CN213580739U - Objective table and microscope for transmission-electron back scattering diffraction analysis of slice sample - Google Patents
Objective table and microscope for transmission-electron back scattering diffraction analysis of slice sample Download PDFInfo
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- CN213580739U CN213580739U CN202022187549.XU CN202022187549U CN213580739U CN 213580739 U CN213580739 U CN 213580739U CN 202022187549 U CN202022187549 U CN 202022187549U CN 213580739 U CN213580739 U CN 213580739U
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Abstract
The utility model relates to the field of analysis and test of scanning electron microscopes, and provides an objective table and a microscope for transmission-electron back scattering diffraction analysis of a slice sample, wherein the objective table comprises a supporting base, a sample supporting seat, an upper clamping piece, a hollow elastic body, a first threaded fastener and a second threaded fastener; one end of the sample supporting seat is fixed on the supporting base through a first threaded fastener, and a first groove, a second groove and a third groove are formed in the upper portion of the other end of the sample supporting seat; 2 slice samples are respectively placed in the first groove and the second groove, and the third groove is matched with the upper clamping piece; the upper clamping piece fixes 2 slice samples, and the second threaded fastener penetrates through the upper clamping piece and the hollow elastic body in sequence to be fixed on the sample supporting seat. The utility model has simple and reasonable structure, and convenient operation of loading and unloading samples; 2 samples are loaded at a time, so that the observation efficiency is high; elastic clamping, and the sample is not damaged in the loading and unloading process; the allowed sample diffraction analysis range is large; no interference signal is mixed, and the analysis result is reliable.
Description
Technical Field
The utility model relates to a scanning electron microscope analysis and test field, in particular to an objective table that is used for thin slice sample transmission-electron back of body diffraction analysis.
Background
In 1913, the bragg diffraction phenomenon is proposed by william-larens bragg and william-henlebox, and bragg diffraction is generated after an incident electron beam interacts with a crystal material sample in an electron microscope, so that the bragg law is followed, and the crystallographic information of the material can be obtained by using bragg diffraction signals. In a Scanning Electron Microscope (SEM), Electron Back Scattering Diffraction (EBSD) of a block sample, namely reflected electron diffraction information, is mainly utilized, the diffraction analysis area size is hundreds of nanometers to several centimeters, the detection space solid angle is large, the angular resolution is high, but the spatial resolution is slightly poor, and the scanning electron microscope has no capability of detecting a fine structure below hundreds of nanometers; the Transmission Electron Microscope (TEM) mainly utilizes transmission electron diffraction information of an analysis area with the thickness of a slice sample being less than 100nm, the spatial resolution reaches 0.1nm, and information such as tiny precipitated phases, dislocation substructures, dislocation density distribution and the like can be accurately measured, but the analysis area is small, the angular resolution is low, only local crystal information can be obtained, and particularly, the statistical property of the test result is poor when the inhomogeneous deformation microstructure is researched.
Transmission Kikuchi Diffraction (TKD) is a new method for SEM to perform crystal structure and orientation imaging analysis of electron transmission thin sample by using transmission electrons. The sheet sample for TEM observation is observed in SEM to collect transmitted electron diffraction information for material crystallography analysis, and the two analysis methods have the advantages of high spatial resolution, high angular resolution and wide analysis area. Meanwhile, signals such as reflection electron diffraction patterns, secondary electrons, back scattered electrons and the like can be collected, general scanning analysis is carried out on the transmission sample, and the analysis has higher spatial resolution than that of a block material due to the fact that the depth of action of the transmission sample and an electron beam is small.
Unlike the typical scanning sample without the requirement of external dimension, the transmission sample is generally a slice sample with the diameter of 3mm, and the electron diffraction analysis also requires that the sample has a certain tilting angle relative to the electron beam, and has certain requirement on a stage for loading the sample.
The traditional loading mode is that a sample is directly adhered to an objective table with a certain tilting angle by using viscose, and the mode is difficult to ensure that the analysis surface of the sample is strictly positioned on an inclined plane with a specific angle; elastic viscose such as carbon viscose also easily causes sample drift in the analysis process; because the sample is thin, the bonded sample is difficult to remove from the objective table, and even if the bonded sample is removed, the bonded sample can not be deformed, so that the bonded sample can not be used for secondary analysis of TEM or SEM.
