JPH0287452A - Electroconductive two-side adhesive sheet for electron microscope - Google Patents
Electroconductive two-side adhesive sheet for electron microscopeInfo
- Publication number
- JPH0287452A JPH0287452A JP63240573A JP24057388A JPH0287452A JP H0287452 A JPH0287452 A JP H0287452A JP 63240573 A JP63240573 A JP 63240573A JP 24057388 A JP24057388 A JP 24057388A JP H0287452 A JPH0287452 A JP H0287452A
- Authority
- JP
- Japan
- Prior art keywords
- specimen
- sheet
- conductive
- openings
- sample
- 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.)
- Granted
Links
- 239000000853 adhesive Substances 0.000 title claims abstract description 28
- 230000001070 adhesive effect Effects 0.000 title claims description 26
- 239000002904 solvent Substances 0.000 claims abstract description 11
- 239000011231 conductive filler Substances 0.000 claims description 7
- 239000012790 adhesive layer Substances 0.000 claims description 6
- 239000011148 porous material Substances 0.000 claims description 5
- 229920000728 polyester Polymers 0.000 abstract description 3
- 229920003002 synthetic resin Polymers 0.000 abstract description 3
- 239000000057 synthetic resin Substances 0.000 abstract description 3
- 239000003795 chemical substances by application Substances 0.000 abstract description 2
- 239000000945 filler Substances 0.000 abstract 2
- 239000004744 fabric Substances 0.000 abstract 1
- 239000000025 natural resin Substances 0.000 abstract 1
- 229910052751 metal Inorganic materials 0.000 description 5
- 239000004820 Pressure-sensitive adhesive Substances 0.000 description 4
- 239000012535 impurity Substances 0.000 description 4
- 239000000463 material Substances 0.000 description 4
- XEKOWRVHYACXOJ-UHFFFAOYSA-N Ethyl acetate Chemical compound CCOC(C)=O XEKOWRVHYACXOJ-UHFFFAOYSA-N 0.000 description 3
- BQCADISMDOOEFD-UHFFFAOYSA-N Silver Chemical compound [Ag] BQCADISMDOOEFD-UHFFFAOYSA-N 0.000 description 3
- YXFVVABEGXRONW-UHFFFAOYSA-N Toluene Chemical compound CC1=CC=CC=C1 YXFVVABEGXRONW-UHFFFAOYSA-N 0.000 description 3
- 239000002184 metal Substances 0.000 description 3
- 239000002759 woven fabric Substances 0.000 description 3
- 229920000178 Acrylic resin Polymers 0.000 description 2
- 239000004925 Acrylic resin Substances 0.000 description 2
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 description 2
- 239000011888 foil Substances 0.000 description 2
- 239000004745 nonwoven fabric Substances 0.000 description 2
- RYGMFSIKBFXOCR-UHFFFAOYSA-N Copper Chemical compound [Cu] RYGMFSIKBFXOCR-UHFFFAOYSA-N 0.000 description 1
- 239000004593 Epoxy Substances 0.000 description 1
- 244000043261 Hevea brasiliensis Species 0.000 description 1
- 229920000877 Melamine resin Polymers 0.000 description 1
- PXHVJJICTQNCMI-UHFFFAOYSA-N Nickel Chemical compound [Ni] PXHVJJICTQNCMI-UHFFFAOYSA-N 0.000 description 1
- 239000004743 Polypropylene Substances 0.000 description 1
- 239000002174 Styrene-butadiene Substances 0.000 description 1
- 230000015572 biosynthetic process Effects 0.000 description 1
- MTAZNLWOLGHBHU-UHFFFAOYSA-N butadiene-styrene rubber Chemical compound C=CC=C.C=CC1=CC=CC=C1 MTAZNLWOLGHBHU-UHFFFAOYSA-N 0.000 description 1
- 229910052799 carbon Inorganic materials 0.000 description 1
- 230000000052 comparative effect Effects 0.000 description 1
- 238000007796 conventional method Methods 0.000 description 1
- 238000004132 cross linking Methods 0.000 description 1
