CN213423022U

CN213423022U - Slice sample clamping device for EBSD test

Info

Publication number: CN213423022U
Application number: CN202021769179.4U
Authority: CN
Inventors: 吴园园; 金传伟; 胡显军
Original assignee: Jiangsu Shagang Group Co Ltd; Jiangsu Shagang Iron and Steel Research Institute Co Ltd
Current assignee: Jiangsu Shagang Group Co Ltd; Jiangsu Shagang Iron and Steel Research Institute Co Ltd
Priority date: 2020-08-23
Filing date: 2020-08-23
Publication date: 2021-06-11
Anticipated expiration: 2030-08-23

Abstract

The utility model relates to a thin slice sample clamping device is used in EBSD test for solve present thin slice sample and be difficult to the centre gripping, the poor problem that can't carry out the EBSD test of edge conductivity. This clamping device includes: the clamping device comprises a clamping surface, a clamping arm, a slewing bearing bolt, a fixing screw, a fixing nut and a base. The utility model discloses a slewing bearing bolt fastening is passed through to two clamping faces, and two clamping faces pass through the centre gripping arm and are connected with two bases respectively, and two vertical faces keep parallel, and is different according to sample thickness, adjusts two fixed screw nuts for reaching the purpose of fixed sample. And after grinding and polishing the sample, directly fixing the sample and the clamping device on a special sample table for a scanning electron microscope to finish the EBSD test. The utility model discloses system appearance is fast, and the testing process is stable, and the test result is reliable.

Description

Slice sample clamping device for EBSD test

Technical Field

The utility model belongs to scanning electron microscope laboratory sample clamping device field, in particular to thin slice sample clamping device is used in EBSD test.

Background

The Electron Back Scattering Diffraction (EBSD) technology can simultaneously obtain the micro-morphology, the structure and the orientation distribution of the crystal material, and is widely applied to the field of material analysis. In different types of sample testing, the sample holding device plays a crucial role in the accuracy of the test result. The traditional method for preparing a thin section sample is to inlay by using resin and then polish. In the method, the edge of the sheet sample is in direct contact with the resin, the edge conductivity is poor, and the following defects exist: (1) when the full thickness analysis is carried out, the EBSD edge calibration rate is low; (2) when the high power structure EBSD is tested, the image jitter causes the crystal grains to be distorted and deformed. The above problems cause low reliability of the collected experimental data, and influence on data judgment in the material analysis process. Therefore, it is necessary to design a sheet sample clamping device for EBSD test to improve the accuracy of the experimental data.

SUMMERY OF THE UTILITY MODEL

The utility model discloses thin slice sample is difficult to the centre gripping to prior art experimentation, and the poor difficult problem that can't carry out the EBSD test of edge conductivity provides a clamping device of thin slice sample is used in EBSD test.

In order to realize the purpose, the utility model discloses a technical scheme be:

a sheet sample holding device for EBSD test comprises: the clamping device comprises a clamping surface, a clamping arm, a slewing bearing bolt, a fixing screw, a fixing nut and a base. Two clamping surfaces of the clamping device are fixed through a slewing bearing bolt, the two clamping surfaces are respectively connected with two bases through clamping arms, two fixed screw nuts are adjusted according to different sample thicknesses to fix samples, and after the samples are prepared, the clamping device is placed in a sample clamping table special for a scanning electron microscope and is fixed through screws.

The two clamping surfaces of the clamping device are fixed together by utilizing a slewing bearing bolt, and the two vertical surfaces of the clamping surfaces are kept parallel.

Furthermore, the two sides of the clamping surface, which are in contact with the sheet sample, are sandwiched by aluminum foil paper, and the two side surfaces of the sheet sample and the two corresponding sides of the clamping surface need to be polished by 1200 # sandpaper, so as to ensure that the clamping surface, the aluminum foil and the side surfaces of the sheet sample are tightly attached.

Furthermore, the upper surface of the clamping surface is kept flush with the analysis surface of the tested slice sample, so that the clamping surface and the aluminum foil can play a role in protecting the side edge of the sample from chamfering after the sample is prepared.

Furthermore, the material of the clamping device needs to have good conductivity, and the hardness of the clamping device is greater than that of the tested slice sample, so that the clamping device can protect the sample in the sample preparation process, and the conductivity is good in the test process.

Further, the two bases are connected by two fixing screws and fixing nuts.

Compared with the prior art, the experimental device has the following beneficial effects:

the utility model discloses a clamping device uses the aluminium foil paper intermediate layer on the both sides of clamping face and the contact of measured sample, can effectively reduce among the conventional art because of inlay the material and lead to electric conductivity poor, the calibration rate low with sample edge direct contact, the image shake leads to the problem of crystalline grain distortion, ensures the reliability of test result. In addition, the device has the advantages of simple structure, convenient operation and strong practicability.

Description of the drawings:

fig. 1 is a schematic view of a sample holding device of the present invention;

FIG. 2 is a schematic view of the clamping device of the present invention clamping a sample;

FIG. 3 is a full-thickness profile of a thin sheet sample to be tested by the clamping device of the present invention;

FIG. 4 is a contrast diagram of EBSD chrysanthemum pool zone for testing the full thickness of the thin sheet sample by the clamping device of the present invention;

FIG. 5 is a topographical view of a sheet sample tested for through thickness by a conventional sample preparation method;

FIG. 6 is a graph of EBSD chrysanthemum pool strip contrast for full thickness of sheet samples tested by conventional sample preparation methods;

FIG. 7 is a contrast chart of EBSD chrysanthemum pool zone for high power tissue orientation analysis by the clamp of the present invention;

FIG. 8 is a contrast chart of EBSD chrysanthemum pool zone of high power tissue orientation analysis by the traditional sample preparation method.

