CN114199917A - Hot chamber radioactive sample inlaying method for improving conductivity and inlaying sample - Google Patents
Hot chamber radioactive sample inlaying method for improving conductivity and inlaying sample Download PDFInfo
- Publication number
- CN114199917A CN114199917A CN202111554346.2A CN202111554346A CN114199917A CN 114199917 A CN114199917 A CN 114199917A CN 202111554346 A CN202111554346 A CN 202111554346A CN 114199917 A CN114199917 A CN 114199917A
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- Prior art keywords
- sample
- conductive metal
- conductivity
- resin
- inlaying
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- 238000000034 method Methods 0.000 title claims abstract description 31
- 230000002285 radioactive effect Effects 0.000 title claims abstract description 17
- 239000002184 metal Substances 0.000 claims abstract description 35
- 229910052751 metal Inorganic materials 0.000 claims abstract description 35
- 229920005989 resin Polymers 0.000 claims abstract description 18
- 239000011347 resin Substances 0.000 claims abstract description 18
- 239000000843 powder Substances 0.000 claims abstract description 14
- 239000000701 coagulant Substances 0.000 claims abstract description 7
- RYGMFSIKBFXOCR-UHFFFAOYSA-N Copper Chemical compound [Cu] RYGMFSIKBFXOCR-UHFFFAOYSA-N 0.000 claims description 26
- 239000003822 epoxy resin Substances 0.000 claims description 8
- 229920000647 polyepoxide Polymers 0.000 claims description 8
- VILCJCGEZXAXTO-UHFFFAOYSA-N 2,2,2-tetramine Chemical group NCCNCCNCCN VILCJCGEZXAXTO-UHFFFAOYSA-N 0.000 claims description 3
- 238000010438 heat treatment Methods 0.000 claims description 3
- 229960001124 trientine Drugs 0.000 claims description 3
- 238000012360 testing method Methods 0.000 claims description 2
- 239000004065 semiconductor Substances 0.000 claims 2
- 238000007711 solidification Methods 0.000 claims 1
- 230000008023 solidification Effects 0.000 claims 1
- 238000005530 etching Methods 0.000 abstract description 11
- 238000005498 polishing Methods 0.000 abstract description 6
- 238000000227 grinding Methods 0.000 abstract description 5
- 238000002360 preparation method Methods 0.000 abstract description 5
- 229910052802 copper Inorganic materials 0.000 description 5
- 239000010949 copper Substances 0.000 description 5
- 239000003795 chemical substances by application Substances 0.000 description 2
- 239000000446 fuel Substances 0.000 description 2
- 239000000463 material Substances 0.000 description 2
- 239000011824 nuclear material Substances 0.000 description 2
- 238000003825 pressing Methods 0.000 description 2
- 239000000853 adhesive Substances 0.000 description 1
- 230000001070 adhesive effect Effects 0.000 description 1
- 238000004458 analytical method Methods 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 238000012512 characterization method Methods 0.000 description 1
- 238000012854 evaluation process Methods 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 239000003758 nuclear fuel Substances 0.000 description 1
- 238000007747 plating Methods 0.000 description 1
- 238000012827 research and development Methods 0.000 description 1
- 238000004626 scanning electron microscopy Methods 0.000 description 1
- 238000005507 spraying Methods 0.000 description 1
- 238000006467 substitution reaction Methods 0.000 description 1
Images
Classifications
-
- 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
- G01N23/22—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 measuring secondary emission from the material
- G01N23/2202—Preparing specimens therefor
-
- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N1/00—Sampling; Preparing specimens for investigation
- G01N1/28—Preparing specimens for investigation including physical details of (bio-)chemical methods covered elsewhere, e.g. G01N33/50, C12Q
- G01N1/36—Embedding or analogous mounting of samples
-
- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N1/00—Sampling; Preparing specimens for investigation
- G01N1/28—Preparing specimens for investigation including physical details of (bio-)chemical methods covered elsewhere, e.g. G01N33/50, C12Q
- G01N1/36—Embedding or analogous mounting of samples
- G01N2001/364—Embedding or analogous mounting of samples using resins, epoxy
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- Physics & Mathematics (AREA)
- Health & Medical Sciences (AREA)
- Life Sciences & Earth Sciences (AREA)
- Chemical & Material Sciences (AREA)
- Analytical Chemistry (AREA)
- Biochemistry (AREA)
- General Health & Medical Sciences (AREA)
- General Physics & Mathematics (AREA)
- Immunology (AREA)
- Pathology (AREA)
- Sampling And Sample Adjustment (AREA)
Abstract
The invention discloses a hot-chamber radioactive sample inlaying method for improving conductivity and an inlaying sample, wherein the inlaying method comprises the following steps: before injecting resin and coagulant to cure, scattering a layer of conductive metal powder on the sample, then placing a plurality of conductive metal wires in the embedded sleeve, wherein one end of each conductive metal wire is in contact with the conductive metal powder, and the other end of each conductive metal wire extends out of the solidified resin layer. According to the invention, the conductive metal powder and the conductive metal wire are added into the embedded sleeve, so that the sample and the metal are effectively connected, and the subsequent sample preparation work such as grinding and polishing is not influenced. The conductivity of the embedded sample is greatly improved, and the subsequent electrochemical etching, scanning electron microscope observation and the like of the sample in the hot chamber are ensured.