SUMMERY OF THE UTILITY MODEL
The utility model aims at solving the defects of the prior art and providing an objective table for transmission-electron back scattering diffraction analysis of a slice sample.
The utility model adopts the following technical scheme:
an object stage for transmission-electron back scattering diffraction analysis of a thin slice sample, the object stage comprising a support base, a sample support base, an upper clamping piece, a hollow elastic body, a first threaded fastener and a second threaded fastener;
the supporting base is a supporting member of the sample supporting seat, and is matched with the sample supporting seat to realize pre-tilt of a tested sample and realize mounting connection with a scanning electron microscope base;
one end of the sample supporting seat is fixed on the supporting base through the first threaded fastener; the upper surface of the sample supporting seat and the horizontal plane form a set angle;
a first groove, a second groove and a third groove are formed in the upper part of the other end of the sample supporting seat; the first groove and the second groove are respectively used for placing 2 slice samples, and the third groove is matched with the upper clamping piece; the first groove and the second groove are symmetrically arranged relative to the third groove;
the upper clamping piece is used for fixing 2 slice samples, and the second threaded fastener sequentially penetrates through the upper clamping piece and the hollow elastic body from top to bottom and is fixed on the sample supporting seat; the hollow elastic body is used for elastically clamping the sheet sample.
Furthermore, a first step is arranged at the top of the supporting base, a second step matched with the first step is arranged at the bottom of the sample supporting seat, the movement between the sample supporting seat and the supporting base is limited when the first step and the second step are clamped, and the first step and the second step are fixed through the first threaded fastener.
Further, the set angle is 20 °.
Further, the top surface of the first step is a first inclined surface, and an included angle between the first inclined surface and the horizontal plane is 20 degrees; a second inclined plane is arranged perpendicular to the first inclined plane, and the first inclined plane and the second inclined plane form a 90-degree step structure; the first inclined plane is provided with 1 first countersunk threaded hole matched with the first threaded fastener; the first inclined surface limits the pre-tilt angle of the sample supporting seat, and the second inclined surface is matched with the first inclined surface to limit the orientation of the sample supporting seat;
the sample supporting seat is integrally of a long sheet structure, and the upper clamping piece, the hollow elastic body and the second threaded fastener are arranged at the top of the sample supporting seat; the second step comprises a third inclined surface and a fourth inclined surface, the third inclined surface is matched with the first inclined surface, and the fourth inclined surface is matched with the second inclined surface; the third inclined plane is strictly parallel to the upper surface of the sample supporting seat, so that the upper surface of the sample supporting seat reaches a set orientation and a set inclination angle; the middle part of second step sets up first countersunk screw hole, and first threaded fastener passes through first countersunk screw hole fixed first step and second step.
Furthermore, the first groove, the second groove and the third groove have the same groove depth and are communicated with each other; the first groove and the second groove are used for respectively placing 1 sheet sample, the shape and the size are the same, the size is slightly larger than the outer size of the sheet sample, and the groove depth value design principle is that an incident path of an incident electron beam to the central area of the sheet sample is not blocked;
through holes for transmission electrons to pass through are formed in the middle parts of the first groove and the second groove, and the shape and size of each through hole are designed according to the principle that the emergent path of the transmission electrons passing through the central area of the sheet sample is not blocked; the third groove is matched with the upper clamping piece, a second countersunk threaded hole is formed in the end part of the third groove, and the second threaded fastener fixes the upper clamping piece and the sample supporting seat through the second countersunk threaded hole;
and the screwing-in depth of the second threaded fastener is adjusted to control the compression degree of the hollow elastic body, so that the upper clamping piece can clamp or unload the tested sample.
Further, the first threaded fastener and the second threaded fastener are both screws.
Furthermore, the upper clamping piece is a long and narrow thin sheet, one end of the upper clamping piece is provided with 1 cylindrical boss with a through hole at the center, the cylindrical boss is matched with the countersunk head of the third groove, and the cylindrical boss can slide up and down in the countersunk head of the third groove.
