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JP3604553B2 - Electron microscope observation method using astigmatism adjustment sheet - Google Patents
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JP3604553B2 - Electron microscope observation method using astigmatism adjustment sheet - Google Patents

Electron microscope observation method using astigmatism adjustment sheet Download PDF

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Publication number
JP3604553B2
JP3604553B2 JP36600197A JP36600197A JP3604553B2 JP 3604553 B2 JP3604553 B2 JP 3604553B2 JP 36600197 A JP36600197 A JP 36600197A JP 36600197 A JP36600197 A JP 36600197A JP 3604553 B2 JP3604553 B2 JP 3604553B2
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Japan
Prior art keywords
sample
sheet
observation
astigmatism
astigmatism adjustment
Prior art date
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Expired - Fee Related
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JP36600197A
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Japanese (ja)
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JPH11185683A (en
Inventor
克美 中村
仁 青山
秀澄 小渕
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Tomoegawa Co Ltd
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Tomoegawa Paper Co Ltd
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Priority to JP36600197A priority Critical patent/JP3604553B2/en
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Description

【0001】
【発明の属する技術分野】
本発明は、走査型電子顕微鏡(SEM)で観察する際に電子ビームのゆがみ調整(非点調整)をすることが容易な非点調整用シートを用いた観察方法に関する。
【0002】
【従来の技術】
従来、電子顕微鏡の電子ビームのゆがみ調整(非点調整)には試料載置台とは別の円柱状の台の上に酸化亜鉛(ZnO)粒子を付着させた非点調整用の標準試料を用いて、ZnOの粒子像を鮮明に観察できるようにして非点調整をしていた。この非点調整は最良の画像を得るために、頻繁に電子ビーム調整が必要であり、電子ビーム調整の度に観察用試料から非点調整用標準試料への観察点の移動が必要であった。
【0003】
【発明が解決しようとする課題】
上記従来の技術によるときは、顕微鏡の観察視野が広く、観察用試料載置台と酸化亜鉛(ZnO)粒子を付着させた標準試料との間を視野を大きく移動させて観察し、電子ビームを調整をする必要があったので、大変手数がかかって能率が悪いという問題があった。また、標準試料は電子ビームを照射されるために鏡体内でオイルが標準粒子に焼き付いてしまい使用上障害となったり、標準粒子は単に台上に付着させてある程度のため、こすると粒子が脱落してしまうという取扱い上の問題があった。
本発明は上記の如き問題を解決するもので、電子顕微鏡観察における能率の向上及び非点調整用標準試料の取扱性の向上を図るものである。
【0004】
請求項1の発明は、シート状支持体上に顔料と結着剤を含有する顔料層を有する非点調整用シートを走査型電子顕微鏡観察用試料載置台上の試料の近くに貼着しておき、該シートに視野を合わせて非点調整した後、観察用試料に視野を合わせて観察することを特徴とする非点調整用シートを用いた電子顕微鏡観察方法であり、請求項2の発明は、顔料層が、顔料としてZnO粒子を用いた塗布層であることを特徴とする請求項1記載の非点調整用シートを用いた電子顕微鏡観察方法である

