CN115128109A - EBSD sample stage based on orientation calibration and correction and image acquisition method - Google Patents
EBSD sample stage based on orientation calibration and correction and image acquisition method Download PDFInfo
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- CN115128109A CN115128109A CN202211068477.4A CN202211068477A CN115128109A CN 115128109 A CN115128109 A CN 115128109A CN 202211068477 A CN202211068477 A CN 202211068477A CN 115128109 A CN115128109 A CN 115128109A
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- 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
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Abstract
The invention belongs to the technical field of back scattering electron diffraction, and particularly relates to an EBSD sample stage based on orientation calibration correction and an image acquisition method, aiming at solving the problem that the traditional EBSD sample stage does not carry out orientation calibration of crystals when observing a sample, so that the deviation between the macro orientation of the sample and the relative orientation of a certain crystal grain in the sample is overlarge. The invention comprises the following steps: setting standard single crystal sample sites, observing the marked single crystal sample and the sample to be detected, obtaining Euler angles of a crystal coordinate system and a reference coordinate system of a sample carrier through the grain orientation of the standard single crystal sample, and further adjusting the rotation angle of a sample stage of a scanning electron microscope to calibrate the orientation, so that the grain orientation is linked with the macroscopic orientation in a three-dimensional space. The method introduces an orientation calibration correction technology on the basis of the original EBSD characterization technology, and provides accurate data for the analysis of the relative relationship between the grain orientation of the sample to be tested and the macroscopic stress loading direction.
Description
Technical Field
The invention belongs to the technical field of back scattering electron diffraction, and particularly relates to an EBSD sample stage based on orientation calibration and correction and an image acquisition method.
Background
Rock samples and metal alloy samples are easy to deform under the action of tension and compression, and the internal microstructures of the rock samples and the metal alloy samples are changed, particularly the grains are changed along certain specific orientations, such as low-index planes, slip planes and the like. The tensile and compressive properties and the deformation mechanism of the rock sample are closely related to the crystal grains and the force application direction. Directly influences the mechanical properties of rock samples and metal alloy samples, and has great influence on the structural stability of the rock samples and the metal samples.
The EBSD currently used to characterize the grain orientation of samples is primarily mounted inside the scanning electron microscope system. The commercial EBSD sample stage adopts conductive silver adhesive, carbon conductive adhesive tape and the like to fix a sample on the EBSD sample stage, the EBSD sample stage can rotate at will without an orientation correction function, whether the normal of the surface of the sample and the normal of the surface of the EBSD probe are positioned on the same plane can be determined only by adopting visual observation, and the angle error judged by the visual observation can reach 5 degrees. In the tensile and compression experiments, the 5 degrees completely exceed the critical value of the mechanical deformation of the rock or metal sample consisting of nanoscale fine crystals. Due to the lack of orientation calibration correction of the EBSD sample stage, the relative orientation deviation of the macro orientation (such as the force application direction) of the sample and a certain crystal grain inside the sample is overlarge, and the influence of the relation between the force application direction and the crystal grain orientation on the deformation process and the tensile property of the sample is prevented from being researched.
Therefore, the method for calibrating and correcting the orientation of the EBSD sample stage with high precision is very necessary for mechanical research.
Disclosure of Invention
In order to solve the above-mentioned problems in the prior art, that is, the conventional EBSD sample stage does not perform crystal orientation calibration when observing a sample, which results in an excessive deviation between the macro orientation of the sample and the relative orientation of a certain crystal grain inside the sample, the present invention provides an EBSD sample stage based on orientation calibration correction, the sample stage comprising:
a column 1, a first vertical surface 2 and a second vertical surface 3;
the first vertical surface 2 and the second vertical surface 3 are perpendicular to the right-angle boundary 4, and the included angle between the first vertical surface 2 and the horizontal plane is within a preset included angle range; the first vertical surface 2 is 20 degrees with the horizontal direction, and the second vertical surface 3 is 70 degrees with the horizontal direction;
at the right angle where the first vertical surface 2 and the second vertical surface 3 intersect, copper carrier fixing plate sites 801 are arranged, and the copper carrier fixing plate sites 801 are grooves with bottom surfaces parallel to the first vertical surface 2 or the second vertical surface 3 and are overlapped with the right angle boundary 4 at the same position;
one side of the copper carrier fixing plate site 801 on the second vertical surface 3 is provided with a rectangular groove as a standard single crystal sample site 5; the other side of the copper carrier fixing plate site 801 on the second vertical surface 3 and the corresponding position on the second vertical surface 3 are provided with a T-shaped platform site 6; the T-shaped platform position points 6 are two intersected cylindrical slots in the normal direction of the first vertical surface 2 and the second vertical surface 3;
a fixing screw hole 7 is arranged at one side of the intersection of the two T-shaped table positions 6 of the column body 1.
