the corresponding fig. 4(b) is more obvious, the deep gray part is the matrix left without stretching twin crystal, the middle gray part is stretching twin crystal, and the two parts are separately stored as a subfile, i.e. the stretching twin crystal and the matrix left without stretching twin crystal are separated to obtain the independent stretching twin crystal and the matrix left without stretching twin crystal, fig. 5(a) and 5(b) are respectively an orientation diagram and an inverse polarity diagram of the matrix left without stretching twin crystal, and fig. 6(a) and 6(b) are respectively an orientation diagram and an inverse polarity diagram of the stretching twin crystal.

6. And calculating the volume fraction of the stretching twin crystal according to the inverse pole figure of the stretching twin crystal and the inverse pole figure of the parent body left without the stretching twin crystal.

As can be seen from fig. 6(b), the number data points of the stretching twin crystal is 32951, and as can be seen from fig. 5(b), the number data points of the matrix in which the stretching twin crystal does not occur is 39675, the volume fraction of the stretching twin crystal is:

wherein f is_sTo stretch twin volume fraction, P_TwinNumber of mass points for stretching twins, P_FemaleThe total number of prime grains (this total number can also be obtained from fig. 4 (b)). Indicating that the stretching twins are in the direction having the c-axis: (<0001>Direction) is about 45% by volume of these grains oriented parallel to the direction of stretching.

In order to obtain accurate volume fraction of the tensile twin crystal, more orientation graphs and antipole graphs can be obtained, more than 3000 crystal grains are contained, and the result is more statistical. After performing multiple EBSD tests, the hair is obtainedThe AZ31magnesium alloy in the Mingzhong extrusion state has the tensile strain of 4 percent<0001>The average of the volume fractions of the stretched twin crystals of the crystal grains oriented parallel to the stretching direction was about 45%. Calculated by formula in background art_t0.4 × 0.45 × 0.13.13 0.0234, the contribution of the tensile twins to the total strain is therefore (_t0.0234/(0.04-0.0006)) up to at least 69%.

The invention relates to a calculation method of the volume fraction of a magnesium alloy drawing twin crystal, which comprises the steps of marking a drawing twin crystal boundary according to the orientation change of the crystal boundary to obtain all drawing twin crystals, then selecting crystal grains meeting the requirement of a specified direction and removing impurities to obtain crystal grains completely meeting the requirement of the specified direction, wherein the crystal grains completely meeting the requirement of the specified direction comprise a twin crystal part and a twin crystal part which does not generate, separating the twin crystal part which does not generate, and then calculating the volume fraction of the drawing twin crystal of the twin crystal part, thereby excluding the influence of human errors on the calculation precision; according to the calculation method, the stretching twin crystals in the sample can be more accurately marked through the EBSD back scattering diffraction pattern and the antipole pattern, so that the stretching twin crystal volume fraction with higher accuracy can be obtained.

The above disclosure is only for the specific embodiments of the present invention, but the scope of the present invention is not limited thereto, and any person skilled in the art can easily conceive of changes or modifications within the technical scope of the present invention, and shall be covered by the scope of the present invention.