CN110534389B - Resettable sample peg and sample resetting method - Google Patents
Resettable sample peg and sample resetting method Download PDFInfo
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- CN110534389B CN110534389B CN201810512734.6A CN201810512734A CN110534389B CN 110534389 B CN110534389 B CN 110534389B CN 201810512734 A CN201810512734 A CN 201810512734A CN 110534389 B CN110534389 B CN 110534389B
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- 238000000034 method Methods 0.000 title claims abstract description 26
- 230000009466 transformation Effects 0.000 claims description 7
- 239000000853 adhesive Substances 0.000 claims description 3
- 230000001070 adhesive effect Effects 0.000 claims description 3
- 230000000007 visual effect Effects 0.000 abstract description 3
- 238000001514 detection method Methods 0.000 description 1
- 239000011343 solid material Substances 0.000 description 1
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- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01J—ELECTRIC DISCHARGE TUBES OR DISCHARGE LAMPS
- H01J37/00—Discharge tubes with provision for introducing objects or material to be exposed to the discharge, e.g. for the purpose of examination or processing thereof
- H01J37/02—Details
- H01J37/20—Means for supporting or positioning the object or the material; Means for adjusting diaphragms or lenses associated with the support
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- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01J—ELECTRIC DISCHARGE TUBES OR DISCHARGE LAMPS
- H01J37/00—Discharge tubes with provision for introducing objects or material to be exposed to the discharge, e.g. for the purpose of examination or processing thereof
- H01J37/26—Electron or ion microscopes; Electron or ion diffraction tubes
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- Sampling And Sample Adjustment (AREA)
- Analysing Materials By The Use Of Radiation (AREA)
Abstract
The invention discloses a sample resetting method for scanning electron microscope analysis, which comprises the following steps: fixing a sample and two positioning columns on the table-board of the sample pile; recording the coordinates of the observed and analyzed sample micro-area and the coordinates of the central mark points of the top surfaces of the two positioning columns; when the sample is observed and analyzed again, new coordinates of the center marking points on the top surfaces of the two positioning columns are obtained; acquiring new coordinates of a sample micro-area observed and analyzed; and resetting the scanning electron microscope to the micro-area of the sample to be observed and analyzed according to the new coordinates of the micro-area of the sample to be observed and analyzed. The sample resetting method provided by the invention can quickly and accurately reset the sample to the original observation visual field, and meets the repeated observation requirements under certain experimental conditions.
Description
Technical Field
The invention relates to the technical field of sample detection, in particular to a sample pile capable of resetting and a sample resetting method.
Background
The scanning electron microscope is an instrument for microscopic observation and analysis of surface appearance and composition characteristics of solid materials. The sample is usually glued to the sample stub and then fixed to the sample stage of the scanning electron microscope. The microscopic characteristics of different areas of the sample can be observed by controlling a mechanical motor of the scanning electron microscope to move the sample stage.
In some research works, the sample needs to be repeatedly observed under a scanning electron microscope for many times, which requires finding the last observation position. Although the scanning electron microscope can record the three-dimensional coordinates of each observation position and reset, the coordinate values of the scanning electron microscope are changed when the sample is fixed on the sample stage next time, so that the previous coordinate values cannot be used. In this case, the search can generally be performed only by combining local topographical features with the general position of the observation area on the sample. Since the observation scale of the scanning electron microscope is often in the nanometer level, and the observation field is only in the micrometer level, the resetting method is difficult and inefficient.
In the prior art, a method for locating a certain position in a sample is provided, which mainly includes taking a picture of the sample by a camera and calculating coordinates of other interest points according to coordinates of some points in the picture. Some scanning electron microscopes now also incorporate such functionality. However, the positioning function cannot realize the above-mentioned reset function because the photograph and position are changed every time the sample is re-inserted.
