JPH02105038A - Electrolytic polishing device for sample of electronic microscope - Google Patents
Electrolytic polishing device for sample of electronic microscopeInfo
- Publication number
- JPH02105038A JPH02105038A JP25698188A JP25698188A JPH02105038A JP H02105038 A JPH02105038 A JP H02105038A JP 25698188 A JP25698188 A JP 25698188A JP 25698188 A JP25698188 A JP 25698188A JP H02105038 A JPH02105038 A JP H02105038A
- Authority
- JP
- Japan
- Prior art keywords
- sample
- electrolytic polishing
- electrodes
- pincette
- crimping means
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
- Pending
Links
- 238000005498 polishing Methods 0.000 title claims abstract description 41
- 239000007788 liquid Substances 0.000 claims abstract description 15
- 239000000463 material Substances 0.000 claims description 9
- 238000001493 electron microscopy Methods 0.000 claims 1
- 230000007774 longterm Effects 0.000 abstract description 4
- 239000004020 conductor Substances 0.000 abstract description 2
- 239000011521 glass Substances 0.000 abstract description 2
- 238000002788 crimping Methods 0.000 abstract 5
- 239000003792 electrolyte Substances 0.000 abstract 1
- BASFCYQUMIYNBI-UHFFFAOYSA-N platinum Chemical compound [Pt] BASFCYQUMIYNBI-UHFFFAOYSA-N 0.000 description 8
- 229910052697 platinum Inorganic materials 0.000 description 4
- QTBSBXVTEAMEQO-UHFFFAOYSA-N Acetic acid Chemical compound CC(O)=O QTBSBXVTEAMEQO-UHFFFAOYSA-N 0.000 description 3
- 150000002500 ions Chemical class 0.000 description 3
- 239000000243 solution Substances 0.000 description 3
- 239000011248 coating agent Substances 0.000 description 2
- 238000000576 coating method Methods 0.000 description 2
- VLTRZXGMWDSKGL-UHFFFAOYSA-N perchloric acid Chemical compound OCl(=O)(=O)=O VLTRZXGMWDSKGL-UHFFFAOYSA-N 0.000 description 2
- 230000008961 swelling Effects 0.000 description 2
- 229910000831 Steel Inorganic materials 0.000 description 1
- 239000003795 chemical substances by application Substances 0.000 description 1
- 239000004035 construction material Substances 0.000 description 1
- 238000010586 diagram Methods 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 238000011156 evaluation Methods 0.000 description 1
- 238000010438 heat treatment Methods 0.000 description 1
- 229910052751 metal Inorganic materials 0.000 description 1
- 239000002184 metal Substances 0.000 description 1
- 239000011259 mixed solution Substances 0.000 description 1
- 239000002245 particle Substances 0.000 description 1
- 230000002093 peripheral effect Effects 0.000 description 1
- 238000004080 punching Methods 0.000 description 1
- 239000010959 steel Substances 0.000 description 1
Landscapes
- Sampling And Sample Adjustment (AREA)
Abstract
Description
【発明の詳細な説明】
［発明の目的］
（産業上の利用分野）
本発明は、電子顕微鏡用試料を平滑かつ均一に電解研磨
できる電解研磨装置に関する。DETAILED DESCRIPTION OF THE INVENTION [Object of the Invention] (Industrial Application Field) The present invention relates to an electrolytic polishing apparatus that can electrolytically polish an electron microscope sample smoothly and uniformly.
