CN110118791B - EBSD equipment sample stage and method for acquiring crack/grain boundary three-dimensional information - Google Patents
EBSD equipment sample stage and method for acquiring crack/grain boundary three-dimensional information Download PDFInfo
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- CN110118791B CN110118791B CN201910423906.7A CN201910423906A CN110118791B CN 110118791 B CN110118791 B CN 110118791B CN 201910423906 A CN201910423906 A CN 201910423906A CN 110118791 B CN110118791 B CN 110118791B
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Abstract
The disclosure provides an EBSD device sample stage and method for acquiring crack/grain boundary three-dimensional information. The EBSD equipment sample stage for acquiring three-dimensional information of cracks/grain boundaries comprises: the device comprises an upright post, a first detection surface and a second detection surface are arranged on the upright post, and the first detection surface and the second detection surface form an included angle of 70 degrees with the horizontal plane; the first detection surface and the second detection surface are adjacent and share the same edge; the first detection surface and the second detection surface are perpendicular to each other.
Description
Technical Field
The disclosure belongs to the field of EBSD equipment sample stages for acquiring crack/grain boundary three-dimensional information, and particularly relates to an EBSD equipment sample stage and a method for acquiring crack/grain boundary three-dimensional information.
Background
The statements in this section merely provide background information related to the present disclosure and may not necessarily constitute prior art.
EBSD, known as Electron back scattered Diffraction (foreign language name), is characterized primarily by Diffraction at the sub-micron level with spatial resolution (giving crystallographic data) while retaining the conventional features of scanning Electron microscopy.
The combination of EBSD and a scanning electron microscope is an effective means for detecting the crystallographic information on the surface of the crystal material at present. Currently, 3D-EBSD is generally adopted for measuring 3-dimensional crystallographic information of crystal materials. EBSD can be used in 3D analysis techniques by combining scanning electron microscopy with Focused Ion Beam (FIB). The inventor finds that the conventional EBSD device sample stage for acquiring the three-dimensional information of the cracks/grain boundaries can only detect one surface of a sample, a Focused Ion Beam (FIB) is used for cutting one layer of the surface of the sample, and after the surface of each layer of the sample is cut, the EBSD data is acquired by combining the EBSD device sample stage for acquiring the three-dimensional information of the cracks/grain boundaries with a fresh surface. This process is repeated and finally 3D-EBSD data of the region of interest is obtained. However, this process typically requires many layers of EBSD data, possibly up to several hundred layers, which takes a long time; bringing significant testing costs.
Disclosure of Invention
In order to solve the above problems, a first aspect of the present disclosure provides an EBSD apparatus sample stage for acquiring crack/grain boundary three-dimensional information, which has a simple structure, and only needs to process two intersecting surfaces of a sample and respectively acquire corresponding EBSD data by using a first detection surface and a second detection surface, thereby saving the time for cutting off the sample surface, greatly improving the EBSD data acquisition efficiency, and achieving the purpose of acquiring 3-dimensional information of a material by using a 2D-EBSD technique, thereby tracking an expansion crystal face of a crack of a crystal material and determining a crystal face index of a grain boundary of a polycrystalline material.
In order to achieve the purpose, the following technical scheme is adopted in the disclosure:
an EBSD device sample stage for acquiring crack/grain boundary three-dimensional information, comprising:
the device comprises an upright post, a first detection surface and a second detection surface are arranged on the upright post, and the first detection surface and the second detection surface form an included angle of 70 degrees with the horizontal plane; the first detection surface is intersected with the second detection surface; the first detection surface and the second detection surface are perpendicular to each other.
A second aspect of the disclosure provides an application of an EBSD apparatus sample stage for acquiring crack/grain boundary three-dimensional information.
The EBSD equipment sample stage for acquiring the crack/grain boundary three-dimensional information can be applied to EBSD equipment, a method for acquiring the crack three-dimensional information of the sample and a method for acquiring the grain boundary three-dimensional information of the sample.
An EBSD device comprises at least one EBSD device sample stage for acquiring three-dimensional information of cracks/grain boundaries.