Description
Technical Field
The invention relates to the technical field of nuclear fuel, in particular to a hot-chamber radioactive sample inlaying method for improving conductivity and an inlaying sample.
Background
In the nuclear material fuel and material research and development and service performance evaluation processes, neutron irradiation examination needs to be carried out, and microscopic characterization such as a scanning electron microscope is carried out on the irradiated radioactive sample. Therefore, the irradiated nuclear material fuel and material samples are subjected to sample preparation such as scanning electron microscopy and the like. Typically, the sample preparation steps include cutting, damascene, polishing, etching, and plating. Wherein, for the manipulator centre gripping and fixed operations such as polish, inlay the indispensable link to the sample. To ensure feasibility and efficiency of operation in hot rooms, inlays typically employ an epoxy resin and a corresponding curing agent. However, epoxy resin has poor conductivity, which seriously affects subsequent electrochemical etching and scanning electron microscope observation.
Therefore, on the premise of fully considering the feasibility and reliability of remote operation in a hot chamber, a simple and feasible method for improving the conductivity of the mosaic sample is urgently needed.
Disclosure of Invention
The invention aims to provide a hot-chamber radioactive mosaic method for improving conductivity, and solves the problem that the conductivity of a hot-chamber radioactive mosaic sample is poor due to the existing pure resin mosaic method.
In addition, the invention also provides a mosaic sample obtained based on the mosaic method.
The invention is realized by the following technical scheme:
a method for inlaying radioactive sample in hot chamber for increasing electric conductivity includes such steps as spraying a layer of electrically conductive metal powder on the sample before resin and solidifying agent are injected, and putting several electrically conductive metal wires in inlaid sleeve tube, where one end of each wire is in contact with electrically conductive metal powder or sample and another end of each wire is extended out of solidified resin layer.
The conductivity of the epoxy resin mosaic sample is low, so that the subsequent electrochemical etching step cannot be carried out, and the representation of a scanning electron microscope is also seriously influenced. The method fully considers the reliability of remote operation in the hot chamber and the convenience of subsequent grinding and polishing operation, and provides a simple and feasible method for improving the conductivity of the radioactive epoxy resin mosaic test sample in the hot chamber.
According to the invention, the conductive metal powder and the conductive metal wire are added into the embedded sleeve, so that the sample and the metal are effectively connected, and the subsequent sample preparation work such as grinding and polishing is not influenced. The conductivity of the embedded sample is greatly improved, and the subsequent electrochemical etching, scanning electron microscope observation and the like of the sample in the hot chamber are ensured.
Further, the conductive metal powder includes copper powder.
Further, the conductive wire comprises a copper wire.
The copper wire not only has conductivity, but also has flexibility, the flexible copper wire does not influence the subsequent steps of mechanical arm clamping, grinding, polishing, pressing and the like, and can ensure the subsequent electrochemical etching and scanning electron microscope observation of the sample in the hot chamber
Further, the adding amount of the conductive metal powder is more than or equal to 500mg, so that the metal copper wire is effectively contacted with the sample.