Further, the hollow elastic body is in a hollow column shape or an annular shape, the outer diameter of the hollow elastic body is slightly smaller than the countersunk head of the third groove, the inner diameter of the hollow elastic body is slightly larger than the second threaded fastener, and the hollow elastic body is placed in the countersunk head of the third groove.
Further, the hollow elastic body is a rubber ring or a spring.
Furthermore, the bottom of the supporting base is provided with a cylindrical nail which is connected and matched with the base of the scanning electron microscope.
Furthermore, the whole supporting base is cylindrical or semi-cylindrical and is made of copper.
A microscope comprising the stage for transmission-electron back-scattered diffraction analysis of a thin slice sample as described above.
The utility model has the advantages that: 2 slice samples can be loaded at one time through one upper clamping piece; compared with the mode of fastening the sample by the viscose, the utility model can take down the sample only by loosening the upper clamping piece, which is very convenient, and can not damage the sample, and the tested sample can be used for secondary analysis; the position of the upper clamping piece is adjusted through the rubber ring with excellent elasticity, so that the clamping degree of the sample is controllable; the central area of the slice sample has no signal interference of a sample supporting seat, and the diffraction pattern has no additional background influence; the upper clamping piece only clamps the slice sample in the edge range, the central area of the sample is not affected at all, and the area for electron back reflection diffraction analysis can be equal to the analysis area of the sample in a transmission electron microscope; rational in infrastructure, convenient operation is simple, and the sample observation efficiency is high, and effective analysis is regional big, and is controllable to the tight degree of clamp of sample, and the handling process is to the sample not damaged, has guaranteed the accuracy and the reliability of sample analysis result.
Drawings
Fig. 1 is a schematic perspective view of a stage for transmission-electron back scattering diffraction analysis of a thin slice sample according to an embodiment of the present invention.
Fig. 2 is a schematic cross-sectional view of an exemplary stage.
FIG. 3 is a schematic structural diagram of a sample holder according to an embodiment.
FIG. 4 is a schematic diagram of an exemplary embodiment of a transmission-electron backscatter diffraction analysis application of the stage.
Wherein: 1-a support base; 101-a first step; 2-sample support base; 201-a first groove; 202-a third groove; 203-a second groove; 204-a second countersunk threaded hole; 205-a first countersunk threaded hole; 206-a second step; 3-a first screw; 4, upper clamping piece; 5-rubber ring; 6-a second screw; 7-first sheet sample; 8-second sheet sample.
Detailed Description
Specific embodiments of the present invention will be described in detail below with reference to the accompanying drawings. It should be noted that technical features or combinations of technical features described in the following embodiments should not be considered as being isolated, and they may be combined with each other to achieve better technical effects.
As shown in fig. 1 and fig. 2, an objective table for transmission-electron backscatter diffraction analysis of a thin slice sample according to an embodiment of the present invention includes a supporting base 1, a sample supporting base 2, a first screw (first screw fastening member) 3, an upper clamping piece 4, a rubber ring 5, and a second screw (second screw fastening member) 6. The design of this example is based on 2 circular flake samples 7, 8 of 3mm diameter commonly used with transmission electron microscopy.
The whole supporting base 1 is semi-cylindrical, copper with good conductivity is selected as a material, the material is consistent with a copper grid commonly used by a transmission electron microscope sample, and interference of more elements on sample analysis is avoided. The top of the supporting base 1 is provided with a first step 101 with an angle of 90 degrees, an included angle of 20 degrees is formed between a first inclined plane (step surface) of the first step 101 and a horizontal plane, and a first countersunk head threaded hole 205 is formed in the center of the first inclined plane (step surface) of the first step 101 and matched with the first screw 3. The bottom of the supporting base 1 is provided with a cylindrical nail which is connected and matched with the base of the scanning electron microscope.
As shown in fig. 3, the sample holder 2 is a round rectangular sheet structure, and a second step 206 with an angle of 90 ° is disposed at the bottom of one end, and the surface of the step is strictly parallel to the upper surface. The second step 206 is centrally provided with a first countersunk threaded hole 205 which is fitted with the first screw 3. The second step 206, in cooperation with the first step 101, defines the orientation and tilt angle of the sample support platform 2. After the sample supporting seat 2 is fixed on the supporting base 1 through the first screw 3, the sample supporting seat 2 is pre-tilted by 20 degrees relative to the horizontal plane.