A method for acquiring three-dimensional information of sample cracks comprises the following steps:
cutting a sample with cracks into a cuboid shape to enable the cracks to be positioned on two intersected surfaces, and polishing the two surfaces where the cracks are positioned;
fixing the polished sample on the first detection surface of the sample stage of the EBSD device for acquiring the crack/crystal boundary three-dimensional information, so that the first surface where the crack is located is parallel to the first detection surface, and the second surface where the crack is located is parallel to the second detection surface;
acquiring orientation information of the crack on the first surface by using an EBSD device to obtain Euler angle and crack vector information of the crystal grain on which the crack is located on the first surface;
after the acquisition of the orientation information of the first surface where the crack is located is finished, rotating the EBSD equipment sample platform for acquiring the crack/crystal boundary three-dimensional information by 90 degrees, so that the second detection surface is opposite to the EBSD equipment probe, keeping the coordinate system of the sample unchanged, obtaining the Euler angle and the crack vector information of the crystal grain where the crack is located on the second surface, and further obtaining the crystallography index three-dimensional information of the crack.
A method for acquiring three-dimensional information of a sample grain boundary comprises the following steps:
cutting a sample of which the crystal face index of the crystal boundary is to be determined into a cuboid shape, enabling the crystal boundary to be detected to appear on two intersected surfaces of the sample at the same time, and polishing the two intersected surfaces;
fixing the polished sample on the first detection surface of the sample stage of the EBSD device for acquiring the crack/crystal boundary three-dimensional information, so that the first surface where the crystal boundary is located is parallel to the first detection surface, and the second surface where the crystal boundary is located is parallel to the second detection surface;
acquiring orientation information on the first surface by utilizing an EBSD device crystal boundary to obtain an Euler angle of a crystal grain to which the crystal boundary belongs on the first surface and vector information of the crystal grain on the first surface;
after the acquisition of the orientation information of the first surface where the grain boundary is located is finished, rotating the sample stage of the EBSD device for acquiring the crack/grain boundary three-dimensional information by 90 degrees, so that the second detection surface is opposite to the probe of the EBSD device, keeping the coordinate system of the sample unchanged, obtaining the Euler angle of the grain boundary on the second surface and the vector information of the grain boundary on the second surface, and further obtaining the crystallographic index three-dimensional information of the crystal face of the grain boundary.
The beneficial effects of this disclosure are:
the EBSD equipment sample platform for acquiring crack/crystal boundary three-dimensional information comprises an upright post, wherein a first detection surface and a second detection surface are arranged on the upright post, and both the first detection surface and the second detection surface form an included angle of 70 degrees with a horizontal plane; the first detection surface is intersected with the second detection surface; the first detection surface and the second detection surface are perpendicular to each other, the EBSD device sample platform for acquiring crack/crystal boundary three-dimensional information is simple in structure, only two intersected surfaces of a sample need to be processed, and corresponding EBSD data are acquired by the first detection surface and the second detection surface respectively, so that the time for cutting the surface of the sample is saved, the EBSD data acquisition efficiency is greatly improved, 3-dimensional information of a material is acquired by using a 2D-EBSD technology, and the purposes of tracking an expansion crystal face of a crack of a crystal material and determining a crystal face index of a crystal boundary of a polycrystalline material are achieved.
Drawings
The accompanying drawings, which are included to provide a further understanding of the disclosure, illustrate embodiments of the disclosure and together with the description serve to explain the disclosure and are not to limit the disclosure.
Fig. 1 is a right side view of an EBSD apparatus sample stage for acquiring crack/grain boundary three-dimensional information according to an embodiment of the disclosure;
FIG. 2 is a front view of an EBSD device sample stage for acquiring crack/grain boundary three-dimensional information according to an embodiment of the disclosure;
FIG. 3 is a left side view of an EBSD device sample stage for acquiring crack/grain boundary three-dimensional information according to an embodiment of the disclosure;
FIG. 4 is a schematic illustration of a sample to be tested containing a crack according to an embodiment of the disclosure;
FIG. 5(a) is a front view of a sample to be examined according to an embodiment of the present disclosure after being stuck to a sample stage;
fig. 5(b) is a right side view of a sample to be tested according to an embodiment of the present disclosure after being stuck on a sample stage.
Detailed Description
The present disclosure is further described with reference to the following drawings and examples.