（従来の技術）
一般に、原子炉の構築材料などの材料評価試験において
は、原子炉内の環境を模擬して配置した試験片を所望温
度に加熱しながら、粒子加速器により所定量のイオン照
射を行い、試験片に損傷を与えてボイドを発生させ、ス
エリング（体積膨脹）Ｉｉを測定したり、機械強度試験
を行って材料を評価することや、試験片を原子炉中に埋
め込んで所定量の中性子照射を行った後、この試験片の
スエリング量をｎ１定したり、機械強度試験を行って材
料を評価することが行われている。(Prior art) Generally, in material evaluation tests such as nuclear reactor construction materials, a particle accelerator is used to irradiate a predetermined amount of ions while heating a test piece placed to simulate the environment inside a nuclear reactor to a desired temperature. The test piece can be damaged to generate voids and the swelling (volume expansion) Ii can be measured, mechanical strength tests can be performed to evaluate the material, and the test piece can be embedded in a nuclear reactor to generate a predetermined amount of voids. After neutron irradiation, the material is evaluated by determining the amount of swelling of the test piece as n1 and by performing a mechanical strength test.
上記イオン照射や中性子照射によって試験片が受けた損
傷を調べる場合には、電子顕微鏡による観察が行われる
が、この観察を容易にすると共に観察精度を向上させる
ため、イオン照射や中性子照射を受ける試験片は、その
前に所定の電解研磨処理を施される。即ち、試験片は先
ず機械研磨によって所定の厚さ、例えば２００μ−程度
まで減肉された後、打抜き機により所定の寸法、例えば
３ＩＩφに打抜かれ、その後、試験片の両面は電解研磨
により鏡面状に仕上げられる。In order to investigate the damage caused to a test piece by ion irradiation or neutron irradiation, observation using an electron microscope is performed.In order to facilitate this observation and improve the observation accuracy, tests in which the test piece is subjected to ion irradiation or neutron irradiation are conducted. The piece is previously subjected to a certain electropolishing treatment. That is, the test piece is first reduced to a predetermined thickness, e.g., about 200μ, by mechanical polishing, and then punched out to a predetermined size, e.g., 3IIφ, by a punching machine.Then, both sides of the test piece are electrolytically polished to a mirror-like finish. Finished in.
この電解研磨は、従来から市販のジェット研磨装置やテ
ヌボール等の電解研磨装置により行われている。This electrolytic polishing has conventionally been carried out using a commercially available jet polishing device or an electrolytic polishing device such as Tenu Ball.
（発明が解決しようとする課題）
しかしながら、上述した従来のジェット研磨装置やテヌ
ボールによる電解研磨では、試験片１は、試料ホルダー
の構造上の影響を受けるため、第３図（ａ）、（ｂ）に
示すように、周辺部に薄肉部１ａが形成されると共に、
両面の中央部にも薄肉部１ｂが形成され、凹凸形状に研
磨されてしまうという欠点があった。(Problems to be Solved by the Invention) However, in the electrolytic polishing using the conventional jet polishing device or tenu ball described above, the test piece 1 is affected by the structure of the sample holder, so as shown in FIGS. ), a thin wall portion 1a is formed in the peripheral portion, and
There was a drawback that a thin wall portion 1b was also formed in the center portions of both surfaces, resulting in polishing into an uneven shape.
本発明は上記課題を解決するためになされたもので、表
面が平滑で均一な試験片（試料）を容易に得ることので
きる電子顕微鏡用試料の電解研磨装置を提供することを
目的とするものである。The present invention has been made to solve the above problems, and an object of the present invention is to provide an electrolytic polishing apparatus for electron microscope samples that can easily obtain a test piece (sample) with a smooth and uniform surface. It is.
［発明の構成］
（課題を解決するための手段）
本発明の電子顕微鏡用試料の電解研磨装置は電解研磨液
を収容する容器と、この容器内に配置した一対の陰電極
と、これらの陰電極の間に配置され、電解研磨される試
料の側面部を挟持するとともに、この試料を陽電極とし
て機能させる試料挟持具とからなり、この試料挟持具の
内、少なくとも前記電解研磨液中に浸漬される部分の表
面が前記電解研磨液に容易に溶解されない材料で構成さ
れていることを特徴とするものである。[Structure of the Invention] (Means for Solving the Problems) The electrolytic polishing apparatus for an electron microscope sample of the present invention includes a container containing an electrolytic polishing liquid, a pair of negative electrodes arranged in the container, and a pair of negative electrodes arranged in the container. It consists of a sample holder placed between the electrodes to sandwich the side surface of the sample to be electrolytically polished and for the sample to function as a positive electrode; The surface of the polished portion is made of a material that is not easily dissolved in the electrolytic polishing liquid.