- 238000001514 detection method Methods 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 239000012777 electrically insulating material Substances 0.000 description 1
- 238000001493 electron microscopy Methods 0.000 description 1
- 239000000835 fiber Substances 0.000 description 1
- 230000005251 gamma ray Effects 0.000 description 1
- 238000010438 heat treatment Methods 0.000 description 1
- 239000012948 isocyanate Substances 0.000 description 1
- 150000002513 isocyanates Chemical class 0.000 description 1
- 239000010410 layer Substances 0.000 description 1
- JDSHMPZPIAZGSV-UHFFFAOYSA-N melamine Chemical compound NC1=NC(N)=NC(N)=N1 JDSHMPZPIAZGSV-UHFFFAOYSA-N 0.000 description 1
- 238000000034 method Methods 0.000 description 1
- 239000000203 mixture Substances 0.000 description 1
- 229920003052 natural elastomer Polymers 0.000 description 1
- 229920001194 natural rubber Polymers 0.000 description 1
- -1 polypropylene Polymers 0.000 description 1
- 229920001155 polypropylene Polymers 0.000 description 1
- 238000004080 punching Methods 0.000 description 1
- 239000011347 resin Substances 0.000 description 1
- 229920005989 resin Polymers 0.000 description 1
- 229910052709 silver Inorganic materials 0.000 description 1
- 239000004332 silver Substances 0.000 description 1
- 239000011115 styrene butadiene Substances 0.000 description 1
- 229920003048 styrene butadiene rubber Polymers 0.000 description 1
- 239000012209 synthetic fiber Substances 0.000 description 1
- 229920002994 synthetic fiber Polymers 0.000 description 1
Abstract
Description
【発明の詳細な説明】
〔産業上の利用分野〕
本発明は、電子顕微鏡用導電性両面粘着シートに関する
ものであり、詳細には、電子屈微鏡で試料を観察する際
、試料を導電状態にして試料載台に貼り付けるための導
電性両面粘着シートに関するものである。Detailed Description of the Invention [Industrial Application Field] The present invention relates to a conductive double-sided adhesive sheet for electron microscopes. This invention relates to a conductive double-sided pressure-sensitive adhesive sheet for attaching to a sample stage.
電子盟微鏡で試料を観察する際は試料を導電状態にして
試料載台に貼り付ける必要がある。従来この試料の貼り
付けには、カーボン粉末混合接着剤または銀粉末混合接
着剤等の通常の導電性接着剤が用いられていた。When observing a sample with an electronic microscope, it is necessary to make the sample conductive and attach it to the sample mount. Conventionally, ordinary conductive adhesives such as carbon powder-mixed adhesives or silver powder-mixed adhesives have been used to attach this sample.
しかしながら、試料を試料載台に貼った接着剤層中に、
接着剤の粘度ｙ＋整に用いられた溶剤が残留したままで
、試料の貼られた試料載台を試料室に入れ、その後試料
室を真空化した際、接着剤層中に残留していた溶剤がガ
ス化して排出する。However, in the adhesive layer that attached the sample to the sample stage,
The viscosity of the adhesive (y +) When the sample stage with the sample attached was placed in the sample chamber with the solvent used to adjust it still remaining, and the sample chamber was then evacuated, the solvent remaining in the adhesive layer was removed. is gasified and emitted.
このガスは試料室内をγりし、電子顕微鏡の観察を困難
にする。This gas creates a gamma ray inside the sample chamber, making observation with an electron microscope difficult.
従って、従来上記の方法においては、接着剤に含有する
溶剤が発揮して接着剤が固化するのを待ってから試料載
台を試料室に入れていた。Therefore, in the conventional method described above, the sample stage was placed in the sample chamber after waiting for the solvent contained in the adhesive to develop and solidify the adhesive.
このように上記従来の接着剤による方法では、試料を試
料載台に接着してから実際に観察するまで待ち時間を要
するという不便があった。As described above, the conventional adhesive method described above has the inconvenience of requiring a waiting time after the sample is adhered to the sample stage until it is actually observed.