It should be noted that the following detailed description is exemplary and is intended to provide further explanation of the disclosure. Unless defined otherwise, all technical and scientific terms used herein have the same meaning as commonly understood by one of ordinary skill in the art to which this disclosure belongs.
It is noted that the terminology used herein is for the purpose of describing particular embodiments only and is not intended to be limiting of example embodiments according to the present disclosure. As used herein, the singular forms "a", "an" and "the" are intended to include the plural forms as well, and it should be understood that when the terms "comprises" and/or "comprising" are used in this specification, they specify the presence of stated features, steps, operations, devices, components, and/or combinations thereof, unless the context clearly indicates otherwise.
In the present disclosure, terms such as "upper", "lower", "left", "right", "front", "rear", "vertical", "horizontal", "side", "bottom", and the like indicate orientations or positional relationships based on those shown in the drawings, and are only relational terms determined for convenience in describing structural relationships of the parts or elements of the present disclosure, and do not refer to any parts or elements of the present disclosure, and are not to be construed as limiting the present disclosure.
In the present disclosure, terms such as "fixedly connected", "connected", and the like are to be understood in a broad sense, and mean either a fixed connection or an integrally connected or detachable connection; may be directly connected or indirectly connected through an intermediate. The specific meanings of the above terms in the present disclosure can be determined on a case-by-case basis by persons skilled in the relevant art or technicians, and are not to be construed as limitations of the present disclosure.
Example one
The EBSD apparatus sample stage for acquiring three-dimensional information of cracks/grain boundaries of the embodiment includes:
the detection device comprises an upright post 1, wherein a first detection surface 2 and a second detection surface 3 are arranged on the upright post 1, and the first detection surface 2 and the second detection surface 3 form an included angle of 70 degrees with the horizontal plane; the first detection surface 2 and the second detection surface 3 intersect; the first detection surface 2 and the second detection surface 3 are perpendicular to each other. The upright post of the present embodiment is a polygon prism, as shown in fig. 1-3.
It is understood that in other embodiments, the pillar is a cylinder or other shapes of cylinders, which can be set by one skilled in the art according to specific working conditions and will not be described in detail herein.
The EBSD equipment sample platform for acquiring the crack/crystal boundary three-dimensional information has a simple structure, only needs to process two intersected surfaces of a sample and respectively utilizes the first detection surface and the second detection surface to acquire corresponding EBSD data, saves the time for cutting the surface of the sample, greatly improves the acquisition efficiency of the EBSD data, realizes the acquisition of 3-dimensional information of a material by utilizing a 2D-EBSD technology, and further achieves the purposes of tracking an expansion crystal face of a crack of a crystal material and determining a crystal face index of a crystal boundary of a polycrystalline material.
Example two
The EBSD apparatus of this embodiment is characterized by comprising at least one sample stage of the EBSD apparatus for acquiring three-dimensional information of cracks/grain boundaries as in embodiment one.
It should be noted that other structures of the EBSD apparatus are all existing structures, and the number of sample stages of the EBSD apparatus for acquiring three-dimensional information of cracks/grain boundaries may be specifically set according to actual situations.
EXAMPLE III
The method for acquiring the three-dimensional information of the sample crack comprises the following steps:
s101: the sample with cracks was cut into a rectangular parallelepiped shape as shown in fig. 4 so that the cracks were located on two intersecting surfaces, and the two surfaces where the cracks were located were polished. Wherein, 1# and 2# represent two sample surfaces perpendicular to each other, respectively.
In specific implementation, vibration polishing or electrolytic polishing is carried out on two surfaces where the cracks are located, and a strain layer on the surface of the sample is removed to enable the strain layer to meet the surface conditions required by EBSD detection.
S102: the polished sample is fixed on the first detection surface of the sample stage of the EBSD device for acquiring crack/grain boundary three-dimensional information as described in embodiment one, so that the first surface where the crack is located is parallel to the first detection surface, and the second surface where the crack is located is flush with the second detection surface.
In specific implementation, the polished sample is fixed on a first detection surface of a sample stage of the EBSD device for acquiring three-dimensional information of cracks/grain boundaries by conductive adhesive.
