JPS62185143A - Preparation of sample for transmission electron microscope - Google Patents
Preparation of sample for transmission electron microscopeInfo
- Publication number
- JPS62185143A JPS62185143A JP2713786A JP2713786A JPS62185143A JP S62185143 A JPS62185143 A JP S62185143A JP 2713786 A JP2713786 A JP 2713786A JP 2713786 A JP2713786 A JP 2713786A JP S62185143 A JPS62185143 A JP S62185143A
- Authority
- JP
- Japan
- Prior art keywords
- paint
- water
- thin film
- water soluble
- sheet
- 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
- 230000005540 biological transmission Effects 0.000 title claims description 8
- 239000003973 paint Substances 0.000 claims abstract description 39
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 23
- 239000010409 thin film Substances 0.000 claims abstract description 16
- 239000010408 film Substances 0.000 claims abstract description 8
- 239000003960 organic solvent Substances 0.000 claims abstract description 7
- 239000011248 coating agent Substances 0.000 claims description 7
- 238000000576 coating method Methods 0.000 claims description 7
- 239000000126 substance Substances 0.000 claims description 6
- 238000005464 sample preparation method Methods 0.000 claims description 5
- 108010025899 gelatin film Proteins 0.000 claims description 4
- 238000004627 transmission electron microscopy Methods 0.000 claims description 2
- 239000002245 particle Substances 0.000 abstract description 13
- 238000000034 method Methods 0.000 abstract description 12
- 239000002952 polymeric resin Substances 0.000 abstract description 10
- 229920003002 synthetic resin Polymers 0.000 abstract description 10
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 abstract description 8
- 229910052799 carbon Inorganic materials 0.000 abstract description 8
- 239000011230 binding agent Substances 0.000 abstract description 7
- 239000006185 dispersion Substances 0.000 abstract description 6
- RYGMFSIKBFXOCR-UHFFFAOYSA-N Copper Chemical compound [Cu] RYGMFSIKBFXOCR-UHFFFAOYSA-N 0.000 abstract description 4
- 229910052802 copper Inorganic materials 0.000 abstract description 4
- 239000010949 copper Substances 0.000 abstract description 4
- 239000000463 material Substances 0.000 abstract description 4
- 238000001704 evaporation Methods 0.000 abstract 1
- 230000008020 evaporation Effects 0.000 abstract 1
- 238000000926 separation method Methods 0.000 abstract 1
- 239000002904 solvent Substances 0.000 description 4
- 238000007796 conventional method Methods 0.000 description 2
- 230000000694 effects Effects 0.000 description 2
- 238000007740 vapor deposition Methods 0.000 description 2
- 108010010803 Gelatin Proteins 0.000 description 1
- 239000002253 acid Substances 0.000 description 1
- 238000005054 agglomeration Methods 0.000 description 1
- 230000002776 aggregation Effects 0.000 description 1
- 230000015572 biosynthetic process Effects 0.000 description 1
- 230000008021 deposition Effects 0.000 description 1
- 230000006866 deterioration Effects 0.000 description 1
- 239000002270 dispersing agent Substances 0.000 description 1
- 238000010828 elution Methods 0.000 description 1
- 238000005516 engineering process Methods 0.000 description 1
- 229920000159 gelatin Polymers 0.000 description 1
- 239000008273 gelatin Substances 0.000 description 1
- 235000019322 gelatine Nutrition 0.000 description 1
- 235000011852 gelatine desserts Nutrition 0.000 description 1
- 239000006247 magnetic powder Substances 0.000 description 1
- 239000012860 organic pigment Substances 0.000 description 1
- 229920005989 resin Polymers 0.000 description 1
- 239000011347 resin Substances 0.000 description 1
- 239000011163 secondary particle Substances 0.000 description 1
- 238000005019 vapor deposition process Methods 0.000 description 1
Landscapes
- Sampling And Sample Adjustment (AREA)
Abstract
Description
【発明の詳細な説明】
産業上の利用分野
本発明は、塗料の分散性評価を目的とした透過電子顕微
鏡試料作成法に関するものである。DETAILED DESCRIPTION OF THE INVENTION Field of Industrial Application The present invention relates to a method for preparing a transmission electron microscope sample for the purpose of evaluating the dispersibility of paint.