また、現在使用されている導電性接着剤は電子顕微鏡の
使用に適するよう組成されていないため、金属系不純物
を含んでいる。そのために電子顕微鏡に付属するＸ線マ
イクロアナライザー等で組成分析する時に、その不純物
が検出されるなめ、バックグランドを意識せざるを得な
い不便もある。Furthermore, the conductive adhesives currently in use are not formulated to be suitable for use with electron microscopes, and therefore contain metallic impurities. Therefore, when the composition is analyzed using an X-ray microanalyzer attached to an electron microscope, impurities are detected, which causes the inconvenience of having to be aware of the background.
本発明者はかかる実情に鑑み、前記の如き問題点を解消
すべく鋭意研究の結果従来の接着剤にかえて、本発明の
導電性両面粘着シートを用いて試料を貼った場合試料を
試料載台に貼り終え次第、試料を試料室にセットし直ち
に試料室を真空にしても溶剤の揮発がないため直ちに電
子謂微鏡のａ察が可能になることを見い出し本発明を完
成したものである。In view of the above circumstances, the inventors of the present invention have conducted extensive research to solve the above-mentioned problems.Instead of using conventional adhesives, the present inventors have found that when a sample is pasted using the conductive double-sided adhesive sheet of the present invention, the sample can be placed on the sample. As soon as the sample is pasted on the stand, the sample is set in the sample chamber and the sample chamber is evacuated immediately, and the solvent does not evaporate, so it has been discovered that a-detection using an electronic microscope is immediately possible, and the present invention has been completed. .
すなわち本発明は複数の開孔を有する絶縁性支持体シー
トの両面および上記開孔中に導電性フィラーを含有し、
溶剤を実質的に含有しない粘着剤層を形成した両面相互
導電性を有する電子顕微鏡用導電性両面粘着シートであ
る。That is, the present invention contains a conductive filler on both sides of an insulating support sheet having a plurality of pores and in the pores,
This is a conductive double-sided pressure-sensitive adhesive sheet for electron microscopy, which has mutual conductivity on both sides and has a pressure-sensitive adhesive layer that does not substantially contain a solvent.
本発明に使用する絶縁性支持体シートは、天然または合
成繊維からなる織布または不織布、ポリエステル等の合
成樹脂フィルム、場合によって紙のシートを使用できる
。これらには後述する導電性フィラーを含有する粘着剤
を塗布したとき、これが侵入充填でき、シート両面を連
通する複数の開孔を設ける必要がある。このため支持体
シートにパンチング加工して必要とする開孔を設けると
よい。また織布を支持体シートとして用いる場合には導
電性フィラー含有粘着剤が侵入しうる程度の開孔を有す
る形の粗い織目のものを用いてもよく、不織布の場合は
単位面積当りの繊維密度を比較釣線にしてやはり上記粘
着剤が侵入しうる開孔を設けるようにしてもよい。The insulating support sheet used in the present invention may be a woven or nonwoven fabric made of natural or synthetic fibers, a synthetic resin film such as polyester, or in some cases a paper sheet. When an adhesive containing a conductive filler, which will be described later, is coated on these, it is necessary to provide a plurality of openings that can penetrate and fill the adhesive and communicate with both surfaces of the sheet. For this reason, it is preferable to punch the support sheet to provide the necessary openings. In addition, when a woven fabric is used as a support sheet, a coarsely woven fabric with pores large enough to allow the conductive filler-containing adhesive to penetrate may be used, and in the case of a non-woven fabric, the number of fibers per unit area It is also possible to use a comparative fishing line for density and provide openings through which the adhesive can penetrate.
これらの場合にはパンチング加工を必要としない、これ
らの材料自体は電気絶縁性材料で構成できる。In these cases, punching is not required, and these materials themselves can be composed of electrically insulating materials.