【0005】
【作用】
これにより、観察試料台上の観察用試料の近傍に非点調整用シートを貼り付けるので、同一試料載置台上に観察試料と、非点調整用標準試料を配置することとなるため、視野を僅かに移動するだけで電子ビーム調整が可能となり、従来のように観察用試料台と標準試料台の間を大きく移動しなければならなかった視野の移動を最小限に押さえることができる。
また、本発明で用いられる非点調整用シートは、任意の面積に裁断することができ、また、必要に応じてシートの裏面に粘着層を設けることによって、これを試料載置台上の観察用試料を配置した以外の任意の空所に貼り付けることが出来るため、観察用試料の近傍に貼り付けられ、非点調整の際の視野の移動を最小限に押さえることができると共に、随時電子ビーム調整が簡単にできるので、容易で正確な観察が可能である。
【0006】
【発明の実施の形態】
図1は本発明で用いられる非点調整用標準試料のシートの構造を示す1例で、図2はこれを用いた試料載置台の斜視図である。
図1において10はシート状支持体で、ZnO等の顔料を含有した塗料を表面に塗布した顔料層(非点調整可能な層)11を設け、裏面には粘着層12が設けられ、非点調整用シート13を構成している。
図2は観察用試料2と非点調整用シートのシート片3とを同一の試料載置台1の上に設けた斜視図である。
【0007】
本発明におけるシート状支持体としては、紙、不織布、プラスチックフィルム等のシート状のものを適宜使用することができる。また、その厚さも特に限定されるものではないが、支持体としての強度や取扱性等の点から50〜300μm程度のものが好ましい。
顔料層に用いられる顔料としては、粒子径1μm以下のものが好ましく適用することができ、倍率が1万倍以上のときは0.05〜0.7μm程度、特に0.1〜0.5μm程度のものが好ましい。具体的には上記の如き1μm以下に調整された酸化亜鉛、酸化チタン、炭酸カルシウム、水酸化アルミニウム等の無機顔料が挙げられる。また、これら顔料の形状は四角形以上の多角形もしくは不定形のものが好ましく、球形のものは非点調整がしにくいことから余り好ましくない。更に、これらの顔料は導電性を有するもの、もしくは導電処理を施されたものも使用できる。
【0008】
顔料層に顔料と共に使用される樹脂は、結着剤として使用されるもので、常温で固体である結着機能を有する各種の樹脂を適宜使用することができる。具体的にはアクリル系樹脂、ポリエステル樹脂、塩化ビニル系樹脂、酢酸ビニル系樹脂、スチレン系樹脂、ウレタン系樹脂等が挙げられる。
【0009】
顔料層は上記の如き顔料と樹脂を主成分とする塗液をシート状支持体の表面に塗布・乾燥することにより形成される。ここで、顔料と樹脂の配合割合は特に限定されるものではないが、顔料100重量部に対して樹脂5〜20重量部程度が、顔料が脱落することのない取扱性の良い顔料層が形成され、しかも非点調整がやりやすいことから好ましい。また、顔料層の厚さは特に限定されないが、10μm以下、特に3〜8μm程度が好適である。
【0010】
かかる状態のものを用いて走査型電子顕微鏡により試料を観察する場合に、同一試料台内に試料と非点調整標準試料とを近接して配置できるため、僅かの視野移動で電子ビームの調整が可能となり、視野の移動を最小限にすることができる。
また、本発明で用いられるシート状非点調整標準試料は任意の大きさに裁断することができること、更に、必要に応じて裏面に粘着層を設けたことにより、試料載置台の任意の個所に貼りつけすることができるので、取扱が簡単で非点調整を容易に行なうことができる。
【0011】
上記のように本発明の観察方法で使用する非点調整用シートは、シート状であるために任意の形状の小片に切り取り易く、試料台の隅でも容易に貼り付けることができるので、▲1▼常に新しい酸化亜鉛粒子像を観察することができる。▲2▼試料と一緒に貼りこめるので、視野を余り動かさなくても良く、観察が便利で正確である、等の利点がある。
【0012】
【実施例】
実施例の配合及び製法は下記のとおりである。
ZnO 100重量部、アクリル系樹脂 5〜20重量部、トルエン50重量部を混合して、ホモジナイザーで攪拌(攪拌速度10,000〜15,000rpm)し、粘度200〜500cpの顔料層用塗料を得た。
次に上記の塗料をポリエステルフィルムの表面にドクター塗工して厚さ5μmの顔料層を設けて、本発明で用いる非点調整用シートを得た。上記で作成したシートの一部を切り取って、図2のように試料載置台上の観察用試料の近傍に貼着し、金蒸着を施して電子顕微鏡観察に用いたところ、非点調整と試料の観察が非常に能率良く実施できた。
【0013】
【発明の効果】
本発明によれば、電子顕微鏡観察における非点調整の際にシート状の非点調整用シートを使用するので、任意の場所で任意の形状サイズに切り取って使用でき、また、これを観察する試料の載置台の試料に隣接した余白部分に貼り付けるだけであり、何等困難性がなく視野を僅かに移動するだけで能率良く観察することができる。
【図面の簡単な説明】
【図1】本発明で使用される非点調整用シートの構造を示す断面図。
【図2】本発明の実施状態の試料台の斜視図。
【符号の説明】
1 試料載置台。
2 観察用試料。
3 非点調整用シート片。
10 シート状支持体。
11 顔料層。
12 粘着層。
13 非点調整用シート。
[0001]
TECHNICAL FIELD OF THE INVENTION
The present invention relates to the observation method is used easy astigmatism adjustment sheet for a distortion adjustment of the electron beam (astigmatism correction) when observed with a scanning electron microscope (SEM).
[0002]
[Prior art]
Conventionally, a standard sample for astigmatism adjustment in which zinc oxide (ZnO) particles are adhered to a column-shaped table different from the sample mounting table is used for electron beam distortion adjustment (astigmatism adjustment) of an electron microscope. Thus, the astigmatism adjustment is performed so that the ZnO particle image can be clearly observed. This astigmatism adjustment required frequent electron beam adjustments to obtain the best image, and it was necessary to move the observation point from the observation sample to the astigmatism adjustment standard sample each time the electron beam adjustment was performed. .
[0003]
[Problems to be solved by the invention]
According to the above conventional technique, the observation field of view of the microscope is wide, and the observation field is largely moved between the observation sample mounting table and the standard sample to which zinc oxide (ZnO) particles are adhered to observe and adjust the electron beam. The problem was that it was very time-consuming and inefficient. In addition, since the standard sample is irradiated with the electron beam, oil is burned into the standard particles in the mirror body and hinders the use of the standard sample. There was a problem in handling that it would.
SUMMARY OF THE INVENTION The present invention solves the above-mentioned problems, and aims to improve the efficiency in observation with an electron microscope and improve the handleability of a standard sample for astigmatism adjustment.
[0004]
According to the first aspect of the present invention, an astigmatism adjustment sheet having a pigment layer containing a pigment and a binder on a sheet-like support is attached near a sample on a sample mounting table for scanning electron microscope observation. 3. An electron microscope observation method using an astigmatism adjustment sheet, wherein the observation is performed by adjusting the visual field to the observation sample after adjusting the visual field to the sheet. the pigment layer, an electron microscope observation method using the astigmatism adjustment sheet according to claim 1, characterized in that the coating layer using the ZnO particles as a pigment.
[0005]
[Action]
As a result, the astigmatism adjustment sheet is adhered to the vicinity of the observation sample on the observation sample stage, so that the observation sample and the standard sample for astigmatism adjustment are arranged on the same sample mounting table. The electron beam can be adjusted with only a slight movement, and the movement of the visual field, which had to be largely moved between the observation sample table and the standard sample table as in the related art, can be minimized.
Further, the astigmatism adjustment sheet used in the present invention can be cut into an arbitrary area, and if necessary, by providing an adhesive layer on the back surface of the sheet, this can be cut for observation on a sample mounting table. Since it can be attached to any space other than where the sample is placed, it can be attached to the vicinity of the observation sample, minimizing the movement of the field of view during astigmatism adjustment, and the electron beam Since the adjustment can be made easily, easy and accurate observation is possible.