（作用）
上述のように構成した本発明の電解研磨装置においては
、試料はピンセットのような試料挟持具によって側面を
挟持されて電解研磨を受けるので、研磨後の試料の両面
は全面にわたって平滑になる。また、試料挟持具の内、
少なくとも電解研磨液中に浸漬される部分の表面は電解
研磨液によって溶解されないので、長期間の使用に耐え
ることができる。(Function) In the electrolytic polishing apparatus of the present invention configured as described above, the sample is subjected to electrolytic polishing with its sides held by a sample holding tool such as tweezers, so that both surfaces of the sample after polishing are smooth over the entire surface. Become. In addition, among the sample holding tools,
At least the surface of the portion immersed in the electropolishing solution is not dissolved by the electropolishing solution, so it can withstand long-term use.
（実施例） 次に、図面を参照しながら本発明の詳細な説明する。(Example) Next, the present invention will be described in detail with reference to the drawings.
第１図は本発明にかかる電子顕微鏡用試料の電解研磨装
置を例示するもので、ガラスビーカー等からなる容器１
０内には、電解研磨液（例えば、酢酸９：過塩素酸１の
混合液）１１が収容されている＝
この電解研磨液中には、一対の電極１２．１３が所定の
間隔をおき、かつ対向して配置されている。これらの電
極はマイナス電位を与えられ、陰電極として機能する。FIG. 1 illustrates an electrolytic polishing apparatus for electron microscope samples according to the present invention, in which a container 1 consisting of a glass beaker, etc.
0 contains an electrolytic polishing liquid (for example, a mixed solution of 9 parts acetic acid and 1 part perchloric acid) 11 = In this electrolytic polishing liquid, a pair of electrodes 12 and 13 are placed at a predetermined distance, and are placed facing each other. These electrodes are given a negative potential and function as negative electrodes.
また、電解研磨液１１中には陰電極１２．１３のほぼ中
間に試料２が配置される。この試料２はピンセットまた
はそれに類似した形状で導電性材料からなる試料挟持具
１４によって周囲２か所を挟持され、位置決めされると
同時に電気的に接続される。試料挟持具１４にはプラス
電位が与えられ、試料２は陽電極として機能する。Further, the sample 2 is placed in the electropolishing liquid 11 approximately in the middle of the cathode 12.13. The sample 2 is held at two points around the periphery by a sample holding tool 14 having a shape similar to tweezers or a conductive material, and is positioned and electrically connected at the same time. A positive potential is applied to the sample holding tool 14, and the sample 2 functions as a positive electrode.
試料挟持具１４としては、第４図に示すように電解研磨
液１１中に浸漬される部分１４ａの全部または表面が電
解研磨液１１によって容易に溶解されない材料、例えば
白金あるいは白金コーティングで構成されている。As shown in FIG. 4, the sample holder 14 has a portion 14a immersed in the electrolytic polishing liquid 11 made of a material that is not easily dissolved by the electrolytic polishing liquid 11, such as platinum or a platinum coating. There is.
“上述のように構成した本発明の電子顕微鏡用試料の電
解研磨装置においては、陽電極２と導通する試料挟持具
１４と陰電極１２．１３の間に２５〜３０Ｖ程度の直流
電圧が印加され、電解研磨液１１の温度を冷却機により
１０−１２℃に維持して１５秒間程度、電解研磨を行う
。“In the electrolytic polishing apparatus for electron microscope samples of the present invention configured as described above, a DC voltage of about 25 to 30 V is applied between the sample holding tool 14 and the negative electrode 12.13, which are electrically connected to the positive electrode 2. Electrolytic polishing is performed for about 15 seconds while maintaining the temperature of the electrolytic polishing liquid 11 at 10-12° C. using a cooler.