Disclosure of Invention
Aiming at the technical problems in the prior art, the invention provides a sample pile capable of resetting and a sample resetting method. According to an aspect of the invention, a sample repositioning method comprises the steps of:
s1, fixing the sample and the two positioning columns on the table-board of the sample pile;
s2, fixing the sample pile bearing the sample and the positioning columns on a sample table of a scanning electron microscope, observing and analyzing the micro-area of the sample by using the scanning electron microscope, and recording the coordinates (x, y) of the micro-area of the sample to be observed and analyzed and the coordinates (x) of the central marking points on the top surfaces of the two positioning columnsa，ya) And (x)b，yb)；
S3, when the sample is observed and analyzed again, the sample pile bearing the sample and the positioning column is fixed on the sample table of the scanning electron microscope again, and new coordinates (x) of the central marking points on the top surfaces of the two positioning columns are obtained through the scanning electron microscopea'，ya') and (x)b'，yb')；
S4, obtaining new coordinates (x) of the mark point of the top surface center of the positioning column according to the plane rectangular coordinate transformation formulaa'，ya') and (x)b'，yb') obtained corresponding to the first observed analysisNew coordinates (x ', y') of the sample micro-area;
and S5, inputting the new coordinates (x ', y') corresponding to the micro-area of the sample observed and analyzed for the first time into a control module of a sample stage of a scanning electron microscope, and moving the observation field of view to the micro-area of the sample corresponding to the micro-area of the sample observed and analyzed for the first time by the scanning electron microscope.
In one implementation, in step S1, the sample is adhered to the sample post by using a conductive adhesive.
In one implementation, the parameters of the coordinate changes are obtained using the following formula:
x0＝x′a-xacosθ+yasinθ
y0＝y′a-xasinθ-yacosθ
where θ is a rotation angle of two coordinate changes (x)0，y0) Is the translation parameter of the coordinate zero point.
In one implementation, the new coordinates (x ', y') of the sample micro-region under observation are obtained using the following formula:
x′＝xcosθ-ysinθ+x0
y′＝xsinθ+ycosθ+y0
in one implementation method, the cross section of the table top of the sample pile is circular, and a connecting line of the two positioning columns passes through the center of the table top of the sample pile.
In one implementation method, the mark point of the positioning column is a cross-shaped wire located at the center of the top surface of the positioning column.
According to another aspect of the present invention, there is provided a repositionable sample post, comprising:
the edge of the end face of the table top is provided with two positioning round holes;
the positioning column is arranged in the positioning round hole;
the sample resetting method using the sample pile comprises the following steps:
s1, fixing the sample and the two positioning columns on the table top of the sample pile;
s2, fixing the sample pile fixed with the sample and the positioning columns on a sample table of a scanning electron microscope, observing and analyzing the micro-area of the sample by using the scanning electron microscope, and recording the coordinates (x, y) of the micro-area of the sample to be observed and analyzed and the coordinates (x) of the central marking points on the top surfaces of the two positioning columnsa，ya) And (x)b，yb)；
S3, when the sample is observed and analyzed again, the sample pile bearing the sample and the positioning column is fixed on the sample table of the scanning electron microscope again, and new coordinates (x) of the two top surface center marking points of the positioning column are obtained through the scanning electron microscopea'，ya') and (x)b'，yb')；
S4, obtaining new coordinates (x) of the mark point of the top surface center of the positioning column according to the plane rectangular coordinate transformation formulaa'，ya') and (x)b'，yb') obtaining new coordinates (x ', y ') corresponding to the sample micro-area of the first observed analysis;
and S5, inputting the new coordinates (x ', y') corresponding to the micro-area of the sample observed and analyzed for the first time into a control module of a sample stage of a scanning electron microscope, and moving the observation field of view to the micro-area of the sample corresponding to the micro-area of the sample observed and analyzed for the first time by the scanning electron microscope.
In one implementation method, a screw is arranged on the circumference of the table top at a position corresponding to the positioning circular hole, and the screw is used for fixing the positioning column in the positioning circular hole.
In one implementation method, a fixing column is arranged at the center of the bottom surface of the table top and can be contained in a fixing hole of a sample table of the scanning electron microscope to fix the sample pile.
In one implementation, the positioning column is located on the table at a height equal to the height of the sample.
Compared with the prior art, the resettable sample pile and the sample resetting method have the advantages that when a scanning electron microscope is used for analyzing a sample, and when the same micro-area of the same sample needs to be observed and analyzed for multiple times, the sample can be quickly and accurately reset to the original observation visual field, and the repeated observation requirements under certain experimental conditions are met.