In some preferred embodiments, the copper carrier fixing plate 8 is configured as a rectangular parallelepiped fixing plate, and the rectangular parallelepiped fixing plate is provided with a copper carrier fixing plate screw hole 9 and a position limiting ring position 10; the screw hole 9 of the copper carrier fixing plate is a circular groove, and the circle center of the circular groove is a circular through structure with the diameter smaller than that of the circular groove; spacing clamping ring position 10 is the combination of two circular recesses and a banded recess, and one of them circular recess cuts with the edge of cuboid fixed plate mutually, and the circular recess that is close to copper carrier fixed plate screw hole 9 is the same through-structure of spacing clamping ring screw hole 11 its centre of a circle for making with copper carrier fixed plate screw hole 9, and the circular recess that cuts mutually with the edge of cuboid fixed plate is circular through-structure, and link up circular still cuts mutually with the edge of cuboid fixed plate.
In another aspect of the present invention, an orientation calibration correction-based EBSD image acquisition method is provided, which is implemented by the above orientation calibration correction-based EBSD sample stage, and the method includes:
step S100, obtaining a sample to be detected and a standard single crystal sample;
s200, selecting a sample carrier and placing a sample to be detected according to the size magnitude of the sample to be detected;
arranging the standard single crystal sample on a standard single crystal sample site;
obtaining an assembled sample table;
step S300, placing the assembled sample stage in a scanning electron microscope and adjusting the assembled sample stage to an imaging position so that the sample stage is positioned in the center of an image of the scanning electron microscope;
step S400, adjusting an EBSD sample stage according to a built-in CCD camera of the scanning electron microscope to enable the surface normal of a standard single crystal sample in an image obtained by the CCD camera and the plane normal of the EBSD probe to be in the same plane;
s500, selecting standard electron beam acceleration voltage and beam current for imaging to obtain an EBSD pattern;
step S600, defining a reference coordinate system based on the sample carrier;
step S700, acquiring the surface crystal grain orientation of a standard single crystal sample based on the EBSD pattern, and calculating the Euler angle between a standard sample crystal coordinate system and a reference coordinate system;
and S800, adjusting the sample stage based on the Euler angle to enable the included angle of the Euler angle to be the minimum value, finishing orientation calibration and obtaining a final image of the sample to be detected.
In some preferred embodiments, the step S200 specifically includes:
if the sample to be detected is a block sample, arranging the sample to be detected on a T-shaped table; when the surface to be detected is a side surface, the T-shaped table is arranged on the T-shaped table position 6 of the first vertical surface 2, and when the surface to be detected is a top surface, the T-shaped table is arranged on the T-shaped table position 6 of the second vertical surface 3;
if the sample to be detected is a nano-scale powder sample, arranging the sample to be detected on a carrier net or a carbon supporting film, and fixing the sample to be detected on a limiting pressure ring position 10 of a copper carrier fixing plate; if the to-be-detected mode is the transmission mode, the copper carrier fixing plate is arranged on the copper carrier fixing plate site 801 of the first vertical surface 2; if the mode to be measured is the reflection mode, the copper carrier fixing plate is arranged on the copper carrier fixing plate site 801 of the second vertical surface 3;
the standard single crystal sample is fixed on the standard single crystal sample site by a conductive tape so that the standard single crystal sample is parallel to the second vertical surface 3.
In some preferred embodiments, the step S300 is specifically:
starting an electron gun, horizontally moving a sample to be detected to a position right below the electron gun, and adjusting the height of the sample to be detected to enable the sample to appear in the center of a scanning electron microscope image;
and inserting the EBSD probe to a preset position of the electron microscope, so that the normal direction of the EBSD probe is aligned with the sample to be detected.
In some preferred embodiments, the step S500 is specifically: and (3) selecting a standard electron beam acceleration voltage of 15-30kV and a beam current of 5-10nA, finding out an image area of a standard single crystal sample, and obtaining an EBSD pattern.
In some preferred embodiments, the reference coordinate system is defined by:
the reference coordinate system is obtained by defining the sample roll direction RD as the x-axis, the sample transverse direction TD as the y-axis, and the sample normal direction ND as the z-axis.