従来の技術
従来、透過電子顕微鏡で、塗料の分散性を評価するため
の試料の作成方法は、塗料を担体としてＰＥＴ等の高分
子樹脂シートに塗り、高分子樹脂シートを適当な溶剤で
溶かし、残った塗料薄膜を銅メツシユで掬い上げる方法
か、あるいは高分子樹脂シートに塗り、その上にカーボ
ン蒸着を行ない、カーボン膜を粒子の保持体としておき
、高分子樹脂シートを適当な溶剤で溶かし、残ったカー
ボン膜を銅メツシユで掬い上げる方法が取られていた。Conventional technology Conventionally, the method of preparing a sample for evaluating the dispersibility of paint using a transmission electron microscope is to apply the paint as a carrier to a polymer resin sheet such as PET, dissolve the polymer resin sheet with an appropriate solvent, Either scoop up the remaining thin film of paint with a copper mesh, or apply it to a polymer resin sheet, then deposit carbon on top of it, use the carbon film as a holder for the particles, and dissolve the polymer resin sheet with an appropriate solvent. The method used was to scoop up the remaining carbon film with a copper mesh.
発明が解決しようとする問題点
塗料中には無機物以外にも有機物、例えば有機顔料分散
剤、高分子樹脂であるバインダー等も多く配合されてい
る場合が多いため、従来の方法のように、高分子樹脂シ
ートの担体上に塗料を塗布し、高分子樹脂シートを適当
な溶剤で溶かして塗膜を得る方法では、高分子樹脂シー
トだけではなく塗料成分までが溶剤に溶けてしまい、粒
子が二次凝集、あるいはバラバラになり、本来の塗料中
の粒子の分散状態が観察できないという不都合があった
。まだその問題を改良したカーボン蒸着で粒子を保持す
る方法でも、バインダーの溶出により粒子の分散状態の
変化が起こる可能性がある事と、カーボン蒸着処理に時
間がかかるという不都合があった。Problems to be Solved by the Invention Paints often contain organic substances in addition to inorganic substances, such as organic pigment dispersants and polymeric resin binders. In the method of applying paint onto a molecular resin sheet carrier and dissolving the polymer resin sheet in an appropriate solvent to obtain a coating film, not only the polymer resin sheet but also the paint components are dissolved in the solvent, resulting in the formation of secondary particles. There was a problem in that the original state of dispersion of particles in the paint could not be observed due to subsequent agglomeration or dispersion. Even with the method of holding particles by carbon vapor deposition, which has improved this problem, there are disadvantages in that the dispersion state of the particles may change due to elution of the binder and that the carbon vapor deposition process takes time.
本発明は以上のような従来方法の欠点を鑑み、粒子の分
散状態をそのまま見るために、バインダー等に変質を起
こさせず、かつカーボン蒸着なしで処理することの出来
る方法を提供せんとするものである。In view of the drawbacks of the conventional methods as described above, the present invention aims to provide a method that allows processing to be performed without causing deterioration of the binder, etc., and without carbon deposition, in order to observe the dispersion state of particles as they are. It is.
問題点を解決するだめの手段
本発明は塗料を高分子樹脂シートに直接塗布せず、例え
ばゼラチンの様な水溶性のシート又は水溶性の薄膜をコ
ートした平滑物質に塗布し、塗布した後に水溶層のシー
トのみを水に溶かし、塗膜をバインダーを残した状態で
透過電子顕微鏡用試料として取り出すようにした試料作
成方法である。Means to Solve the Problem In the present invention, the paint is not applied directly to a polymeric resin sheet, but is applied to a water-soluble sheet such as gelatin or a smooth material coated with a water-soluble thin film, and after application, the paint is applied to a water-soluble sheet. This is a sample preparation method in which only the layer sheet is dissolved in water, and the coating film is taken out as a transmission electron microscopy sample with the binder remaining.