The back of the 1# sample is adhered to the A side of the sample stage, so that the 1# side faces outwards, and the 2# surface of the sample is flush with the B side of the sample stage. The adhered samples are in a state that the included angle between the No. 1 and the No. 2 forms an angle of 70 degrees with the horizontal plane, and the No. 1 and the No. 2 meet the angle requirement required by the EBSD detection, as shown in FIGS. 5(a) -5 (b).
S103: and acquiring orientation information of the crack on the first surface by using an EBSD device to obtain Euler angle and vector information of the crack on the first surface.
Specifically, orientation information of the 1# surface is acquired by using EBSD, the sample platform is rotated to ensure that the 1# surface is opposite to the direction of an EBSD probe, a sample coordinate system Sij is determined, an area containing cracks is selected, then acquisition is started, and the Euler angle of the crystal grain to which the cracks to be detected belong on the 1# surface is obtained
Simultaneously obtaining the vector information of the cracks on the 1# surface
S104: after the acquisition of the orientation information of the first surface where the crack is located is completed, the EBSD equipment sample stage for acquiring the crack/grain boundary three-dimensional information as described in the first embodiment is rotated by 90 degrees, so that the second detection surface is over against the EBSD equipment probe, the sample coordinate system is kept unchanged, the Euler angle and the crack vector information of the crystal grain to which the crack belongs on the second surface are obtained, and further the three-dimensional information of the crystallographic index of the crack is obtained.
Specifically, after the 1# plane orientation information is acquired, the sample does not need to be taken down, the sample table is rotated clockwise by 90 degrees in a preset mode (for example, in an SE2 mode), the 2# plane is opposite to the direction of the EBSD probe after the rotation is completed, and the eye tracks the change of the crack in the screen during the rotation process, so that the crack to be detected is ensured to be displayed in the screen all the time. Selecting a sample coordinate system Sij which is the same as the sample coordinate system Sij in the previous step, selecting a region containing cracks, starting to collect, and then obtaining the Euler angle of the crystal grains to which the cracks belong on the 2# surface
Simultaneously obtaining the vector information of the crack on the 2# surface
After the acquisition of the orientation information is completed, the orientation information on two crystal planes of the crack is obtained, and the crystallographic calculation is performed to obtain the crystallographic index of the crystal plane to which the crack belongs, wherein the process is as follows:
(1) conversion of orientation matrix according to conversion formula
Obtaining orientation matrixes g of crystal grains 1# and 2# on the surface of the sample respectively1And g2；
(2) Crystallographic orientation conversion
Vector information of cracks acquired during acquisition of front orientation informationAndare all vector information in the sample coordinate system, which now needs to be converted from the sample coordinate system to the crystal orientation of the crystal coordinate system
And
the conversion formula is as follows:
{Cij}＝gij·{Sij}，
namely:
at this time
And
is two crystal directions of the crack on two mutually perpendicular crystal planes, and⊥
then
And
and the crystal plane is the crack propagation crystal plane.
(3) Normal direction of crack propagation crystal plane
According to the principle: the cross product of two mutually perpendicular vectors is perpendicular to the two vectors. Namely, it is
And
is a vector product of
And
normal to the crystal plane.
The method has the advantages that the corresponding EBSD data are obtained by processing two intersected surfaces of the sample and respectively utilizing the first detection surface and the second detection surface, so that the time for cutting the surface of the sample is saved, the EBSD data obtaining efficiency is greatly improved, the 3-dimensional information of the material is obtained by utilizing the 2D-EBSD technology, and the purpose of tracking the crystal face index of the expansion crystal face of the crack of the crystal material is further achieved.
Example four
The method for acquiring the three-dimensional information of the sample grain boundary comprises the following steps:
s201: cutting a sample to be determined with the crystal face index of the crystal boundary into a cuboid shape, enabling the crystal boundary to be detected to appear on two intersected surfaces of the sample at the same time, and polishing the two intersected surfaces.
In specific implementation, the crystal boundary to be detected simultaneously appears on two intersected surfaces of the sample, and vibration polishing or electrolytic polishing is carried out, so that a strain layer on the surface of the sample is removed to enable the strain layer to meet the surface condition required by EBSD detection.
S202: the polished sample is fixed on the first detection surface of the sample stage of the EBSD apparatus for acquiring crack/grain boundary three-dimensional information as described in embodiment one, so that the first surface where the grain boundary is located is parallel to the first detection surface, and the second surface where the grain boundary is located is flush with the second detection surface.