In some of the preferred embodiments of the present invention,
the Euler angle acquiring method comprises the following steps:
three primary crystal directions of EBSD-patterned crystal grains are taken as coordinate axes
Obtaining a standard sample crystal coordinate system along the direction, performing first rotation on the standard sample crystal coordinate system along a Z axis, performing second rotation by taking an X axis of the standard sample crystal coordinate system after the first rotation as a rotating shaft, and performing third rotation by taking a Z axis of the standard sample crystal coordinate system after the second rotation as a rotating shaft to obtain a coordinate axis XYZ coincident with a coordinate axis XYZ of a reference coordinate system, wherein a rotating angle of the first rotation, a rotating angle of the second rotation and a rotating angle of the third rotation are Euler angles respectively
、
And
。
in some preferred embodiments, the step S800 specifically includes:
the R axis of the EBSD sample platform is taken as a rotating shaft, the pose of the EBSD sample platform is adjusted, and the rotating angle and the Euler angle on the R axis are recorded
The Euler angle is selected
Taking the position of the EBSD sample stage corresponding to the rotation angle on the R axis when the value is the minimum value as a first calibration position;
the T axis of the EBSD sample platform is taken as a rotating shaft, the pose of the EBSD sample platform is adjusted, and the rotating angle and the Euler angle on the T axis are recorded
The Euler angle is selected
Taking the position of the EBSD sample stage corresponding to the rotation angle on the T axis when the value is the minimum value as a second calibration position;
and when the first calibration position and the second calibration position are met, finishing orientation calibration and obtaining a final sample image to be detected.
In some preferred embodiments, the method further includes a step of performing imaging observation through a scanning electron microscope after orientation calibration, specifically:
after correction, the surface normal of the sample to be detected and the surface normal of the EBSD probe are positioned on the same plane, and the grain orientation distribution diagram and the surface single grain orientation of the sample to be detected are obtained through the EBSD pattern and can be connected with the macroscopic force application direction of the sample.
The invention has the beneficial effects that:
(1) the method calibrates the sample to be tested by the orientation of the standard single crystal sample, and provides accurate data for the analysis of the relative relationship between the subsequent crystal grain orientation of the sample to be tested and the macroscopic stress loading direction;
(2) the invention collects the back scattering electron diffraction (EBSD) patterns of rock samples and metal alloy tensile samples with specific orientations, can represent the orientations of crystal grains, and establishes the relationship between the crystal grain orientations and macroscopic orientations (such as tensile directions) in three-dimensional space. The method makes it possible to establish the relation between the specific grain orientation and the macroscopic orientation of the sample to be measured, and provides a reliable basis for the analysis of the deformation process and the tensile property of the sample by the relation between the force application direction and the grain orientation.
Drawings
Other features, objects and advantages of the present application will become more apparent upon reading of the following detailed description of non-limiting embodiments thereof, made with reference to the accompanying drawings in which:
FIG. 1 is a schematic structural diagram of an EBSD sample stage based on orientation calibration correction in an embodiment of the present invention;
FIG. 2 is a schematic structural diagram of a copper carrier mounting plate according to an embodiment of the present invention;
FIG. 3 is a schematic diagram of a limiting pressure ring according to an embodiment of the invention;
FIG. 4 is a schematic view of a butyl station in an embodiment of the invention;
FIG. 5 is a schematic flow chart of an EBSD image acquisition method based on orientation calibration correction according to an embodiment of the present invention;
FIG. 6 is a schematic view of the orientation of the T-shaped mounting table in the embodiment of the present invention;
FIG. 7 is a schematic diagram of a copper carrier fixing plate placed on a sample stage according to an embodiment of the present invention;
FIG. 8 is a schematic diagram illustrating the effect of placing the copper carrier fixing plate on the sample stage according to the embodiment of the present invention;
FIG. 9 is a schematic diagram illustrating the effect of adjusting the image position according to the embodiment of the present invention;
FIG. 10 is a schematic diagram showing the effect of the EBSD pattern in the example of the present invention;
FIG. 11 is a graph showing the R-axis rotation angle and
the relationship between the angle and the recorded T-axis rotation angle
Schematic representation of the relationship between angles.
Detailed Description
The present application will be described in further detail with reference to the following drawings and examples. It is to be understood that the specific embodiments described herein are merely illustrative of the invention and are not to be construed as limiting the invention. It should be noted that, for convenience of description, only the portions related to the related invention are shown in the drawings.
It should be noted that the embodiments and features of the embodiments in the present application may be combined with each other without conflict. The present application will be described in detail below with reference to the embodiments with reference to the attached drawings.
The invention provides an EBSD sample stage based on orientation calibration correction, which provides accurate data for analyzing the relative relationship between the grain orientation and the macroscopic stress loading direction of a subsequent sample to be detected and provides a reliable basis for analyzing the deformation process and the tensile property of the sample by the relation between the force application direction and the grain orientation.