Because inlay the in-process, can have the sample that partial copper powder and copper wire can't contact, consequently, the metallic copper that adds should the capacity, inlay the completion back, copper wire and sample can effective connection.
Further, the diameter of the conductive wire is 0.5-0.6 mm.
Further, the number of the conductive wires is 30 to 50.
Furthermore, the other end of the conductive metal wire vertically extends out of the resin layer and horizontally extends outwards, so that the conductive metal wire is in an L-shaped structure.
Further, the method comprises the following steps:
s1, placing the sample with the observation surface facing downwards in an embedded sleeve, then scattering conductive metal powder in the embedded sleeve to cover a layer of conductive metal on the upper end surface of the sample, and placing a plurality of conductive metal wires;
s2, heating the resin and the coagulant to 50-60 ℃, and pouring into the embedded sleeve;
and S3, standing until the resin is solidified.
Further, the resin is epoxy resin, and the coagulant is triethylene tetramine.
A mosaic sample prepared by the mosaic method.
Compared with the prior art, the invention has the following advantages and beneficial effects:
1. the method greatly improves the conductivity of the embedded sample by using the metallic copper, is simple to operate and convenient to develop in a hot chamber, and the flexible copper wire does not influence the subsequent steps of clamping, polishing, pressing and the like of a mechanical arm, so that the subsequent electrochemical etching and scanning electron microscope observation of the sample in the hot chamber can be guaranteed.
2. The mosaic method can obtain a radioactive epoxy resin mosaic sample with high conductivity, and meets the requirements of electrochemical etching with applied voltage and scanning electron microscope observation with high magnification (more than 100000).
Drawings
The accompanying drawings, which are included to provide a further understanding of the embodiments of the invention and are incorporated in and constitute a part of this application, illustrate embodiment(s) of the invention and together with the description serve to explain the principles of the invention. In the drawings:
FIG. 1 shows a mosaic sample obtained by the mosaic method 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 further described in detail below with reference to examples and accompanying drawings, and the exemplary embodiments and descriptions thereof are only used for explaining the present invention and are not meant to limit the present invention.
Example 1:
as shown in fig. 1, the method for inlaying radioactive samples in a hot chamber for improving the conductivity comprises the following steps:
s1, placing the sample with the observation surface facing downwards in the center of an embedded sleeve, then scattering about 500mg of copper powder into the embedded sleeve to cover a layer of copper powder on the upper end surface of the sample, placing 30-50 thin copper wires with the length of 4cm and the diameter of 0.5mm, enabling one end of each copper wire to be in contact with the copper powder or the sample, and enabling the other end of each copper wire to extend out of the solidified resin layer;
s2, slightly heating epoxy resin and a coagulant (triethylene tetramine) to 50-60 ℃ (reducing the viscosity of the resin and improving the embedding density), pouring into the embedding sleeve, and controlling the adding amount to reach the top end of the grinding sleeve;
and S3, standing for more than 8 hours, flattening the fine copper on the back surface of the inlaid sample by using a pressure head after the resin is solidified, and enabling the copper wire to be in an L-shaped structural wire, thus finishing the inlaying work.
In the electrochemical etching process, the copper wire on the back of the embedded sample is clamped by the electrode to complete etching. In the analysis process of the scanning electron microscope, the copper wire can be in close contact with the conductive adhesive of the sample stage, so that the electric charge irradiated on the observation surface of the sample is effectively conducted, and the improvement of the shape resolution of the scanning electron microscope is facilitated.
Therefore, this embodiment is through adding metal copper powder, metal copper wire in inlaying the cover pipe, effectively is connected sample and metal copper, promotes the electric conductivity of inlaying the sample by a wide margin, and the simple operation does not influence sample preparation work such as follow-up mill polish simultaneously, can ensure in the hot chamber sample electrochemical etching and scanning electron microscope observation etc..
The above-mentioned embodiments are intended to illustrate the objects, technical solutions and advantages of the present invention in further detail, and it should be understood that the above-mentioned embodiments are merely exemplary embodiments of the present invention, and are not intended to limit the scope of the present invention, and any modifications, equivalent substitutions, improvements and the like made within the spirit and principle of the present invention should be included in the scope of the present invention.