Drawings
Preferred embodiments of the present invention will be described in detail below with reference to the accompanying drawings. In the figure:
fig. 1 shows a flow chart of a sample resetting method according to the invention.
Fig. 2 is a first schematic view of an observation field of a sample pile carrying a sample and a positioning column in a sample stage of a scanning electron microscope according to an embodiment of the present invention.
Fig. 3 is a second schematic view of an observation field of a sample pile carrying a sample and a positioning column in a sample stage of a scanning electron microscope according to an embodiment of the present invention.
Fig. 4 shows a top view of a repositionable sample post according to an embodiment of the present invention.
Fig. 5 shows a front view of a repositionable sample post according to an embodiment of the present invention.
In the drawings, like parts are provided with like reference numerals. The figures are not drawn to scale.
Detailed Description
The invention will be further explained with reference to the drawings.
As shown in fig. 1, a sample reduction method according to the present invention is shown, comprising the steps of:
s1, fixing the sample and the two positioning columns on the table top of the sample pile;
s2, fixing the sample pile bearing the sample and the positioning columns on a sample stage of a scanning electron microscope, observing and analyzing the micro-area of the sample by using the scanning electron microscope, and recording the coordinates (x, y) of the micro-area of the sample subjected to the observation and analysis and the two positioning columnsCoordinates (x) of the top surface center mark pointa，ya) And (x)b，yb)；
S3, when the sample is observed and analyzed again, the sample pile bearing the sample and the positioning columns is fixed on the sample table of the scanning electron microscope again, and new coordinates (x) of the central marking points of the top surfaces of the two positioning columns are obtained through the scanning electron microscopea'，ya') and (x)b'，yb')；
S4, obtaining new coordinates (x) of the mark point of the top surface center of the positioning column according to the plane rectangular coordinate transformation formulaa'，ya') and (x)b'，yb') obtaining new coordinates (x ', y ') corresponding to the sample micro-area of the first observed analysis;
and S5, inputting the new coordinates (x ', y') corresponding to the micro-area of the sample observed and analyzed for the first time into a control module of a sample stage of a scanning electron microscope, and moving the observation field of view to the micro-area of the sample corresponding to the micro-area of the sample observed and analyzed for the first time by the scanning electron microscope.
When a scanning electron microscope is used for analyzing a sample, and when the same micro-area of the same sample needs to be observed and analyzed for multiple times, the sample resetting method provided by the invention can quickly and accurately reset the sample to the original observation visual field, and meets the repeated observation requirements under certain experimental conditions.
In one embodiment, in step S1, the sample is attached to the sample post by using a conductive adhesive. Preferably, the sample is pasted in the middle position of the sample pile, and the arrangement of the positioning pile cannot be influenced.
In an embodiment, as shown in fig. 2 and 3, fig. 2 and 3 are schematic views of an observation field of view of a sample stage of a scanning electron microscope for the first time placing a sample pile (carrying a sample and a positioning column) and a schematic view of an observation field of view of a sample stage of a scanning electron microscope for the second time placing a sample pile (carrying a sample and a positioning column) respectively. In FIG. 2, A (x)a，ya) And B (x)b，yb) And respectively showing the coordinates of the central marking points of the two positioning columns when the sample pile is placed on the sample table of the scanning electron microscope for the first time. In fig. 3, the coordinate system shown by the broken line is the coordinate system when observed for the first time by the scanning electron microscope, and the coordinate system shown by the solid line isThe coordinate system is the coordinate system A' (x) observed by the scanning electron microscope for the second timea'，ya') and B' (x)b'，yb') respectively shows the coordinates of the central marking points of the two positioning columns when the sample pile is placed on the sample table of the scanning electron microscope for the second time. Using a plane rectangular coordinate transformation formula:
x′＝xcosθ-ysinθ+x0
y′＝xsinθ+ycosθ+y0
and when the sample pile bearing the sample and the positioning column is placed on a sample table of the scanning electron microscope for the second time, obtaining a new coordinate C ' (x ', y ') corresponding to the micro-area of the sample to be observed and analyzed. In the above formula, θ is the rotation angle of the coordinate system twice before and after (x)0，y0) Is a coordinate origin translation parameter.