The invention relates to an EBSD sample platform based on orientation calibration correction, which comprises: a column 1, a first vertical surface 2 and a second vertical surface 3;
the first vertical surface 2 and the second vertical surface 3 are perpendicular to the right-angle boundary 4, and the included angle between the first vertical surface 2 and the horizontal plane is within a preset included angle range; the first vertical surface 2 is 20 degrees with the horizontal direction, and the second vertical surface 3 is 70 degrees with the horizontal direction;
at the right angle where the first vertical surface 2 and the second vertical surface 3 intersect, copper carrier fixing plate sites 801 are arranged, and the copper carrier fixing plate sites 801 are grooves with bottom surfaces parallel to the first vertical surface 2 or the second vertical surface 3 and are overlapped with the right angle boundary 4 at the same position;
one side of the copper carrier fixing plate site 801 on the second vertical surface 3 is provided with a rectangular groove as a standard single crystal sample site 5; the other side of the copper carrier fixing plate site 801 on the second vertical surface 3 and the corresponding position on the second vertical surface 3 are provided with a T-shaped platform site 6; the T-shaped platform position points 6 are two intersected cylindrical slots in the normal direction of the first vertical surface 2 and the second vertical surface 3;
a fixing screw hole 7 is arranged on one side of the column body 1 close to the T-shaped table position 6.
In order to more clearly describe the EBSD sample stage based on the alignment calibration, the following describes in detail each structural component in the embodiment of the present invention with reference to fig. 1.
The EBSD sample platform based on orientation calibration correction of the first embodiment of the invention comprises a step cylinder 1, a first vertical surface 2 and a second vertical surface 3, wherein the structural components are described in detail as follows:
the first vertical surface 2 and the second vertical surface 3 are perpendicular to the right-angle boundary 4, the included angle between the first vertical surface 2 and the horizontal plane is within a preset included angle range, the preset included angle range is a set included angle range which can meet detection of a transmission mode and a reflection mode at the same time, preferably 10-40 degrees, and the included angle between the second vertical surface 3 and the horizontal plane can be selected within 50-80 degrees; the image quality is best when the first vertical surface 2 and the horizontal direction form an angle of 20 degrees, and the second vertical surface 3 and the horizontal direction form an angle of 70 degrees; the diameter of the cylinder in this example was chosen to be 25 mm.
Copper carrier fixing plate sites 801 are arranged at right angles where the first vertical surface 2 and the second vertical surface 3 intersect, the copper carrier fixing plate sites 801 are grooves with bottom surfaces parallel to the first vertical surface 2 or the second vertical surface 3, copper carrier fixing plate screw positions are arranged in the grooves and coincide with the right-angle boundary 4 at the same position;
the copper carrier fixing plate 8 is configured as a cuboid fixing plate as shown in fig. 2, and a copper carrier fixing plate screw hole 9 and a limiting pressing ring site 10 are arranged on the cuboid fixing plate; the limiting compression ring is shown in fig. 3, a screw hole 9 of the copper carrier fixing plate is a circular groove, and the center of the circular groove is a circular through structure with a diameter smaller than that of the circular groove; spacing clamping ring site 10 is the combination of two circular recesses and a banded recess, and one of them circular recess cuts with the edge of cuboid fixed plate mutually, and the centre of a circle of the circular recess that is close to copper carrier fixed plate screw hole 9 is the link up structure the same with copper carrier fixed plate screw hole 9, and the circular recess that cuts mutually with the edge of cuboid fixed plate is circular link up structure, and link up circular still and cut mutually with the edge of cuboid fixed plate.
One side of the copper carrier fixing plate site 801 on the second vertical surface 3 is provided with a rectangular groove as a standard single crystal sample site 5; the other side of the copper carrier fixing plate site 801 on the second vertical surface 3 and the corresponding position on the second vertical surface 3 are provided with a T-shaped platform site 6; the T-shaped platform position points 6 are two intersected cylindrical slots in the normal direction of the first vertical surface 2 and the second vertical surface 3; the depth of the standard single crystal sample site 5 is 0.3-0.8mm so as to facilitate observation, the observation effect of the standard single crystal sample can be adjusted by customizing the thickness of the silicon wafer in practical application, and the observation effect is good when the depth is 0.5 mm.
