CN113176284A - Sample preparation method suitable for radioactive small punch test and transmission electron microscope - Google Patents
Sample preparation method suitable for radioactive small punch test and transmission electron microscope Download PDFInfo
- Publication number
- CN113176284A CN113176284A CN202110301584.6A CN202110301584A CN113176284A CN 113176284 A CN113176284 A CN 113176284A CN 202110301584 A CN202110301584 A CN 202110301584A CN 113176284 A CN113176284 A CN 113176284A
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- cylindrical blank
- blank
- sample
- cutting machine
- electron microscope
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- 230000005540 biological transmission Effects 0.000 title claims abstract description 24
- 238000012360 testing method Methods 0.000 title claims abstract description 24
- 230000002285 radioactive effect Effects 0.000 title claims abstract description 21
- 238000005464 sample preparation method Methods 0.000 title claims abstract description 21
- 238000000034 method Methods 0.000 claims abstract description 10
- 238000005520 cutting process Methods 0.000 claims description 45
- 238000001816 cooling Methods 0.000 claims description 3
- 239000012188 paraffin wax Substances 0.000 claims description 3
- 238000002360 preparation method Methods 0.000 abstract description 2
- 235000012431 wafers Nutrition 0.000 description 6
- 229910003460 diamond Inorganic materials 0.000 description 5
- 239000010432 diamond Substances 0.000 description 5
- 238000012986 modification Methods 0.000 description 2
- 230000004048 modification Effects 0.000 description 2
- 238000005498 polishing Methods 0.000 description 2
- 238000004080 punching Methods 0.000 description 2
- 230000006978 adaptation Effects 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 238000005485 electric heating Methods 0.000 description 1
- 238000002474 experimental method Methods 0.000 description 1
- 239000000463 material Substances 0.000 description 1
- 238000005259 measurement Methods 0.000 description 1
- 230000002035 prolonged effect Effects 0.000 description 1
Images
Classifications
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- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- 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
- G01N23/20—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 by using diffraction of the radiation by the materials, e.g. for investigating crystal structure; by using scattering of the radiation by the materials, e.g. for investigating non-crystalline materials; by using reflection of the radiation by the materials
- G01N23/20008—Constructional details of analysers, e.g. characterised by X-ray source, detector or optical system; Accessories therefor; Preparing specimens therefor
-
- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N2223/00—Investigating materials by wave or particle radiation
- G01N2223/05—Investigating materials by wave or particle radiation by diffraction, scatter or reflection
- G01N2223/056—Investigating materials by wave or particle radiation by diffraction, scatter or reflection diffraction
-
- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N2223/00—Investigating materials by wave or particle radiation
- G01N2223/10—Different kinds of radiation or particles
- G01N2223/102—Different kinds of radiation or particles beta or electrons
Abstract
The invention relates to a sample preparation method suitable for a radioactive small punch test and a transmission electron microscope. The samples of the radioactive small punch test and the transmission electron microscope prepared by the method have uniform thickness and smooth surface. The whole sample preparation process is completed in the hot chamber through the manipulator, so that the operator can be prevented from any radioactive irradiation.
Description
Technical Field
The invention relates to a sample preparation method of a slice sample, in particular to a sample preparation method suitable for a radioactive small punch test and a transmission electron microscope.
Background
In the experiment process, small punch test samples, transmission electron microscope samples and the like generally need to cut sheets with proper thickness from blanks for grinding and polishing, and when the sheets are ground and polished to a specified thickness, small wafers with the diameter of phi 3mm or other diameters are punched from the sheets by using a puncher and are used for small punch tests and transmission electron microscope analysis. For radioactive samples, when the small punch test samples and the transmission electron microscope samples are prepared in the mode, operators are difficult to effectively protect so as to avoid damage of radioactivity to hands, eyes and other parts, for example, in the process of grinding and polishing sample slices, hands are needed to fix and take down the samples from a grinding table, the thickness of the samples needs to be measured, and the small punch test and the transmission electron microscope samples have thin thickness and strict requirements on the thickness of the samples, so that the thickness measurement needs to be repeatedly carried out; in the process of punching the small pieces, a user needs to directly operate the puncher, the small pieces need to be carefully observed in order to avoid wasting polished sheet materials, the irradiation time of an operator is greatly prolonged, certain harm is caused to the body of the operator, and the thickness uniformity of the sample prepared by the method is poor.
Disclosure of Invention
The invention aims to provide a sample preparation method suitable for a radioactive small-punch test and a transmission electron microscope, so that a small-diameter thin slice sample with uniform thickness and smooth surface is obtained, and an operator is prevented from any radioactive irradiation.