なお、支持体シートとして金属箔を用いた導電性支持体
シートを採用する場合は、この金属に含まれている不純
物までの多くの金属元素をバックグランドに意識しなけ
ればならないので、かかる支持体シートは本発明におい
ては好ましくない。In addition, when adopting a conductive support sheet using metal foil as the support sheet, it is necessary to be aware of the many metal elements contained in the metal, including impurities, in the background. Sheets are not preferred in this invention.
本発明に用いる導電性フィラーとしては、カーボン粉、
銀粉、銅粉、ニッケル粉等の大きさが０Ｏ−０１μｍ〜
１０μｍの微細な導電性フィラーを用いることができる
が、これらは、観察の際、不純物が検出されない程度の
純度のものでなければならない。The conductive filler used in the present invention includes carbon powder,
The size of silver powder, copper powder, nickel powder, etc. is 00-01 μm ~
Although 10 μm fine conductive fillers can be used, they must be of such purity that no impurities are detected during observation.
また本発明に用いる粘着剤材料としては、アクリル系樹
脂、天然ゴム、スチレン・ブタジェン系樹脂及び必要に
より、イソシアネート、メラミン、エポキシ等のこれら
の架橋硬化剤成分からなる材料が使用できる。Further, as the adhesive material used in the present invention, materials comprising acrylic resin, natural rubber, styrene-butadiene resin, and if necessary, crosslinking curing agent components thereof such as isocyanate, melamine, and epoxy can be used.
（導電性粘着剤の調整）
銀粉 ７０重量部（福山金属
箔粉社製シル：７−トＡＧＣ−８）アクリル樹脂系粘着
剤 ７５重量部（三洋化成社製ポリシック３１
０Ｓ＞
溶剤（トルエン／酢酸エチル＝１／１）８０重量部を非
金属製分散機にて均一に混合分散して本発明の導電性粘
着剤を調製した。(Adjustment of conductive adhesive) Silver powder 70 parts by weight (Sil: 7-T AGC-8 manufactured by Fukuyama Metal Foil & Powder Co., Ltd.) Acrylic resin adhesive 75 parts by weight (Polysic 31 manufactured by Sanyo Chemical Co., Ltd.)
0S> A conductive adhesive of the present invention was prepared by uniformly mixing and dispersing 80 parts by weight of a solvent (toluene/ethyl acetate = 1/1) using a nonmetallic disperser.
（電子顕微鏡用導電性両面粘着シートの形成）！＋１１
ｉＩ性を有するポリプロピレンフィルムの上に、上記の
導電性粘着剤を４０μｍの厚みに均一に塗布し、８０℃
で５分間加熱して溶剤を発揮させた導電性粘着剤層を形
成したものを２枚製作した。(Formation of conductive double-sided adhesive sheet for electron microscopes)! +11
The above conductive adhesive was uniformly applied to a thickness of 40 μm on a polypropylene film having iI properties, and heated at 80°C.
Two sheets were manufactured with a conductive adhesive layer formed by heating for 5 minutes to release the solvent.
次にそのうちの一枚の導電性粘着剤層の面上に開孔を有
する絶縁性支持体シート材料のポリエステルシートを積
重し、更にその上に他の一枚の導電性粘着剤層を積重し
た。しかる後、常温にて２０ｋｇの加重を加えて４８時
間圧着し本発明の電子顕微鏡用導電性両面粘着シートを
形成した。Next, a polyester sheet of an insulating support sheet material having holes is stacked on the surface of one of the conductive adhesive layers, and another conductive adhesive layer is further stacked on top of that. It was heavy. Thereafter, pressure bonding was carried out for 48 hours under a load of 20 kg at room temperature to form the conductive double-sided pressure-sensitive adhesive sheet for electron microscopes of the present invention.
このようにして形成した本発明の粘着シートを用いて試
料を試料載台に′接着して電子顕微鏡で観察したところ
、試料室を真空化した際溶剤の排出がなく、直ちに観察
することができ、また導電性フィラー以外の金属元素の
混入が少ないのでバックグランドを無視して観察するこ
とができた。When a sample was adhered to a sample stage using the adhesive sheet of the present invention thus formed and observed under an electron microscope, it was found that when the sample chamber was evacuated, no solvent was discharged and observation could be made immediately. Furthermore, since there was little mixing of metal elements other than the conductive filler, it was possible to observe the background while ignoring it.