A fixed screw hole 7 is arranged at one side of the intersection of two T-shaped table positions 6 of the column body 1; in this embodiment, a screw specification of M1.6 is adopted, and one screw can be used to fix the t-shaped table inserted into the two t-shaped table sites 6. The diameter of the T-shaped platform selected in the embodiment is 13mm, as shown in FIG. 4;
the EBSD image acquiring method based on orientation calibration and correction according to the second embodiment of the present invention is implemented by the above EBSD sample stage based on orientation calibration and correction, and as shown in fig. 5, the method includes:
and S100, obtaining a sample to be detected and a standard single crystal sample.
S200, selecting a sample carrier and placing a sample to be detected according to the size magnitude of the sample to be detected;
arranging the standard single crystal sample on a standard single crystal sample site;
obtaining an assembled sample table;
in this embodiment, the step S200 specifically includes:
the sample to be measured is divided into a block sample and a nano-scale sample, and the block sample is subjected to mechanical polishing, ion polishing or electrolytic polishing and other stepsOf rock, metal or semiconductor, etc. having a smooth surface, the size of which is limited to 1X 1 cm 2 Hereinafter, the height is not more than 1 cm, and it is necessary to stick on a T-type sample stand for use. The nano-scale samples comprise nano-scale flake samples and nano-scale powder samples. Wherein the nanoscale thin slice sample is rock, metal or semiconductor extracted and thinned at a fixed point by a focused ion beam-scanning electron microscope system, the extracted sample is generally placed on a copper cylindrical carrier net, and the size of the thin area for observation is generally 20 × 20 μm 2 The thickness is not more than 200 nm. The nano-level powder sample is a nano-particle sample of metal, compound and the like uniformly dispersed on a carbon supporting film (copper mesh), and the size is generally below 200 nm.
If the sample to be detected is a block sample, arranging the sample to be detected on a T-shaped table; when the surface to be measured is a side surface, the t-shaped stage is disposed on the t-shaped stage site 6 of the first vertical surface 2 as shown in fig. 6 (c), and when the surface to be measured is a top surface, the t-shaped stage is disposed on the t-shaped stage site 6 of the second vertical surface 3 as shown in fig. 6 (d);
if the sample to be detected is a nano-scale powder sample, arranging the sample to be detected on a carrier net or a carbon supporting film, and fixing the sample to be detected on a limiting pressure ring position 10 of a copper carrier fixing plate; if the mode to be tested is the transmission mode, the copper carrier fixing plate is disposed on the first vertical surface 2 as shown in fig. 7 (a) or fig. 8, where fig. 8 (a) is a front view, and the copper carrier fixing plate is disposed on the copper carrier fixing plate site 801 of the first vertical surface 2; fig. 8 (b) is a top view, in which a copper carrier fixing plate and a limiting press ring are respectively fastened by fixing screws, and a carrier net is placed in a circular groove of the limiting press ring; if the mode to be measured is the reflection mode, the copper carrier fixing plate is arranged on the copper carrier fixing plate site 801 of the second vertical surface 3; the grid can be a copper cylindrical grid as shown in fig. 7 (b);
the standard single crystal sample is fixed on the standard single crystal sample site by a conductive tape so that the standard single crystal sample is parallel to the second vertical surface 3. The standard single crystal sample is used for sample orientation calibration and is a single crystal sample with conductivity and a specific crystal face on the surface, and the standard single crystal sample is adopted in the exampleA single crystal silicon sample with a crystal face of (110) and the size limited to 3 x 3mm 2 The thickness is 0.5mm or less.
Step S300, placing the assembled sample stage in a scanning electron microscope and adjusting the assembled sample stage to an imaging position so that the sample stage is positioned in the center of an image of the scanning electron microscope;
in this embodiment, the step S300 specifically includes:
setting the emission direction of an electron gun to be vertical downward, starting the electron gun, horizontally moving a sample to be detected to be right below the electron gun, and adjusting the height of the sample to be detected to enable a sample image to be positioned in the center of a scanning electron microscope image;
and inserting the EBSD probe to a preset position of the electron microscope to enable the normal direction of the EBSD probe to be aligned with the sample to be detected, as shown in figure 9.
And S400, adjusting the EBSD sample stage according to the built-in CCD camera of the scanning electron microscope to enable the surface normal of the standard single crystal sample in the image obtained by the CCD camera and the plane normal of the EBSD probe to be in the same plane. Whether the two parts are in the same plane can be judged by an image recognition method or naked eyes.
Step S500, selecting standard electron beam acceleration voltage and beam current for imaging to obtain an EBSD pattern, as shown in FIG. 10, wherein (a) in FIG. 10 is an EBSD pattern of monocrystalline silicon with a crystal plane (110), and (b) in FIG. 10 is a monocrystalline silicon pattern with a crystal plane (111);
in this embodiment, the step S500 specifically includes: and (3) selecting a standard electron beam acceleration voltage of 15-30kV and a beam current of 5-10nA, finding out an image area of a standard single crystal sample, and obtaining an EBSD pattern.