In the figure: 1-clamp clamping surface, 2-clamping arm, 3-pivoting support bolt, 4-fixing screw, 5-fixing nut, 6-base, 7-aluminum foil, 8-slice sample, a-clamp, b-aluminum foil, c-matrix and d-embedding resin.

Detailed Description

The invention is further illustrated with reference to the following figures and examples, which should not be construed as limiting the invention.

Referring to fig. 1 and 2, a sheet sample clamping device for EBSD test includes a clamping surface 1, a clamping arm 2, a rotation support bolt 3, a fixing screw 4, a fixing nut 5, and a base 6; two clamping surfaces 1 of the clamping device are fixed through a slewing bearing bolt 3, two vertical surfaces of the clamping surfaces 1 are kept parallel, the slewing bearing bolt 3 can enable the two clamping surfaces to move according to different sample thicknesses, and the purpose of fixing a sample is achieved by adjusting a base 6 connected with a screw 4 for fixing and a nut 5 for fixing. The both sides that clamping face 1 and thin slice sample 8 contacted need the aluminium foil 7 intermediate layer, and two sides of

thin slice sample

8 and 1 both sides of corresponding clamping face need polish with 1200 # abrasive paper to guarantee that clamping face 1, aluminium foil 7 are inseparable with the side laminating of thin slice sample 8, and the analysis face of thin slice sample 8 and the upper surface of clamping face 1 will keep flushing, in order to ensure that after the sample preparation, clamping face 1 and aluminium foil 7 can play the purpose of protection sample side not chamfer.

Example 1

Selecting a 10mm multiplied by 0.5mm thin silicon steel sample, polishing two side faces of the thin silicon steel sample smoothly, wrapping aluminum foils 7 on two sides, placing the thin silicon steel sample between two clamping faces 1 of a clamping device, adjusting the positions of a fixing screw 4 and a fixing nut 5 according to the thickness of the thin silicon steel sample, and fixing the sample. After the fixing, the sample is polished to meet the EBSD analysis requirement, the sample is subjected to full-thickness EBSD texture analysis, for example, fig. 3 and 4 are respectively a morphology graph and a chrysanthemum pool strip contrast graph after the EBSD analysis, the analysis area in fig. 4 is a rectangular mark area in fig. 3, the brightness of the chrysanthemum pool strip contrast graph represents the quality of the chrysanthemum pool pattern during calibration, the full-thickness contrast of the chrysanthemum pool pattern in fig. 4 is relatively uniform, and the whole calibration rate reaches 95%.

Comparative example 1

In order to compare the utility model discloses the implementation effect of method selects the same thickness sample and utilizes traditional resin to inlay and carry out the EBSD experiment, is the topography map as figure 5, and the both sides direct contact resin of sample, the electric conductivity is poor, and figure 6 is chrysanthemum pond area contrast map after the EBSD analysis, and the analysis area both sides are close to the resin region, and chrysanthemum pond area is very dark, and whole mark rate is only 61%, and the accuracy of data is relatively poor.

Example 2

Select 10mm 1 mm's duplex steel sample, the centre gripping mode is the same with embodiment 1, selects sample scanning area, enlargies 5000 times, carries out high power tissue orientation analysis, figure 7 is the utility model discloses the EBSD chrysanthemum pool area contrast picture that the method carried out high power tissue orientation analysis, picture luminance is even, and the crystalline grain boundary is clear, and the calibration rate reaches 99%.

Comparative example 2

In order to compare the utility model discloses the implementation of method selects the same sample and utilizes traditional resin to inlay and carry out the EBSD experiment, as shown in FIG. 8, and the picture is bright dark inequality, and the image shake leads to crystalline grain distortion, and the calibration rate is only 57%, and data reliability is in doubt.

The present invention can be embodied in other specific forms without departing from the spirit or essential attributes thereof, and it is to be understood that various changes and modifications can be made therein by those skilled in the art without departing from the spirit and scope of the invention as defined in the appended claims.

Claims

1. A sheet sample clamping device for EBSD test is characterized by comprising: the clamping device comprises a clamping surface (1), a clamping arm (2), a rotary support bolt (3), a fixing screw (4), a fixing nut (5) and a base (6); two clamping surfaces (1) of the clamping device are fixed through a slewing bearing bolt (3), the two clamping surfaces (1) are respectively connected with two bases (6) through clamping arms (2), the two bases (6) are fixedly connected through two fixing screws (4) and fixing nuts (5), and a clamping device body is fixed in a special adjustable-width sample clamping table for a scanning electron microscope.

2. The wafer sample clamping device for EBSD testing of claim 1 wherein: two clamping surfaces (1) of the clamping device are fixed together by a slewing bearing bolt (3), and two vertical surfaces of the clamping surfaces (1) are kept parallel.

3. The wafer sample clamping device for EBSD testing of claim 1 wherein: the two clamping surfaces (1) are respectively and fixedly connected with the two bases (6) through the clamping arms (2).

4. The wafer sample clamping device for EBSD testing of claim 1 wherein: both sides of the holding surface (1) in contact with the sheet sample to be measured were polished with 1200-size sandpaper.

5. The wafer sample clamping device for EBSD testing of claim 1 wherein: the material of the clamping device is required to be harder than that of the sample of the slice to be measured.

6. The wafer sample clamping device for EBSD testing of claim 1 wherein: the two bases (6) are connected with a fixing nut (5) through two fixing screws (4).