このようにすれば、試料２の両面は第２図に示すように
平滑かつ均一に鏡面研磨され、所望の試験片が得られる
。In this way, both surfaces of the sample 2 are polished to a smooth and uniform mirror finish as shown in FIG. 2, and a desired test piece is obtained.
なお、上記において、試料挟持具１４として、第５図（
ａ）に示すように、全体がスチール製の試料挟持具１５
を使用すると、当初は尖頭状の試料挟持具先端部１５ａ
は電解研磨液１１中に浸漬され、かつプラス電位に保た
れるため、自身も電解研磨によって激しく消耗（溶解）
し、比較的短時間の内に、第５図（ｂ）に示すような形
状となり、試料挟持機能が低下してしまうが、本発明装
置においては、電解研磨液１１中に浸漬される部分１４
ａの全部または表面が電解研磨液１１によって容易に溶
解されない材料、例えば白金あるいは白金コーティング
で構成されているので、長期間の使用に際しても電解研
磨を受けることはなく元のままの試料挟持機能を維持す
る。In addition, in the above, the sample holding tool 14 is shown in FIG.
As shown in a), a sample holder 15 made entirely of steel
When using the sample holder, the tip 15a of the sample holder initially has a pointed shape.
is immersed in the electrolytic polishing solution 11 and kept at a positive potential, so it is also severely consumed (dissolved) by electrolytic polishing.
However, in a relatively short period of time, the shape becomes as shown in FIG. 5(b), and the sample clamping function deteriorates.
Since the whole or surface of a is made of a material that is not easily dissolved by the electrolytic polishing liquid 11, such as platinum or a platinum coating, it will not undergo electrolytic polishing even during long-term use and will retain its original sample holding function. maintain.
なお、上記実施例においては、３■φ程度のディスク状
の試料（金属試験片）を電解研磨する例につき述べたが
、本発明はこれに限定されるものではなく、任意の形状
および寸法の試料の電解研磨に広く適用することができ
る。In the above example, an example was described in which a disk-shaped sample (metal test piece) of about 3 mm diameter was electrolytically polished, but the present invention is not limited to this, and can be applied to any shape and size. It can be widely applied to electrolytic polishing of samples.
また、電解研磨液および試料挟持具の先端部の構成材料
も上記実施例に限定されるものでなく、種々の材料を適
宜組合わせて使用できることは勿論である。Furthermore, the materials constituting the electrolytic polishing liquid and the tip of the sample holder are not limited to the above embodiments, and it goes without saying that various materials can be used in appropriate combinations.
［発明の効果］
以上説明したように、本発明に係る電子顕微鏡用試料の
電解研磨装置によれば、平滑かつ均一に鏡面研磨された
試料を製作できる。また、試料挟持具は長時間の使用に
対しても初期の機能を保持することができる。[Effects of the Invention] As explained above, according to the electrolytic polishing apparatus for electron microscope specimens according to the present invention, it is possible to produce a specimen that has been mirror-polished to a smooth and uniform surface. Further, the sample holder can maintain its initial function even after long-term use.