Step S600, defining a reference coordinate system based on the sample carrier;
in this embodiment, the reference coordinate system is defined by:
the sample roll direction RD is defined as the x-axis, the sample transverse direction TD is defined as the y-axis, and the sample normal direction ND is defined as the z-axis, to obtain a reference coordinate system.
And S700, acquiring the surface crystal grain orientation of the standard single crystal sample based on the EBSD pattern, and calculating the Euler angle between the standard sample crystal coordinate system and the reference coordinate system.
In this embodiment, the euler angle is obtained by:
three primary crystal directions of EBSD-patterned crystal grains are taken as coordinate axes
Obtaining a standard sample crystal coordinate system along the direction, performing first rotation on the standard sample crystal coordinate system along a Z axis, performing second rotation by taking an X axis of the standard sample crystal coordinate system after the first rotation as a rotating shaft, and performing third rotation by taking a Z axis of the standard sample crystal coordinate system after the second rotation as a rotating shaft to obtain a coordinate axis XYZ coincident with a coordinate axis XYZ of a reference coordinate system, wherein a rotating angle of the first rotation, a rotating angle of the second rotation and a rotating angle of the third rotation are Euler angles respectively
、
And
。
step S800, adjusting an EBSD sample stage based on the Euler angle to enable the EBSD sample stage to be in a state of being in contact with the Euler angle
The angle is the minimum value, orientation calibration is completed, and a final sample image to be detected is obtained;
in this embodiment, the step S800 specifically includes:
the position and the posture of the EBSD sample stage are adjusted by taking the R axis of the EBSD sample stage as a rotating shaft, and the rotating angle and the Euler angle on the R axis are recorded
The value relationship of (a) is selected from the Euler angle
Angle of rotation on the R-axis at minimumThe position of the EBSD sample stage is used as a first calibration position;
the T axis of the EBSD sample platform is taken as a rotating shaft, the pose of the EBSD sample platform is adjusted, and the rotating angle and the Euler angle on the T axis are recorded
The Euler angle is selected
Taking the position of the EBSD sample stage corresponding to the rotation angle on the T axis when the value is the minimum value as a second calibration position;
and when the first calibration position and the second calibration position are met, finishing orientation calibration and obtaining a final sample image to be detected.
In this embodiment, the R axis is vertical and is along the firing direction of the electron gun when properly positioned; the T axis is horizontal and is perpendicular to the emission direction of the electron gun and the normal direction of the EBSD probe when being correctly placed. The angle of rotation along the R-axis and the T-axis is controllable and readable internally by the scanning electron microscope.
As shown in fig. 11, the R axis rotation angle and
the angle is 0.7 DEG, the minimum included angle is 0.7 DEG when the angle is 111.3 DEG, the T-axis rotation angle is equal to
The angle is 0.3 DEG when the angle is-4 DEG, and the angle is the smallest
And when the angle is less than 0.5 degrees, the normal direction of the surface crystal grain of the standard single crystal sample is coincided with the Z axis of the coordinate axis of the reference system of the sample table, and the positioning correction is finished. Image acquisition can be performed by a carl zeiss company electron microscope (Crossbeam model 540) with the control software "SmartSEM" that can manipulate the EBSD sample stage to rotate along the R, T axis. The real-time acquisition of EBSD patterns, calculation of Euler angles and acquisition of grain orientation distribution maps can be realized by the control software "Aztec" of EBSD (Oxford Nordlys type) of Oxford corporation.
In this embodiment, the method further includes a step of performing imaging observation by using a scanning electron microscope after orientation calibration, specifically:
after correction, the surface normal of the sample to be detected and the surface normal of the EBSD probe are positioned on the same plane, the grain orientation distribution diagram and the surface single grain orientation of the sample to be detected are obtained through the EBSD pattern, and the connection with the macroscopic force application direction of the sample is established.
It can be clearly understood by those skilled in the art that, for convenience and brevity of description, the specific working process and related description of the system described above may refer to the corresponding process in the foregoing method embodiments, and will not be described herein again.
It can be clearly understood by those skilled in the art that, for convenience and brevity of description, the specific working processes and related descriptions of the storage device and the processing device described above may refer to the corresponding processes in the foregoing method embodiments, and are not described herein again.