The technical scheme of the invention is as follows: a sample preparation method suitable for a radioactive small punch test and a transmission electron microscope is characterized in that a sample blank is operated by a manipulator in a hot chamber, the sample blank is firstly prepared into a cylindrical blank with a specified diameter through a cutting machine, and then the cylindrical blank is cut along the axial direction perpendicular to the cylindrical blank to obtain a wafer sample with a specified thickness.
Further, the sample preparation method suitable for the radioactivity small punch test and the transmission electron microscope specifically comprises the following steps:
(1) fixing a sample blank to be sampled on a cutting machine by a mechanical arm in a hot chamber through a pneumatic clamp;
(2) cutting a sample blank into a cylindrical blank with a projection with a specified diameter by a cutting machine;
(3) the cylindrical blank with the bulge is fixed on the cutting machine again through a pneumatic clamp by using a manipulator;
(4) cutting off the convex part along the axial direction parallel to the cylindrical blank with the convex part by a cutting machine to obtain a regular cylindrical blank;
(5) adhering the regular cylindrical blank to a cylindrical blank base, and fixing the cylindrical blank base on a cutting machine through a pneumatic clamp by utilizing a manipulator;
(6) and cutting along the axial direction perpendicular to the cylindrical blank by a cutting machine to obtain a wafer sample with a specified thickness.
Further, according to the sample preparation method suitable for the small-bore-punch test of radioactivity and the transmission electron microscope, in the step (5), the semi-circular groove matched with the cylindrical blank is formed in the base of the cylindrical blank, and the cylindrical blank is adhered in the semi-circular groove.
Further, according to the sample preparation method suitable for the small radioactive plunger test and the transmission electron microscope, in the step (5), the cylindrical blank base is heated to a certain temperature, paraffin is coated in the semicircular groove, the cylindrical blank is placed in the semicircular groove, and after cooling, the cylindrical blank base is fixed on the cutting machine through the pneumatic clamp by using the manipulator.
Further, in the sample preparation method suitable for the radioactive small-punch test and the transmission electron microscope as described above, the sample blank in the step (1) has a rectangular structure.
Further, the sample preparation method suitable for the radioactive small punch test and the transmission electron microscope as described above, wherein the diameter of the cylindrical blank is 3 mm.
The invention has the following beneficial effects: the sample preparation method suitable for the small radioactive punch test and the transmission electron microscope provided by the invention does not adopt the traditional punching mode, but firstly prepares the blank into a cylindrical shape and then directly cuts the cylindrical blank into a sheet sample. The samples of the radioactive small punch test and the transmission electron microscope prepared by the method have uniform thickness and smooth surface. The whole sample preparation process is completed in the hot chamber through the manipulator, so that the operator can be prevented from any radioactive irradiation.
Drawings
FIG. 1 is a schematic flow chart of a sample preparation method provided in an embodiment of the present invention;
FIG. 2 is a schematic end view of a cylindrical blank with a projection according to an embodiment of the present invention;
fig. 3 is a schematic view of a cylindrical blank base structure in an embodiment of the present invention.
Detailed Description
In order to make the objects, technical solutions and advantages of the present invention more apparent, the present invention is described in further detail below with reference to the accompanying drawings and embodiments. It should be understood that the specific embodiments described herein are merely illustrative of the invention and are not intended to limit the invention.
The invention provides a sample preparation method suitable for a radioactive small punch test and a transmission electron microscope, which is characterized in that a sample blank is operated by a manipulator in a hot chamber, the sample blank is firstly prepared into a cylindrical blank with a specified diameter by a cutting machine, then the cylindrical blank is cut along the axial direction vertical to the cylindrical blank, and a wafer sample with a specified thickness is obtained by cutting, and the sample preparation method specifically comprises the following steps:
(1) fixing a sample blank to be sampled on a cutting machine by a mechanical arm in a hot chamber through a pneumatic clamp;
(2) cutting a sample blank into a cylindrical blank with a projection with a specified diameter by a cutting machine;
(3) the cylindrical blank with the bulge is fixed on the cutting machine again through a pneumatic clamp by using a manipulator;
(4) cutting off the convex part along the axial direction parallel to the cylindrical blank with the convex part by a cutting machine to obtain a regular cylindrical blank;
(5) adhering the regular cylindrical blank to a cylindrical blank base, and fixing the cylindrical blank base on a cutting machine through a pneumatic clamp by utilizing a manipulator;
(6) and cutting along the axial direction perpendicular to the cylindrical blank by a cutting machine to obtain a wafer sample with a specified thickness.