作用
以上のｔｌに成により、塗布担体から塗料を有機溶剤を
用いず分離できる。By forming a tl higher than the action, the paint can be separated from the coating carrier without using an organic solvent.
実施例 以下、本発明の詳細な説明する。Example The present invention will be explained in detail below.
本実施例では水溶性かつ塗料中の有機溶剤に不溶のシー
ト又は水溶性の薄膜をコートした平滑物質に塗料を塗布
した後、このシート又は平滑物質を水で溶解し塗膜を得
る。このように、本実施例ではＬ記構酸により、塗料が
高分子樹脂シート等に直接塗布されず、水溶性薄膜上に
塗布しであるので、塗料を塗布した水溶性薄膜を水溶性
薄膜が水に接する方向で水に浮かべ、水溶性＃１摸が溶
けた後、残って水面に浮かんだ塗料を銅メツシユでサン
プリングし、水分を乾燥除去しておく。この方法は有機
溶剤を用いなくとも、塗布担体から塗料を分離すること
ができるので、簡単であり、しかもカーボン蒸着しなく
とも塗料本来の粒子分散を観察することが可能である。In this embodiment, a paint is applied to a smooth substance coated with a sheet or water-soluble thin film that is water-soluble and insoluble in the organic solvent in the paint, and then the sheet or smooth substance is dissolved in water to obtain a coating film. As described above, in this example, the paint is not applied directly to the polymer resin sheet, etc., but on the water-soluble thin film due to the structural acid L, so the water-soluble thin film coated with the paint is Float it in the water in the direction in which it touches the water, and after the water-soluble #1 sample has dissolved, sample the remaining paint floating on the water surface with a copper mesh, and dry and remove the water. This method is simple because the paint can be separated from the coated carrier without using an organic solvent, and furthermore, it is possible to observe the original particle dispersion of the paint without carbon vapor deposition.
本実施例が特に磁性塗料の分散性評１ｉ１ｒｉに効果を
持つのは、従来の方法がパイングーの損失で粒子の保持
が完全ではないため、磁性粉が、その磁気的性質で凝集
、反発し、本来の粒子状態を観察しにくいのに対し、本
実施例ではバインダーがそのまま存在するので、前述の
不都合が生じないからである。The reason why this example is particularly effective in evaluating the dispersibility of magnetic paint is that the conventional method does not completely retain the particles due to the loss of particles, so the magnetic powder aggregates and repels due to its magnetic properties. This is because, while it is difficult to observe the original particle state, in this example, the binder exists as it is, so the above-mentioned disadvantage does not occur.
従って、本実施例にかかる塗料の分散性評価用試料作成
方法は透過電子顕微鏡で分散性を評価する上で、極めて
利用価値の高い方法である。Therefore, the method for preparing a sample for evaluating the dispersibility of a paint according to this example is an extremely useful method for evaluating the dispersibility using a transmission electron microscope.
尚、水溶性薄膜としてゼラチン膜を用いるのは、ゼラチ
ン膜が、すばやく水に溶ける性質が本発明に適している
ためである。The reason why a gelatin film is used as the water-soluble thin film is that the gelatin film is suitable for the present invention because it quickly dissolves in water.
発明の効果
本発明による塗料の分散性評価用透過電子顕微鏡試料作
成方法は、塗布担体と塗料を分離するに際し、有機溶剤
を用いないため、塗料成分中の有機物を変質させないの
で、バインダーの損失による粒子の移動が起こらず、塗
料本来の粒子状態を観察する事を可能にするという効果
がある。Effects of the Invention The method of preparing a transmission electron microscope sample for evaluating the dispersibility of paint according to the present invention does not use an organic solvent when separating the paint from the coating carrier, so organic substances in the paint components are not altered, so there is no possibility of loss of binder. This has the effect that particle movement does not occur, making it possible to observe the original particle state of the paint.