[0006]
BEST MODE FOR CARRYING OUT THE INVENTION
FIG. 1 is an example showing a structure of a sheet of a standard sample for astigmatism adjustment used in the present invention, and FIG. 2 is a perspective view of a sample mounting table using the same.
In FIG. 1, reference numeral 10 denotes a sheet-like support, which is provided with a pigment layer (a layer capable of adjusting the astigmatism) 11 in which a paint containing a pigment such as ZnO is applied to the surface, and an adhesive layer 12 is provided on the back surface. The adjustment sheet 13 is configured.
FIG. 2 is a perspective view in which the observation sample 2 and the sheet piece 3 of the astigmatism adjustment sheet are provided on the same sample mounting table 1.
[0007]
As the sheet-like support in the present invention, a sheet-like support such as paper, nonwoven fabric, and plastic film can be appropriately used. The thickness of the support is not particularly limited, but is preferably about 50 to 300 μm from the viewpoint of strength as a support, handling properties, and the like.
As the pigment used in the pigment layer, those having a particle diameter of 1 μm or less can be preferably applied, and when the magnification is 10,000 times or more, about 0.05 to 0.7 μm, particularly about 0.1 to 0.5 μm. Are preferred. Specific examples include inorganic pigments such as zinc oxide, titanium oxide, calcium carbonate, and aluminum hydroxide adjusted to 1 μm or less as described above. Further, the shape of these pigments is preferably a polygon having more than a quadrangle or an irregular shape, and a spherical shape is not preferred because it is difficult to adjust the astigmatism. Further, these pigments having conductivity or having undergone a conductive treatment may be used.
[0008]
The resin used together with the pigment in the pigment layer is used as a binder, and various resins having a binding function that is solid at ordinary temperature can be used as appropriate. Specific examples include acrylic resins, polyester resins, vinyl chloride resins, vinyl acetate resins, styrene resins, urethane resins, and the like.
[0009]
The pigment layer is formed by applying a coating liquid containing the above-described pigment and resin as main components on the surface of the sheet-like support and drying it. Here, the mixing ratio of the pigment and the resin is not particularly limited, but about 5 to 20 parts by weight of the resin with respect to 100 parts by weight of the pigment forms a pigment layer with good handleability without the pigment falling off. It is preferable because the astigmatism adjustment is easily performed. The thickness of the pigment layer is not particularly limited, but is preferably 10 μm or less, particularly preferably about 3 to 8 μm.
[0010]
When observing a sample with a scanning electron microscope using such an object, the sample and the astigmatism-adjusted standard sample can be arranged close to each other in the same sample stage, so that the electron beam can be adjusted with a slight visual field movement. This makes it possible to minimize the movement of the visual field.
In addition, the sheet-shaped astigmatism-adjusted standard sample used in the present invention can be cut into an arbitrary size, and further, by providing an adhesive layer on the back surface as necessary, at an arbitrary position on the sample mounting table. Since it can be pasted, it is easy to handle and the astigmatism adjustment can be easily performed.
[0011]
As described above, since the astigmatism adjustment sheet used in the observation method of the present invention is in a sheet shape, it can be easily cut into small pieces of an arbitrary shape, and can be easily attached even at the corner of the sample table. ▼ New zinc oxide particle images can always be observed. {Circle around (2)} Since the sample can be pasted together with the sample, there is an advantage that the field of view does not need to be moved so much that observation is convenient and accurate.
[0012]
【Example】
The formulations and production methods of the examples are as follows.
100 parts by weight of ZnO, 5 to 20 parts by weight of an acrylic resin, and 50 parts by weight of toluene are mixed and stirred with a homogenizer (stirring speed: 10,000 to 15,000 rpm) to obtain a pigment layer paint having a viscosity of 200 to 500 cp. Was.
Next, the above coating material was doctor-coated on the surface of the polyester film to provide a pigment layer having a thickness of 5 μm, thereby obtaining a sheet for adjusting astigmatism used in the present invention. A part of the sheet prepared above was cut out, attached to the vicinity of the sample for observation on the sample mounting table as shown in FIG. 2, and subjected to gold vapor deposition and used for electron microscope observation. Was very efficiently performed.
[0013]
【The invention's effect】
According to the present invention, since a sheet-like astigmatism adjustment sheet is used at the time of astigmatism adjustment in electron microscopic observation, it can be used by cutting it to an arbitrary shape and size at an arbitrary place, and a sample for observing this. Is simply attached to a blank portion adjacent to the sample on the mounting table, and it is possible to observe efficiently with only a slight movement of the field of view without any difficulty.
[Brief description of the drawings]
FIG. 1 is a cross-sectional view showing the structure of an astigmatism adjustment sheet used in the present invention.
FIG. 2 is a perspective view of a sample stage in an embodiment of the present invention.
[Explanation of symbols]
1 Sample mounting table.
2 Observation sample.
3 Sheets for astigmatism adjustment.
10 Sheet support.
11 Pigment layer.
12 Adhesive layer.
13 Astigmatism adjustment sheet.