Examples
The embodiment is a sample preparation method suitable for a radioactive small punch test and a transmission electron microscope, and the specific operation flow is shown in fig. 1, and the method comprises the following steps:
(1) in the hot chamber, firstly, the pneumatic clamp is installed at a specific position of the diamond curve cutting machine, then the sample blank 1 to be prepared is placed on the pneumatic clamp on the diamond curve cutting machine by utilizing the manipulator, and the sample blank 1 is clamped by the pneumatic clamp, wherein the sample blank 1 can adopt a rectangular structure in the embodiment.
(2) After clamping the sample blank, a cylindrical blank 2 with a protrusion of phi 3mm can be cut out from the sample blank 1 by setting a diamond curve cutting machine, and the end face of the cylindrical blank is shown in fig. 2. The reason that the cylindrical blank is provided with the bulge is that when the cutting process is finished, the connecting part between the phi 3mm cylinder and the original sample blank is less, so that the phi 3mm cylinder can automatically fall off when the cutting process is not finished, and the axial bulge part can be generated at the falling part, so that the interface of the phi 3mm cylinder in the vertical axial direction is not a regular circle but is provided with a certain bulge.
(3) And (3) re-clamping the cylindrical blank 2 with the convex phi 3mm by using the manipulator, placing a pneumatic clamp, and re-fixing the cylindrical blank 2 with the convex phi 3 mm.
(4) And cutting off the convex part by using a diamond curve cutting machine in parallel to the axial direction of the phi 3mm cylindrical blank with the convex part, thereby obtaining the regular phi 3mm cylindrical blank 3.
(5) The method comprises the steps of placing a cylindrical blank base 5 (shown in figure 3) on an electric heating furnace, smearing paraffin in a semicircular groove of the cylindrical blank base after the cylindrical blank base 5 is heated, enabling the semicircular groove to be matched with the cylindrical blank in size, then placing a phi 3mm cylindrical blank 3 in the semicircular groove of the cylindrical blank base 5, after cooling, enabling the phi 3mm cylindrical blank 3 to be adhered in the semicircular groove of the cylindrical blank base, and then placing the cylindrical blank base on a pneumatic clamp by utilizing a manipulator. The phi 3mm cylindrical blank is adhered to the base of the cylindrical blank, so that the phenomenon that the surface of the thin sheet is uneven due to the fact that the thin sheet is broken in advance when the cutting of the thin sheet is nearly finished can be avoided.
(6) The cylindrical blank base is fixed on a diamond curve cutting machine through a pneumatic clamp, the cutting machine is set, and cutting is performed perpendicular to the axial direction of the phi 3mm cylindrical blank 3, so that a phi 3mm wafer sample 4 with a specified thickness (generally about 0.1-1 mm) can be obtained.
Other embodiments of the invention will be apparent to those skilled in the art from consideration of the specification and practice of the invention disclosed herein. This application is intended to cover any variations, uses, or adaptations of the invention following, in general, the principles of the invention and including such departures from the present disclosure as come within known or customary practice within the art to which the invention pertains. Thus, if such modifications and application-adaptive changes to the present invention are within the scope of the claims of the present invention and their equivalents, the present invention is also intended to include such modifications and application-adaptive changes.
The above-described embodiments are merely illustrative of the present invention, and the present invention may be embodied in other specific forms or other specific forms without departing from the spirit or essential characteristics thereof. The described embodiments are, therefore, to be considered in all respects as illustrative and not restrictive. The scope of the invention should be indicated by the appended claims, and any changes that are equivalent to the intent and scope of the claims should be construed to be included therein.
Claims (6)
1. A sample preparation method suitable for a radioactive small punch test and a transmission electron microscope is characterized in that a sample blank is operated in a hot chamber by a mechanical arm, the sample blank is firstly prepared into a cylindrical blank with a specified diameter through a cutting machine, then the cylindrical blank is cut along the axial direction perpendicular to the cylindrical blank, and a wafer sample with a specified thickness is obtained through cutting.
2. The sample preparation method suitable for the small-punch test of radioactivity and the transmission electron microscope as claimed in claim 1, which comprises the following steps:
(1) fixing a sample blank to be sampled on a cutting machine by a mechanical arm in a hot chamber through a pneumatic clamp;
(2) cutting a sample blank into a cylindrical blank with a projection with a specified diameter by a cutting machine;
(3) the cylindrical blank with the bulge is fixed on the cutting machine again through a pneumatic clamp by using a manipulator;
(4) cutting off the convex part along the axial direction parallel to the cylindrical blank with the convex part by a cutting machine to obtain a regular cylindrical blank;
(5) adhering the regular cylindrical blank to a cylindrical blank base, and fixing the cylindrical blank base on a cutting machine through a pneumatic clamp by utilizing a manipulator;
(6) and cutting along the axial direction perpendicular to the cylindrical blank by a cutting machine to obtain a wafer sample with a specified thickness.