In the above formula, to obtain the new coordinates C ' (x ', y ') of the micro-region of the sample to be observed and analyzed, sin θ, cos θ, x are first obtained0，y0. Specifically, new coordinates A' (x) of two positioning column top surface center marking pointsa'，ya') and B' (x)b'，yb') are substituted into the above transformation equations, respectively, to obtain:
x′a＝xacosθ-yasinθ+x0
y′a＝xasinθ+yacosθ+y0
x′b＝xbcosθ-ybsinθ+x0
y′b＝xbsinθ+ybcosθ+y0
solving for the above-mentioned xa'，ya'，xb'，ybThe system of equations of' yields:
x0＝x′a-xacosθ+yasinθ
y0＝y′a-xasinθ-yacosθ
the obtained sin theta, cos theta, x0，y0The formulas for x ' and y ' are substituted in order to obtain new coordinates C ' (x ', y ') of the sample micro-area under observation for analysis.
As shown in fig. 2 and 5, a resettable sample post is provided, which can implement the aforementioned sample resetting method, and comprises a table top 1 and two positioning posts 2. The edge of the end face of the table top 1 is provided with two positioning round holes 12, and the positioning columns 2 are arranged in the positioning round holes 12. The height of the positioning column 2 extending out of the table top is equal to the height of the sample 3, so that when the sample is observed under a scanning electron microscope, the pictures of the observation micro-area of the sample 3 and the mark points of the positioning column 2 can be kept clear at the same time.
Preferably, the cross section of the table top 1 of the resettable sample pile is circular, and the line connecting the two positioning columns 2 passes through the center of the table top 1 of the sample pile. The two positioning posts 2 may or may not be symmetrical with respect to the diameter of the sample stub. It can be understood that the line connecting the two positioning pillars 2 may not pass through the center of the table top 1.
In one embodiment, as shown in fig. 2, the mark point of the positioning column 2 is a cross-shaped wire 21 located at the center of the top surface of the positioning column 2.
In one embodiment, the positioning post 2 is fixed in the positioning circular hole 12 of the table top 1 in the following manner. As shown in fig. 2, a screw 11 is provided on the circumference of the table top 1 corresponding to the positioning circular hole 12, and after the positioning column 2 is inserted into the positioning circular hole 12, the screw 11 is tightened to fix the positioning column 2 in the positioning circular hole 12.
In an embodiment, a fixing column 13 is disposed at a central position of the bottom surface of the table top 1, and the fixing column 13 can be accommodated in a fixing hole of a sample stage of a scanning electron microscope to fix a sample pile, so as to ensure that the position of the sample pile under the scanning electron microscope is unchanged during each observation.
The above description is only a preferred embodiment of the present invention, but the scope of the present invention is not limited thereto, and any person skilled in the art can easily make changes or variations within the technical scope of the present invention disclosed, and such changes or variations should be covered within the scope of the present invention. Therefore, the protection scope of the present invention shall be subject to the protection scope of the claims.
Claims (10)
1. A method of sample retrieval comprising the steps of:
s1, fixing the sample and the two positioning columns on the table top of the sample pile;
s2, fixing the sample pile fixed with the sample and the positioning columns on a sample table of a scanning electron microscope, observing and analyzing the micro-area of the sample by using the scanning electron microscope, and recording the coordinates (x, y) of the micro-area of the sample to be observed and analyzed and the coordinates (x) of the central marking points on the top surfaces of the two positioning columnsa，ya) And (x)b，yb)；
S3, when the sample is observed and analyzed again, the sample pile bearing the sample and the positioning column is fixed on the sample table of the scanning electron microscope again, and new coordinates (x) of the two top surface center marking points of the positioning column are obtained through the scanning electron microscopea'，ya') and (x)b'，yb')；
S4, obtaining new coordinates (x) of the mark point of the top surface center of the positioning column according to the plane rectangular coordinate transformation formulaa'，ya') and (x)b'，yb') obtaining new coordinates (x ', y ') corresponding to the sample micro-area of the first observed analysis;
and S5, inputting the new coordinates (x ', y') corresponding to the micro-area of the sample observed and analyzed for the first time into a control module of a sample stage of a scanning electron microscope, and moving the observation field of view to the micro-area of the sample corresponding to the micro-area of the sample observed and analyzed for the first time by the scanning electron microscope.