Those of skill in the art would appreciate that the various illustrative modules, method steps, and modules described in connection with the embodiments disclosed herein may be implemented as electronic hardware, computer software, or combinations of both, and that programs corresponding to the software modules, method steps may be located in Random Access Memory (RAM), memory, Read Only Memory (ROM), electrically programmable ROM, electrically erasable programmable ROM, registers, hard disk, a removable disk, a CD-ROM, or any other form of storage medium known in the art. To clearly illustrate this interchangeability of electronic hardware and software, various illustrative components and steps have been described above generally in terms of their functionality. Whether such functionality is implemented as electronic hardware or software depends upon the particular application and design constraints imposed on the solution. Skilled artisans may implement the described functionality in varying ways for each particular application, but such implementation decisions should not be interpreted as causing a departure from the scope of the present invention.
The terms "first," "second," and the like are used for distinguishing between similar elements and not necessarily for describing or implying a particular order or sequence.
The terms "comprises," "comprising," or any other variation thereof, are intended to cover a non-exclusive inclusion, such that a process, method, article, or apparatus that comprises a list of elements does not include only those elements but may include other elements not expressly listed or inherent to such process, method, article, or apparatus.
So far, the technical solutions of the present invention have been described in connection with the preferred embodiments shown in the drawings, but it is apparent to those skilled in the art that the scope of the present invention is not limited to these specific embodiments. Equivalent changes or substitutions of related technical features can be made by those skilled in the art without departing from the principle of the invention, and the technical scheme after the changes or substitutions can fall into the protection scope of the invention.
Claims (10)
1. An EBSD sample stage based on orientation calibration correction, the sample stage comprising: the device comprises a column body (1), a first vertical surface (2) and a second vertical surface (3);
the first vertical surface (2) and the second vertical surface (3) are perpendicular to the right-angle boundary (4), and the included angle between the first vertical surface (2) and the horizontal plane is within a preset included angle range;
copper carrier fixing plate sites (801) are arranged at the right angles where the first vertical surface (2) and the second vertical surface (3) are intersected, the copper carrier fixing plate sites (801) are grooves with bottom surfaces parallel to the first vertical surface (2) or the second vertical surface (3), and the copper carrier fixing plate sites and the right-angle boundary (4) are overlapped at the same position;
one side of the copper carrier fixing plate site (801) on the second vertical surface (3) is provided with a rectangular groove as a standard single crystal sample site (5); t-shaped platform sites (6) are arranged on the other side of the copper carrier fixing plate site (801) on the second vertical surface (3) and corresponding positions on the first vertical surface (2); the T-shaped platform point (6) is two intersected cylindrical slots in the normal direction of the first vertical surface (2) and the second vertical surface (3);
a fixing screw hole (7) is arranged on one side of the intersection of the two T-shaped table positions (6) of the column body (1).
2. The EBSD sample stage based on orientation calibration correction according to claim 1, wherein the copper carrier fixing plate (8) is configured as a cuboid fixing plate, and a copper carrier fixing plate screw hole (9) and a position limiting ring position point (10) are arranged on the cuboid fixing plate; the screw hole (9) of the copper carrier fixing plate is a circular groove, and the circle center of the circular groove is a circular through structure with the diameter smaller than that of the circular groove; spacing clamping ring position point (10) are the combination of two circular recesses and a banded recess, and one of them circular recess cuts with the edge of cuboid fixed plate mutually, and the circular recess that is close to copper carrier fixed plate screw hole (9) is spacing clamping ring screw hole (11), and its centre of a circle is the link up structure the same with copper carrier fixed plate screw hole (9), and the circular recess that cuts mutually with the edge of cuboid fixed plate is circular link up structure, and link up circular still and cut mutually with the edge of cuboid fixed plate.
3. An orientation calibration correction-based EBSD image acquisition method, which is implemented by the orientation calibration correction-based EBSD sample stage of any one of claims 1-2, the method comprising:
step S100, obtaining a sample to be detected and a standard single crystal sample;
s200, selecting a sample carrier and placing a sample to be tested according to the size magnitude of the sample to be tested;
arranging the standard single crystal sample on a standard single crystal sample site;
obtaining a sample platform which is assembled;
step S300, placing the assembled sample stage in a scanning electron microscope and adjusting the assembled sample stage to an imaging position so that the sample stage image is in the center of the scanning electron microscope image;
step S400, adjusting an EBSD sample stage according to a built-in CCD camera of the scanning electron microscope to enable the surface normal of a standard single crystal sample in an image obtained by the CCD camera and the plane normal of the EBSD probe to be in the same plane;
s500, selecting standard electron beam acceleration voltage and beam current for imaging to obtain an EBSD pattern;
step S600, defining a reference coordinate system based on the sample carrier;
step S700, acquiring the surface crystal grain orientation of a standard single crystal sample based on the EBSD pattern, and calculating the Euler angle between a standard sample crystal coordinate system and a reference coordinate system;
and S800, adjusting an EBSD sample stage based on the Euler angle to enable the included angle of the Euler angle to be the minimum value, finishing orientation calibration and obtaining a final sample image to be detected.