Claims (2)

シート状支持体上に顔料と結着剤を含有する顔料層を有する非点調整用シートを走査型電子顕微鏡観察用試料載置台上の試料の近くに貼着しておき、該シートに視野を合わせて非点調整した後、観察用試料に視野を合わせて観察することを特徴とする非点調整用シートを用いた電子顕微鏡観察方法。 A sheet for astigmatism adjustment having a pigment layer containing a pigment and a binder on a sheet-like support is pasted near a sample on a sample mounting table for observation with a scanning electron microscope, and a field of view is formed on the sheet. An electron microscope observation method using an astigmatism adjustment sheet, wherein the observation is performed by adjusting the field of view to the observation sample after the adjustment. 顔料層が、顔料としてZnO粒子を用いた塗布層であることを特徴とする請求項1記載の非点調整用シートを用いた電子顕微鏡観察方法The electron microscope observation method using the astigmatism adjustment sheet according to claim 1, wherein the pigment layer is a coating layer using ZnO particles as a pigment.
JP36600197A 1997-12-24 1997-12-24 Electron microscope observation method using astigmatism adjustment sheet Expired - Fee Related JP3604553B2 (en)

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Application Number Priority Date Filing Date Title
JP36600197A JP3604553B2 (en) 1997-12-24 1997-12-24 Electron microscope observation method using astigmatism adjustment sheet

Publications (2)

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JP3604553B2 true JP3604553B2 (en) 2004-12-22

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JP4995478B2 (en) * 2006-04-18 2012-08-08 株式会社日立ハイテクノロジーズ Nanoimprint spacer, method for producing electron microscope adjustment sample using the same, electron microscope adjustment sample, and electron microscope equipped with the same
JP4810399B2 (en) * 2006-11-06 2011-11-09 株式会社日立ハイテクノロジーズ Sample table for electron beam equipment

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