Claims (4)
水溶性の薄膜をコートした平滑物質に塗料を塗布した後
、このシート又は上記薄膜を水で溶解し塗膜を得ること
を特徴とする透過電子顕微鏡試料作成法。(1) A coating is applied to a smooth substance coated with a sheet or water-soluble thin film that is water-soluble and insoluble in the organic solvent in the paint, and then the sheet or the thin film is dissolved in water to obtain a coating film. Transmission electron microscopy sample preparation method.
特許請求の範囲第１項記載の透過電子顕微鏡試料作成法
。(2) The transmission electron microscope sample preparation method according to claim 1, wherein the water-soluble thin film is a gelatin film.
の範囲第１項記載の透過電子顕微鏡試料作成法。(3) The transmission electron microscope sample preparation method according to claim 1, wherein the paint is a magnetic paint.
塗料であることを特徴とする特許請求の範囲第１項記載
の透過電子顕微鏡試料作成法。(4) The transmission electron microscope sample preparation method according to claim 1, wherein the water-soluble thin film is a gelatin film and the paint is a magnetic paint.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| JP2713786A JPS62185143A (en) | 1986-02-10 | 1986-02-10 | Preparation of sample for transmission electron microscope |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| JP2713786A JPS62185143A (en) | 1986-02-10 | 1986-02-10 | Preparation of sample for transmission electron microscope |
Publications (1)
| Publication Number | Publication Date |
|---|---|
| JPS62185143A true JPS62185143A (en) | 1987-08-13 |
Family
ID=12212661
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| JP2713786A Pending JPS62185143A (en) | 1986-02-10 | 1986-02-10 | Preparation of sample for transmission electron microscope |
Country Status (1)
| Country | Link |
|---|---|
| JP (1) | JPS62185143A (en) |
Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN100360708C (en) * | 2004-05-12 | 2008-01-09 | 中国科学院金属研究所 | Method for preparing film specimen in use for transmission electron microscope |
| CN104596820A (en) * | 2015-01-23 | 2015-05-06 | 中国科学院武汉岩土力学研究所 | Soil particle SEM sample preparation method |
| CN105973660A (en) * | 2016-04-26 | 2016-09-28 | 中国石油化工股份有限公司 | Method for preparing artificial rock core and artificial rock core prepared by method |
| US20220214250A1 (en) * | 2021-01-07 | 2022-07-07 | Jeol Ltd. | Specimen Pretreatment Method |
Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JPS5343590A (en) * | 1976-09-30 | 1978-04-19 | Battelle Institut E V | Method and tool for collecting especially scientific or diagnosis specimens |
| JPS62121332A (en) * | 1985-11-21 | 1987-06-02 | Johoku Ika Kiki Seisakusho:Kk | Preparing method for sample for microscope observation |
-
1986
- 1986-02-10 JP JP2713786A patent/JPS62185143A/en active Pending
Patent Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JPS5343590A (en) * | 1976-09-30 | 1978-04-19 | Battelle Institut E V | Method and tool for collecting especially scientific or diagnosis specimens |
| JPS62121332A (en) * | 1985-11-21 | 1987-06-02 | Johoku Ika Kiki Seisakusho:Kk | Preparing method for sample for microscope observation |
Cited By (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN100360708C (en) * | 2004-05-12 | 2008-01-09 | 中国科学院金属研究所 | Method for preparing film specimen in use for transmission electron microscope |
| CN104596820A (en) * | 2015-01-23 | 2015-05-06 | 中国科学院武汉岩土力学研究所 | Soil particle SEM sample preparation method |
| CN105973660A (en) * | 2016-04-26 | 2016-09-28 | 中国石油化工股份有限公司 | Method for preparing artificial rock core and artificial rock core prepared by method |
| US20220214250A1 (en) * | 2021-01-07 | 2022-07-07 | Jeol Ltd. | Specimen Pretreatment Method |
| JP2022106483A (en) * | 2021-01-07 | 2022-07-20 | 日本電子株式会社 | Pretreatment method for sample |
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