In specific implementation, the polished sample is fixed on a first detection surface of a sample stage of the EBSD device for acquiring three-dimensional information of cracks/grain boundaries by conductive adhesive.
S203: and acquiring orientation information on the first surface by using the grain boundary of the EBSD equipment to obtain the Euler angle of the grain boundary on the first surface and the vector information of the grain boundary on the first surface.
Specifically, the EBSD is used for collecting orientation information of the first surface, the sample platform is rotated to enable the first surface to face the direction of the EBSD probe, a sample coordinate system Sij is determined, an area containing a grain boundary to be detected is selected, then the collection is started, and the Euler angle (phi) of the grain boundary on the first surface is obtained1,Φ,φ2)1Simultaneously obtaining the vector information of the crystal grains to which the crystal boundaries belong on the first surface
S204: after the acquisition of the orientation information of the first surface where the crystal boundary is located is finished, rotating the sample stage of the EBSD equipment for acquiring the crack/crystal boundary three-dimensional information by 90 degrees, so that the second detection surface is opposite to the probe of the EBSD equipment, the coordinate system of the sample is kept unchanged, the Euler angle of the crystal grain to which the crystal boundary belongs on the second surface and the vector information of the crystal grain to which the crystal boundary belongs on the second surface are obtained, and further the three-dimensional information of the crystallographic index of the crystal face to which the crystal boundary belongs is obtained.
Specifically, after the first surface orientation information is acquired, the sample does not need to be taken down, the sample table is rotated clockwise by 90 degrees in a preset mode (for example, in an SE2 mode), the second surface faces the direction of the EBSD probe after the rotation is completed, and the eye tracks the change of the grain boundary in the screen during the rotation process, so that the grain boundary to be detected is ensured to be displayed in the screen all the time. Selecting a sample coordinate system Sij which is the same as the sample coordinate system Sij in the previous step, selecting a region containing cracks, starting to collect, and then obtaining the Euler angle of the crystal grain to which the crystal grain boundary belongs on the second surfaceSimultaneously obtaining the vector information of the crystal boundary on the second surface
After the acquisition of the orientation information is completed, the orientation information on two crystal faces of the crystal grain to which the grain boundary belongs is obtained, and the crystallographic index of the crystal face to which the crystal grain to which the grain boundary belongs is obtained through the following crystallographic calculation, wherein the process is as follows:
(1) conversion of orientation matrix according to conversion formula
Respectively obtaining orientation matrixes g of crystal grains on the surface of the sample on the first surface and the second surface1And g2；
(2) Crystallographic orientation conversion
Vector information of grain boundary obtained during acquisition of front orientation information
And
are all vector information in the sample coordinate system, which now needs to be converted from the sample coordinate system to the crystal orientation of the crystal coordinate systemAnd
the conversion formula is as follows:
{Cij}＝gij·{Sij}，
namely:
at this time
And
is two crystal directions of the crack on two mutually perpendicular crystal planes, and
⊥
then
And
and the crystal plane is the crystal plane of the crystal boundary.
(3) Normal direction of crack propagation crystal plane
According to the principle: the cross product of two mutually perpendicular vectors is perpendicular to the two vectors. Namely, it is
And
is a vector product of
And
normal to the crystal plane.
The method has the advantages that the corresponding EBSD data are obtained by processing two intersecting surfaces of the sample and respectively utilizing the first detection surface and the second detection surface, so that the time for cutting the surface of the sample is saved, the EBSD data obtaining efficiency is greatly improved, the 3-dimensional information of the material is obtained by utilizing the 2D-EBSD technology, and the purpose of determining the crystal face index of the grain boundary of the polycrystalline material is further achieved.
The above description is only a preferred embodiment of the present disclosure and is not intended to limit the present disclosure, and various modifications and changes may be made to the present disclosure by those skilled in the art. Any modification, equivalent replacement, improvement and the like made within the spirit and principle of the present disclosure should be included in the protection scope of the present disclosure.