4. The EBSD image acquisition method based on orientation calibration correction according to claim 3, wherein the step S200 specifically includes:
if the sample to be detected is a block sample, arranging the sample to be detected on a T-shaped table; when the surface to be detected is a side surface, the T-shaped table is arranged on the T-shaped table position point (6) of the first vertical surface (2), and when the surface to be detected is a top surface, the T-shaped table is arranged on the T-shaped table position point (6) of the second vertical surface (3);
if the sample to be detected is a nano-scale powder sample, arranging the sample to be detected on a carrier net or a carbon supporting film, and fixing the sample to be detected on a limiting pressure ring site (10) of a copper carrier fixing plate; if the mode to be tested is a transmission mode, arranging the copper carrier fixing plate on a copper carrier fixing plate site (801) of the first vertical surface (2); if the mode to be measured is a reflection mode, arranging the copper carrier fixing plate on a copper carrier fixing plate site (801) of the second vertical surface (3);
and fixing the standard single crystal sample on a standard single crystal sample position through a conductive adhesive tape, so that the standard single crystal sample is parallel to the second vertical surface (3).
5. The EBSD image acquisition method based on orientation calibration correction according to claim 3, wherein the step S300 specifically includes:
setting the emission direction of an electron gun to be vertical downward, starting the electron gun, horizontally moving a sample to be detected to be right below the electron gun, and adjusting the height of the sample to be detected to enable a sample image to be positioned in the center of a scanning electron microscope image;
and inserting the EBSD probe to a preset position of the electron microscope to enable the normal direction of the EBSD probe to be aligned with the sample to be detected.
6. The EBSD image acquisition method based on orientation calibration correction according to claim 3, wherein the step S500 specifically includes: and (3) selecting a standard electron beam acceleration voltage of 15-30kV and a beam current of 5-10nA, finding out an image area of a standard single crystal sample, and obtaining an EBSD pattern.
7. The EBSD image acquisition method based on orientation calibration correction according to claim 3, wherein the reference coordinate system is defined by:
the reference coordinate system is obtained by defining the sample roll direction RD as the x-axis, the sample transverse direction TD as the y-axis, and the sample normal direction ND as the z-axis.
8. The EBSD image acquisition method based on orientation calibration correction according to claim 3, wherein the Euler angle is acquired by:
three primary crystal directions of EBSD-patterned crystal grains are taken as coordinate axes
Obtaining a standard sample crystal coordinate system along the direction, performing first rotation on the standard sample crystal coordinate system along a Z axis, performing second rotation by taking an X axis of the standard sample crystal coordinate system after the first rotation as a rotating shaft, performing third rotation by taking a Z axis of the standard sample crystal coordinate system after the second rotation as a rotating shaft, obtaining a coordinate axis XYZ coincident with a coordinate axis XYZ of a reference coordinate system, wherein a rotating angle of the first rotation, a rotating angle of the second rotation and a rotating angle of the third rotation are Euler angles respectively
、
And
。
9. the EBSD image acquisition method based on orientation calibration correction according to claim 8, wherein the step S800 specifically includes:
the R axis of the EBSD sample platform is taken as a rotating shaft, the pose of the EBSD sample platform is adjusted, and the rotating angle and the Euler angle on the R axis are recorded
The Euler angle is selected
Taking the position of the EBSD sample stage corresponding to the rotation angle on the R axis when the position is the minimum value as a first calibration position;
the T axis of the EBSD sample platform is taken as a rotating shaft, the pose of the EBSD sample platform is adjusted, and the rotating angle and the Euler angle on the T axis are recorded
The Euler angle is selected
Taking the position of the EBSD sample stage corresponding to the rotation angle on the T axis when the value is the minimum value as a second calibration position;
and when the first calibration position and the second calibration position are met, finishing orientation calibration and obtaining a final image of the sample to be detected.
10. The method for acquiring the EBSD image based on orientation calibration and correction according to claim 3, further comprising a step of performing imaging observation by a scanning electron microscope after orientation calibration, specifically:
after correction, the surface normal of the sample to be detected and the surface normal of the EBSD probe are positioned on the same plane, the grain orientation distribution diagram and the surface single grain orientation of the sample to be detected are obtained through the EBSD pattern, and the connection with the macroscopic force application direction of the sample is established.
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