The top of the other end of the sample support base 2 is provided with a first groove 201, a second groove 203 and a third groove 202. The third groove 203 is located at the center line of the sample support seat 2, the first groove 201 and the second groove 203 are symmetrically distributed at two sides of the end part of the third groove 202, and the first groove 201, the second groove 203 and the third groove 202 are communicated and have the same groove depth. The first groove 201 and the second groove 203 are both circular, the diameter of each groove is slightly larger than 3mm, each groove is used for placing a circular sheet sample 7 and 8 with the diameter of 3mm, the sheet samples have 20-degree inclination angles relative to the horizontal plane, and the 20-degree tilting requirement of the transmission-electron backscatter diffraction analysis of the sheet samples is met. In the centers of the first groove 201 and the second groove 203, a circular through hole with the diameter of 2.4mm is respectively arranged, the projection range of the circular through hole on the sheet samples 7 and 8 is an analyzable area of the samples, and the exit path of electrons after the electron beams incident in the area pass through the samples is not blocked and interference signals are not generated on the sample supporting seat 2. Under the perpendicular projection direction of the first groove 201 and the second groove 203, a part of the material of the support base 1 is removed, further avoiding the generation of interference signals originating from the support base 1. The basic shape of the third recess 202 is a rounded rectangle, which fits the upper jaw 4. One end of the third recess 202 is provided with a second countersunk threaded hole 204, wherein the threaded hole is engaged with the second screw 6.
The upper clamping piece 4 is basically in the shape of a round-corner rectangular thin slice, and one end of the upper clamping piece is provided with a cylindrical boss with a through hole at the center. The upper jaw 4 cooperates with the third groove 202 while pressing on top of the edges of the sheet samples 7 and 8, and functions to secure the sheet samples 7 and 8. The cylindrical boss is matched with the countersunk head of the second countersunk head threaded hole 204, and the cylindrical boss can move up and down in the countersunk head of the second countersunk head threaded hole 204.
The hollow elastic body selects the rubber ring 5, the outer diameter of the rubber ring 5 is slightly smaller than the countersunk diameter of the second countersunk head threaded hole 204, the inner diameter of the rubber ring 5 is slightly larger than the second screw 6, and the rubber ring is placed in the countersunk head of the second countersunk head threaded hole 204.
The second screw 6 is matched with a threaded hole of the second countersunk head threaded hole 204, sequentially passes through a central hole of the cylindrical boss and the center of the rubber ring 5 from top to bottom, and is fixed on the sample supporting seat 2.
The rubber ring 5 and the second screw 6 are matched with the upper clamping piece 4 to realize the loading and unloading of the sample, the compression degree of the upper clamping piece 4 to the rubber ring 5 is controlled through the screwing-in depth of the second screw 6, and then the clamping or loosening of the upper clamping piece 4 to the thin slice samples 7 and 8 is controlled.
The transmission-electron backscatter diffraction analysis application of the stage in the examples is shown in figure 4.
The utility model has simple and reasonable structure, and convenient operation of loading and unloading samples; 2 samples can be loaded at one time, and the observation efficiency is high; elastic clamping, and no damage to the sample in the loading and unloading processes; the allowed sample diffraction analysis range is large; no interference signal is mixed, and the analysis result of the sample is reliable.
While several embodiments of the present invention have been presented herein, it will be appreciated by those skilled in the art that changes can be made to the embodiments herein without departing from the spirit of the invention. The above-described embodiments are merely exemplary and should not be taken as limiting the scope of the invention.
Claims (10)
1. An object stage for transmission-electron back scattering diffraction analysis of a slice sample, which is characterized by comprising a supporting base, a sample supporting seat, an upper clamping piece, a hollow elastic body, a first threaded fastener and a second threaded fastener;
one end of the sample supporting seat is fixed on the supporting base through the first threaded fastener; the upper surface of the sample supporting seat and the horizontal plane form a set angle;
a first groove, a second groove and a third groove are formed in the upper part of the other end of the sample supporting seat; the first groove and the second groove are respectively used for placing 2 slice samples, and the third groove is matched with the upper clamping piece; the first groove and the second groove are symmetrically arranged relative to the third groove;
the upper clamping piece is used for fixing 2 slice samples, and the second threaded fastener sequentially penetrates through the upper clamping piece and the hollow elastic body from top to bottom and is fixed on the sample supporting seat; the hollow elastic body is used for elastically clamping the sheet sample.