第１図は本発明装置の概略構成を示す説明図、第２図（
ａ）、（ｂ）は本発明装置によって電解研磨された試料
の形状を示す平面図と縦断面図、第３図（ａ）、（ｂ）
は従来装置によって電解研磨された試料の形状を示す平
面図と縦断面図、第４図は本発明装置において使用され
る試料挟持具の斜視図、第５図（ａ）、（ｂ）は本発明
によらない試料挟持具の形状変化の様子を説明する斜視
図である。
１・・・・・・・・・試料（試験片）
２・・・・・・・・・試料（陽電極）
１０・・・・・・・・・容器
１１・・・・・・・・・電解研磨液
１２．１３・・・陰電極
１４・・・・・・・・・試料挾持具
１５．１５゛・・・試料挟持具。
代理人 弁理士 則 近 憲 佑
ｎ 第子丸 健
第２図 第３図
第４図
（ｃｌ） （ｂ）
第５図FIG. 1 is an explanatory diagram showing the schematic configuration of the device of the present invention, and FIG. 2 (
a) and (b) are a plan view and a vertical cross-sectional view showing the shape of a sample electrolytically polished by the apparatus of the present invention; FIGS. 3(a) and (b)
4 is a perspective view of a sample holding tool used in the device of the present invention, and FIGS. FIG. 3 is a perspective view illustrating how the shape of the sample holder changes, which is not based on the invention. 1... Sample (test piece) 2... Sample (positive electrode) 10... Container 11...・Electrolytic polishing liquid 12.13...Cathode electrode 14...Sample holding tool 15.15゛...Sample holding tool. Agent Patent Attorney Nori Ken Ken Daikomaru Figure 2 Figure 3 Figure 4 (cl) (b) Figure 5
Claims (1)
対の陰電極と、これらの陰電極の間に配置され、電解研
磨される試料の側面部を挟持するとともに、この試料を
陽電極として機能させる試料挟持具とからなり、この試
料挟持具の内、少なくとも前記電解研磨液中に浸漬され
る部分の表面が前記電解研磨液によって容易に溶解され
ない材料で構成されていることを特徴とする電子顕微鏡
用試料の電解研磨装置。A container containing an electrolytic polishing solution, a pair of negative electrodes placed inside the container, and a pair of negative electrodes placed between these negative electrodes to sandwich the side surface of the sample to be electropolished, and to use this sample as the positive electrode. The specimen holder is characterized in that at least the surface of the portion of the sample holder that is immersed in the electrolytic polishing liquid is made of a material that is not easily dissolved by the electrolytic polishing liquid. Electrolytic polishing device for samples for electron microscopy.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| JP25698188A JPH02105038A (en) | 1988-10-14 | 1988-10-14 | Electrolytic polishing device for sample of electronic microscope |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| JP25698188A JPH02105038A (en) | 1988-10-14 | 1988-10-14 | Electrolytic polishing device for sample of electronic microscope |
Publications (1)
| Publication Number | Publication Date |
|---|---|
| JPH02105038A true JPH02105038A (en) | 1990-04-17 |
Family
ID=17300065
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| JP25698188A Pending JPH02105038A (en) | 1988-10-14 | 1988-10-14 | Electrolytic polishing device for sample of electronic microscope |
Country Status (1)
| Country | Link |
|---|---|
| JP (1) | JPH02105038A (en) |
Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JP2006292766A (en) * | 2006-05-31 | 2006-10-26 | Hitachi Ltd | Beam member, and sample processing device and sample extraction method using beam member |
| JP2011133493A (en) * | 2011-03-25 | 2011-07-07 | Hitachi Ltd | Sample processing apparatus |
| JP2016183393A (en) * | 2015-03-26 | 2016-10-20 | Ｊｆｅスチール株式会社 | Electrolytic polishing device and electrolytic polishing method |
| EP4318543A1 (en) * | 2022-08-02 | 2024-02-07 | Leica Mikrosysteme GmbH | Sample holder for holding a sample carrier, handling tool and corresponding methods |
-
1988
- 1988-10-14 JP JP25698188A patent/JPH02105038A/en active Pending
Cited By (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JP2006292766A (en) * | 2006-05-31 | 2006-10-26 | Hitachi Ltd | Beam member, and sample processing device and sample extraction method using beam member |
| JP2011133493A (en) * | 2011-03-25 | 2011-07-07 | Hitachi Ltd | Sample processing apparatus |
| JP2016183393A (en) * | 2015-03-26 | 2016-10-20 | Ｊｆｅスチール株式会社 | Electrolytic polishing device and electrolytic polishing method |
| EP4318543A1 (en) * | 2022-08-02 | 2024-02-07 | Leica Mikrosysteme GmbH | Sample holder for holding a sample carrier, handling tool and corresponding methods |
| WO2024028223A1 (en) * | 2022-08-02 | 2024-02-08 | Leica Mikrosysteme Gmbh | Sample holder for holding a sample carrier, handling tool and corresponding methods |
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