2. The sample resetting method according to claim 1, wherein in the step S1, the sample is stuck to the sample stub by using a conductive adhesive.
3. The sample resetting method according to claim 2, characterized in that the parameters of the coordinate change are obtained using the following formula:
x0＝x′a-xacosθ+yasinθ
y0＝y′a-xasinθ-yacosθ
where θ is a rotation angle of two coordinate changes (x)0，y0) Is the translation parameter of the coordinate zero point.
4. A method for resetting a sample according to claim 3, characterized in that the new coordinates (x ', y') of the micro-area of the sample under observation and analysis are obtained using the following formula:
x′＝xcosθ-ysinθ+x0
y′＝xsinθ+ycosθ+y0。
5. the method for resetting the sample as claimed in claim 1, wherein the cross section of the table top of the sample post is circular, and the line connecting the two positioning posts passes through the center of the table top of the sample post.
6. The method for repositioning samples as claimed in claim 1, wherein the marking point of the positioning column is a cross-hair located at the center of the top surface of the positioning column.
7. A repositionable sample post, comprising:
the edge of the end face of the table top is provided with two positioning round holes;
the positioning column is arranged in the positioning round hole;
the sample resetting method using the sample pile comprises the following steps:
s1, fixing the sample and the two positioning columns on the table top of the sample pile;
s2, fixing the sample pile fixed with the sample and the positioning columns on a sample table of a scanning electron microscope, observing and analyzing the micro-area of the sample by using the scanning electron microscope, and recording the coordinates (x, y) of the micro-area of the sample to be observed and analyzed and the coordinates (x) of the central marking points on the top surfaces of the two positioning columnsa，ya) And (x)b，yb)；
S3, when the sample is observed and analyzed again, the sample pile bearing the sample and the positioning column is fixed on the sample table of the scanning electron microscope again, and new coordinates (x) of the two top surface center marking points of the positioning column are obtained through the scanning electron microscopea'，ya') and (x)b'，yb')；
S4, obtaining new coordinates (x) of the mark point of the top surface center of the positioning column according to the plane rectangular coordinate transformation formulaa'，ya') and (x)b'，yb') obtaining new coordinates (x ', y ') corresponding to the sample micro-area of the first observed analysis;
and S5, inputting the new coordinates (x ', y') corresponding to the micro-area of the sample observed and analyzed for the first time into a control module of a sample stage of a scanning electron microscope, and moving the observation field of view to the micro-area of the sample corresponding to the micro-area of the sample observed and analyzed for the first time by the scanning electron microscope.
8. The repositionable sample post of claim 7, wherein a screw is disposed on a circumference of the table at a position corresponding to the circular positioning hole, the screw being configured to fix the positioning post in the circular positioning hole.
9. The repositionable sample post according to claim 7, wherein a fixing post is disposed at a center of a bottom surface of the table top, and the fixing post is receivable in a fixing hole of a sample stage of a scanning electron microscope to fix the sample post.
10. The repositionable sample post of claim 7, wherein the positioning post is positioned above the table at a height equal to the height of the sample.
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Families Citing this family (6)
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| CN111610212B (en) * | 2020-06-03 | 2023-04-18 | 成都理工大学 | Scanning electron microscope sample positioning device and method for oil and gas reservoir transformation experiment |
| CN112630242B (en) * | 2020-12-03 | 2023-01-10 | 成都先进金属材料产业技术研究院股份有限公司 | Navigation method for scanning electron microscope sample |
| CN112945996A (en) * | 2021-01-26 | 2021-06-11 | 西安科技大学 | Rapid in-situ comparison method based on scanning electron microscope |
| CN113899920B (en) * | 2021-10-08 | 2022-08-23 | 华南理工大学 | Micro-area positioning and retrieving method |
| CN114203504B (en) * | 2021-11-23 | 2023-10-24 | 百实创(北京)科技有限公司 | Tilting structure of transmission electron microscope sample stage |
| CN117727610B (en) * | 2024-02-07 | 2024-05-03 | 国仪量子技术(合肥)股份有限公司 | Reset control method, device and system for sample stage scanning site and storage medium |
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