Claims (10)
1. The embedding method of the radioactive sample in the hot chamber for improving the conductivity is characterized in that before resin and a coagulant are injected for solidification, a layer of conductive metal powder is firstly scattered on the sample, then a plurality of conductive metal wires are placed in an embedding sleeve, one end of each conductive metal wire is in contact with the conductive metal powder or the sample, and the other end of each conductive metal wire extends out of a solidified resin layer.
2. The method for enhanced conductivity of hot chamber radioactive specimen inlay of claim 1, wherein said conductive metal powder comprises copper powder.
3. The method of claim 1, wherein the conductive wire comprises copper wire.
4. The method for thermal intracavitary radioactive sample inlay to enhance conductivity of claim 1, wherein said conductive metal powder is added in an amount of 500mg or more.
5. The method of claim 1, wherein the diameter of the conductive wire is 0.5-0.6 mm.
6. The method for hot-chamber radioactive sample inlay of claim 1, wherein the number of the conductive wires is 30 to 50.
7. The method for embedding a radioactive sample in a hot chamber for improving conductivity of a semiconductor device according to claim 1, wherein the other end of the conductive wire extends vertically out of the resin layer and horizontally outward, so that the conductive wire has an L-shaped structure.
8. The method of claim 1, comprising the steps of:
s1, placing the sample with the observation surface facing downwards in an embedded sleeve, then scattering conductive metal powder in the embedded sleeve to cover a layer of conductive metal on the upper end surface of the sample, and placing a plurality of conductive metal wires;
s2, heating the resin and the coagulant to 50-60 ℃, and pouring into the embedded sleeve;
and S3, standing until the resin is solidified.
9. The method for embedding a radioactive sample in a hot chamber for improving conductivity of a semiconductor device according to claim 1, wherein the resin is an epoxy resin and the coagulant is triethylene tetramine.
10. A mosaic test sample prepared by the mosaic process of any one of claims 1 to 9.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN202111554346.2A CN114199917A (en) | 2021-12-17 | 2021-12-17 | Hot chamber radioactive sample inlaying method for improving conductivity and inlaying sample |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN202111554346.2A CN114199917A (en) | 2021-12-17 | 2021-12-17 | Hot chamber radioactive sample inlaying method for improving conductivity and inlaying sample |
Publications (1)
| Publication Number | Publication Date |
|---|---|
| CN114199917A true CN114199917A (en) | 2022-03-18 |
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Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN202111554346.2A Pending CN114199917A (en) | 2021-12-17 | 2021-12-17 | Hot chamber radioactive sample inlaying method for improving conductivity and inlaying sample |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN114199917A (en) |
Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN115684229A (en) * | 2022-09-21 | 2023-02-03 | 哈尔滨工业大学 | Preparation method of micron-sized particle section capable of being repeatedly used for electron microscope observation |
Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN204029761U (en) * | 2014-09-02 | 2014-12-17 | 武汉钢铁(集团)公司 | ESEM is with exempting from conducting resinl sample holder |
| CN105547783A (en) * | 2015-12-30 | 2016-05-04 | 北京钢研高纳科技股份有限公司 | Embedding method for metallographic specimen |
| CN109187128A (en) * | 2018-09-11 | 2019-01-11 | 包头钢铁（集团）有限责任公司 | The preparation method of sample |
-
2021
- 2021-12-17 CN CN202111554346.2A patent/CN114199917A/en active Pending
Patent Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN204029761U (en) * | 2014-09-02 | 2014-12-17 | 武汉钢铁(集团)公司 | ESEM is with exempting from conducting resinl sample holder |
| CN105547783A (en) * | 2015-12-30 | 2016-05-04 | 北京钢研高纳科技股份有限公司 | Embedding method for metallographic specimen |
| CN109187128A (en) * | 2018-09-11 | 2019-01-11 | 包头钢铁（集团）有限责任公司 | The preparation method of sample |
Non-Patent Citations (1)
| Title |
|---|
| 杞居意: "金相试样的环氧树脂镶嵌法", 《理化检验.物理分册》, pages 59 - 60 * |
Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN115684229A (en) * | 2022-09-21 | 2023-02-03 | 哈尔滨工业大学 | Preparation method of micron-sized particle section capable of being repeatedly used for electron microscope observation |
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