本発明のシートを用いた場合は、従来の導電性接着剤を
用いたときのような待ち時間を要することもなく、また
バックグランドを意識する必要もないので、電子閉微鋪
観察の際試料を貼付るための導電性両面粘着シートとし
て好適である。When using the sheet of the present invention, there is no waiting time required when using conventional conductive adhesives, and there is no need to be aware of the background, so it is possible to It is suitable as a conductive double-sided adhesive sheet for pasting.
特許出願人 神東塗料株式会社Patent applicant Shinto Paint Co., Ltd.
Claims (1)
上記開孔中に導電性フィラーを含有し、溶剤を実質的に
含有しない粘着剤層を形成した両面相互導電性を有する
電子顕微鏡用導電性両面粘着シート。1. For electron microscopes with mutual conductivity on both sides, which contains a conductive filler on both sides of an insulating support sheet having a plurality of pores and in the pores, and forms an adhesive layer that does not substantially contain a solvent. Conductive double-sided adhesive sheet.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| JP63240573A JPH0610968B2 (en) | 1988-09-26 | 1988-09-26 | Conductive double-sided adhesive sheet for electron microscope |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| JP63240573A JPH0610968B2 (en) | 1988-09-26 | 1988-09-26 | Conductive double-sided adhesive sheet for electron microscope |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| JPH0287452A true JPH0287452A (en) | 1990-03-28 |
| JPH0610968B2 JPH0610968B2 (en) | 1994-02-09 |
Family
ID=17061532
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| JP63240573A Expired - Lifetime JPH0610968B2 (en) | 1988-09-26 | 1988-09-26 | Conductive double-sided adhesive sheet for electron microscope |
Country Status (1)
| Country | Link |
|---|---|
| JP (1) | JPH0610968B2 (en) |
Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US5418586A (en) * | 1991-02-22 | 1995-05-23 | Seiko Epson Corporation | Projection type liquid crystal projector |
| FR2772513A1 (en) * | 1996-08-05 | 1999-06-18 | Peter Frasca | Specimen holder for electron microscope, holder supporting many specimen grids |
| DE10227761A1 (en) * | 2002-06-21 | 2004-01-15 | Rjl Micro & Analytic Gmbh | Method for fixing particles on a filter medium, e.g. for electron or stereo-microscopic examination of residual dirt on machine parts, involves treatment with adhesive solution which is then dried to form crosslinks |
-
1988
- 1988-09-26 JP JP63240573A patent/JPH0610968B2/en not_active Expired - Lifetime
Cited By (7)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US5418586A (en) * | 1991-02-22 | 1995-05-23 | Seiko Epson Corporation | Projection type liquid crystal projector |
| US5651599A (en) * | 1991-02-22 | 1997-07-29 | Seiko Epson Corporation | Projection type liquid crystal projector |
| US5988818A (en) * | 1991-02-22 | 1999-11-23 | Seiko Epson Corporation | Projection type liquid crystal projector |
| USRE40296E1 (en) | 1991-02-22 | 2008-05-06 | Seiko Epson Corporation | Projection type liquid crystal projector |
| USRE42740E1 (en) | 1991-02-22 | 2011-09-27 | Seiko Epson Corporation | Projector |
| FR2772513A1 (en) * | 1996-08-05 | 1999-06-18 | Peter Frasca | Specimen holder for electron microscope, holder supporting many specimen grids |
| DE10227761A1 (en) * | 2002-06-21 | 2004-01-15 | Rjl Micro & Analytic Gmbh | Method for fixing particles on a filter medium, e.g. for electron or stereo-microscopic examination of residual dirt on machine parts, involves treatment with adhesive solution which is then dried to form crosslinks |
Also Published As
| Publication number | Publication date |
|---|---|
| JPH0610968B2 (en) | 1994-02-09 |
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