3. The sample preparation method suitable for use in a small radioactive punch test and a transmission electron microscope according to claim 2, wherein in the step (5), the base of the cylindrical blank is provided with a semicircular groove adapted to the cylindrical blank, and the cylindrical blank is adhered to the semicircular groove.
4. The sample preparation method suitable for the radioactive small punch test and the transmission electron microscope according to claim 3, wherein in the step (5), the cylindrical blank base is heated to a certain temperature, paraffin is coated in the semicircular groove, the cylindrical blank is placed in the semicircular groove, and after cooling, the cylindrical blank base is fixed on the cutting machine by a mechanical hand through a pneumatic clamp.
5. The method of claim 2, wherein the sample blank of step (1) is of rectangular configuration.
6. The method of any one of claims 1-5, wherein the cylindrical blank has a diameter of 3 mm.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN202110301584.6A CN113176284A (en) | 2021-03-22 | 2021-03-22 | Sample preparation method suitable for radioactive small punch test and transmission electron microscope |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN202110301584.6A CN113176284A (en) | 2021-03-22 | 2021-03-22 | Sample preparation method suitable for radioactive small punch test and transmission electron microscope |
Publications (1)
| Publication Number | Publication Date |
|---|---|
| CN113176284A true CN113176284A (en) | 2021-07-27 |
Family
ID=76922478
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN202110301584.6A Pending CN113176284A (en) | 2021-03-22 | 2021-03-22 | Sample preparation method suitable for radioactive small punch test and transmission electron microscope |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN113176284A (en) |
Citations (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JP2009192341A (en) * | 2008-02-14 | 2009-08-27 | Sumitomo Metal Mining Co Ltd | Preparation method of sliced sample for transmission electron microscope, and sample stand used therefor |
| CN101579887A (en) * | 2009-06-17 | 2009-11-18 | 江苏高淳陶瓷股份有限公司 | Honeycomb ceramic dry green body dual-blade cutting machine |
| CN105835246A (en) * | 2016-05-14 | 2016-08-10 | 洛阳金诺机械工程有限公司 | Cutting device for crystalline silicon bar and cutting method for cutting device |
| CN107121446A (en) * | 2017-04-25 | 2017-09-01 | 大连交通大学 | A kind of Cross-section transmission tem sample mechanical pre-thinning method |
| CN206561515U (en) * | 2017-01-13 | 2017-10-17 | 许昌天戈硅业科技有限公司 | A kind of Pneumatic clamping device cut for sapphire ingot |
| CN110000436A (en) * | 2019-05-06 | 2019-07-12 | 中国原子能科学研究院 | A kind of wire cutting sample clamp |
-
2021
- 2021-03-22 CN CN202110301584.6A patent/CN113176284A/en active Pending
Patent Citations (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JP2009192341A (en) * | 2008-02-14 | 2009-08-27 | Sumitomo Metal Mining Co Ltd | Preparation method of sliced sample for transmission electron microscope, and sample stand used therefor |
| CN101579887A (en) * | 2009-06-17 | 2009-11-18 | 江苏高淳陶瓷股份有限公司 | Honeycomb ceramic dry green body dual-blade cutting machine |
| CN105835246A (en) * | 2016-05-14 | 2016-08-10 | 洛阳金诺机械工程有限公司 | Cutting device for crystalline silicon bar and cutting method for cutting device |
| CN206561515U (en) * | 2017-01-13 | 2017-10-17 | 许昌天戈硅业科技有限公司 | A kind of Pneumatic clamping device cut for sapphire ingot |
| CN107121446A (en) * | 2017-04-25 | 2017-09-01 | 大连交通大学 | A kind of Cross-section transmission tem sample mechanical pre-thinning method |
| CN110000436A (en) * | 2019-05-06 | 2019-07-12 | 中国原子能科学研究院 | A kind of wire cutting sample clamp |
Non-Patent Citations (1)
| Title |
|---|
| 王贤: ""基于小冲杆试验的超声表面滚压TC4钛合金氢脆行为研究"", 《中国优秀硕士学位论文全文数据库（工程科技I辑）》 * |
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| PB01 | Publication | ||
| PB01 | Publication | ||
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Application publication date: 20210727 |
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| RJ01 | Rejection of invention patent application after publication |