Claims (10)
1. An EBSD device sample stage for acquiring crack/grain boundary three-dimensional information, comprising:
the device comprises an upright post, a first detection surface and a second detection surface are arranged on the upright post, and the first detection surface and the second detection surface form an included angle of 70 degrees with the horizontal plane; the first detection surface is intersected with the second detection surface; the first detection surface and the second detection surface are perpendicular to each other.
2. The EBSD device sample stage for acquiring crack/grain boundary three-dimensional information as claimed in claim 1, wherein the pillars are polygonal.
3. The EBSD device sample stage for acquiring crack/grain boundary three-dimensional information as claimed in claim 1, wherein the pillar is a cylinder.
4. An EBSD device, characterized by comprising at least one EBSD device sample stage for acquiring crack/grain boundary three-dimensional information according to any one of claims 1 to 3.
5. A method for acquiring three-dimensional information of sample cracks is characterized by comprising the following steps:
cutting a sample with cracks into a cuboid shape to enable the cracks to be positioned on two intersected surfaces, and polishing the two surfaces where the cracks are positioned;
fixing the polished sample on a first detection surface of the EBSD device sample stage for acquiring the crack/grain boundary three-dimensional information according to any one of claims 1 to 3, so that a first surface where the crack is located is parallel to the first detection surface, and a second surface where the crack is located is flush with the second detection surface;
acquiring orientation information of the crack on the first surface by using an EBSD device to obtain Euler angle and crack vector information of the crystal grain on which the crack is located on the first surface;
after the acquisition of the orientation information of the first surface where the crack is located is finished, rotating the EBSD equipment sample stage for acquiring the crack/grain boundary three-dimensional information according to any one of claims 1 to 3 by 90 degrees, so that the second detection surface is opposite to the probe of the EBSD equipment, keeping the coordinate system of the sample unchanged, obtaining the Euler angle and the crack vector information of the crystal grain where the crack is located on the second surface, and further obtaining the three-dimensional information of the crystallographic index of the crack.
6. The method for acquiring the three-dimensional information of the sample cracks as claimed in claim 5, wherein the vibration polishing or the electrolytic polishing is performed on the two surfaces where the cracks are located, and the strain layer on the sample surface is removed to enable the sample surface to meet the surface conditions required by the EBSD detection.
7. The method for acquiring the three-dimensional information of the crack of the sample as claimed in claim 5, wherein the polished sample is fixed on the first detection surface of the sample stage of the EBSD device for acquiring the three-dimensional information of the crack/grain boundary by using conductive adhesive.
8. A method for acquiring three-dimensional information of a sample grain boundary is characterized by comprising the following steps:
cutting a sample of which the crystal face index of the crystal boundary is to be determined into a cuboid shape, enabling the crystal boundary to be detected to appear on two intersected surfaces of the sample at the same time, and polishing the two intersected surfaces;
fixing the polished sample on a first detection surface of the EBSD device sample stage for acquiring the crack/grain boundary three-dimensional information according to any one of claims 1 to 3, wherein the first surface where the grain boundary is located is parallel to the first detection surface, and the second surface where the grain boundary is located is flush with the second detection surface;
acquiring orientation information on the first surface by using an EBSD device crystal boundary to obtain an Euler angle of a crystal grain to which the crystal boundary belongs on the first surface and vector information of the crystal grain on the first surface;
after the acquisition of the orientation information of the first surface where the grain boundary is located is completed, rotating the EBSD device sample stage for acquiring crack/grain boundary three-dimensional information, which is defined in any one of claims 1 to 3, by 90 degrees, so that the second detection surface is over against the probe of the EBSD device, keeping the sample coordinate system unchanged, obtaining the Euler angle of the grain boundary on the second surface and the vector information of the grain boundary on the second surface, and further obtaining the three-dimensional information of the crystallographic index of the crystal boundary on the crystal face.
9. The method for acquiring the three-dimensional information of the grain boundaries of the sample as claimed in claim 8, wherein the intersecting surfaces are subjected to vibration polishing or electrolytic polishing, and a strain layer on the surface of the sample is removed to make the surface meet the surface conditions required by EBSD detection.
10. The method for acquiring the three-dimensional information of the grain boundaries of the sample as claimed in claim 8, wherein the polished sample is fixed on the first detection surface of the sample stage of the EBSD device for acquiring the three-dimensional information of the cracks/grain boundaries by using conductive adhesive.
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