2. The stage of claim 1, wherein the support base is provided with a first step at a top portion thereof, the sample holder is provided with a second step at a bottom portion thereof, the first step and the second step are engaged to limit movement between the sample holder and the support base, and the first step and the second step are fixed by the first threaded fastener.
3. The stage for transmission-electron back-scattered diffraction analysis of a thin flake sample according to claim 1 or 2, wherein the set angle is 20 °.
4. The stage of claim 2, wherein the top surface of the first step is a first slope, and the first slope is at an angle of 20 ° to the horizontal; a second inclined plane is arranged perpendicular to the first inclined plane, and the first inclined plane and the second inclined plane form a 90-degree step structure; the first inclined plane is provided with 1 first countersunk threaded hole matched with the first threaded fastener;
the sample supporting seat is integrally of a long sheet structure, and the upper clamping piece, the hollow elastic body and the second threaded fastener are arranged at the top of the sample supporting seat; the second step comprises a third inclined surface and a fourth inclined surface, the third inclined surface is matched with the first inclined surface, and the fourth inclined surface is matched with the second inclined surface; the first threaded fastener fixes the first step and the second step through the first countersunk head threaded hole.
5. The stage according to claim 1, wherein the first, second and third grooves have the same groove depth and are connected to each other;
through holes for transmission electrons to pass through are formed in the middle parts of the first groove and the second groove; the third groove is matched with the upper clamping piece to fix the slice sample, a second countersunk threaded hole is formed in the end part of the third groove, and the second threaded fastener fixes the upper clamping piece and the sample supporting seat through the second countersunk threaded hole;
and the screwing-in depth of the second threaded fastener is adjusted to control the compression degree of the hollow elastic body, so that the upper clamping piece can clamp or unload the tested slice sample.
6. The stage according to claim 1, wherein the upper clamping plate is an elongated thin plate and has 1 cylindrical boss with a through hole at its center at one end, the cylindrical boss is engaged with the countersunk head of the third groove, and the cylindrical boss can slide up and down in the countersunk head of the third groove.
7. The stage of claim 1, wherein the hollow elastomer is a hollow cylinder or ring with an outer diameter slightly smaller than the countersunk head of the third recess and an inner diameter slightly larger than the second threaded fastener, and the hollow elastomer is disposed within the countersunk head of the third recess.
8. The stage for transmission-electron back-scattered diffraction analysis of a thin sheet sample according to claim 1, wherein the hollow elastomer is a rubber ring or a spring.
9. The stage for transmission-electron back-scattered diffraction analysis of a thin slice sample according to claim 1, wherein the bottom of the support base is provided with cylindrical pins for coupling with the base of a scanning electron microscope.
10. A microscope comprising a stage for transmission-electron back-scattered diffraction analysis of a thin slice sample as claimed in any one of claims 1 to 9.
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| Application Number | Priority Date | Filing Date | Title |
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| CN202022187549.XU CN213580739U (en) | 2020-09-29 | 2020-09-29 | Objective table and microscope for transmission-electron back scattering diffraction analysis of slice sample |
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| CN202022187549.XU CN213580739U (en) | 2020-09-29 | 2020-09-29 | Objective table and microscope for transmission-electron back scattering diffraction analysis of slice sample |
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| CN213580739U true CN213580739U (en) | 2021-06-29 |
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN113588696A (en) * | 2021-09-28 | 2021-11-02 | 中铝材料应用研究院有限公司 | Sample pre-tilt loading device for EBSD experiment |
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2020
- 2020-09-29 CN CN202022187549.XU patent/CN213580739U/en active Active
Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN113588696A (en) * | 2021-09-28 | 2021-11-02 | 中铝材料应用研究院有限公司 | Sample pre-tilt loading device for EBSD experiment |
| CN113588696B (en) * | 2021-09-28 | 2021-12-17 | 中铝材料应用研究院有限公司 | Sample pre-tilt loading device for EBSD experiment |
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