JPS586268B2 - Capsule device for electron microscope - Google Patents
Capsule device for electron microscopeInfo
- Publication number
- JPS586268B2 JPS586268B2 JP51131261A JP13126176A JPS586268B2 JP S586268 B2 JPS586268 B2 JP S586268B2 JP 51131261 A JP51131261 A JP 51131261A JP 13126176 A JP13126176 A JP 13126176A JP S586268 B2 JPS586268 B2 JP S586268B2
- Authority
- JP
- Japan
- Prior art keywords
- sample
- gas
- electron microscope
- capsule device
- objective lens
- 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.)
- Expired
Links
Description
【発明の詳細な説明】
本発明は電子顕微鏡のカプセル装置（雰囲気ガス試料室
）に関するものである。DETAILED DESCRIPTION OF THE INVENTION The present invention relates to a capsule device (atmospheric gas sample chamber) for an electron microscope.
一般に電子顕微鏡で観察する試料は真空中に置かれてい
る。Generally, samples observed with an electron microscope are placed in a vacuum.
ところが近年、試料を高温、低温、または雰囲気ガス中
等、特別な環境におき観察する技術が発達して来た。However, in recent years, techniques have been developed for observing samples in special environments such as high temperatures, low temperatures, or atmospheric gases.
そのため雰囲気ガス試料室（通常カプセルと呼ばれてい
る）としては、薄膜の窓を設けた方式のものと、ピンホ
ールを有する隔壁を多段的に用いる差動排気方式の二種
が開発されている。Therefore, two types of atmospheric gas sample chambers (usually called capsules) have been developed: one with a thin film window, and the other with a differential pumping system using multiple partition walls with pinholes. .
ところがこれらのカプセルは次に述べるような問題点を
もっている。However, these capsules have the following problems.
電子顕微鏡の試料は一般に対物レンズのボールピースの
ギャップ内に置かれており、このギヤップ内に入るカプ
セルの大きさは約１ｃｍ位である。A sample for an electron microscope is generally placed in a gap between a ball piece of an objective lens, and the size of the capsule that fits into this gap is about 1 cm.
このような小さなカプセルの中で加熱、引張り、および
ガス導入を行なうためには、特別設計された微小な部品
で構成される機構が必要であり、また、試料をこれにセ
ットする技術も容易なことではない。In order to perform heating, tension, and gas introduction inside such a small capsule, a mechanism consisting of specially designed minute parts is required, and the technology for setting the sample in this mechanism is also simple. That's not the point.
本発明は、このような従来技術の問題点を解決したもの
であって、前記の差動排気系の隔壁の位置と孔径を適当
に設定することによって、従来の試料ホルダーをそのま
ま利用して試料の雰囲気を変えることができることを特
徴としたカプセル装置である。The present invention solves the problems of the prior art, and by appropriately setting the position and hole diameter of the partition wall of the differential pumping system, the sample can be mounted using the conventional sample holder as is. This capsule device is characterized by its ability to change the atmosphere.
その結果は、特別設計された精密構造のカプセルを必要
とせず、しかもトップエントリ一方式の従来技術に簡単
な操作を加えるだけで高温、ガス反応実験が可能である
。As a result, high-temperature gas reaction experiments can be performed without the need for a specially designed capsule with a precision structure, and by simply adding simple operations to the conventional top-entry technology.
すなわち本発明は集束レンズの上、下および対物レンズ
の下部に固定隔壁を設け、該隔壁に例えば０．５ｍｍφ
程度の細孔を穿ちさらに通常の試料ホルダーをセットし
た後にこの試料ホルダーを、例えば頂部に３ｍｍφ程度
の細孔を穿ったカップ型の隔壁で覆うことを特徴とした
カプセル装置である。That is, in the present invention, fixed partition walls are provided above and below the focusing lens and below the objective lens, and the partition walls have a diameter of, for example, 0.5 mm.
This capsule device is characterized in that, after a normal sample holder is set in which a pore of about 3 mm in diameter is bored, the sample holder is covered with a cup-shaped partition wall having a pore of about 3 mm in diameter at the top, for example.
以下図面により本発明の要旨を説明する。The gist of the present invention will be explained below with reference to the drawings.
第１図は本発明装置の縦断側面略図で、１は加速管、２
は鏡体、３は通常のトップエントリー型試料台１９にセ
ットされた試料、４は対物レンズポールピースでその中
央ギャップ内に試料３が収容されている。FIG. 1 is a schematic longitudinal cross-sectional view of the device of the present invention, in which 1 is an acceleration tube, 2
3 is a mirror body, 3 is a sample set on a normal top entry type sample stage 19, and 4 is an objective lens pole piece, in which the sample 3 is accommodated in the center gap.
このギャップの下面には有孔隔壁７（孔径０．５ｍｍφ
）が固定されており、試料３を保持する試料台１９はカ
ップ型隔壁８で覆われている。The lower surface of this gap has a perforated partition wall 7 (hole diameter 0.5 mmφ).
) is fixed, and a sample stage 19 holding the sample 3 is covered with a cup-shaped partition wall 8.
この外に集束レンズ１５の上下にも有孔隔壁５，６が取
付けられている。In addition to this, perforated partition walls 5 and 6 are attached above and below the focusing lens 15.
加速管１にはイオンポンプがあり、その直下に油拡散ポ
ンプ９、主排気系のポンプ１０および対物レンズギャッ
プの側面のポンプ１１からなる差動排気系が構成されて
おり、それぞれに真空計１２．１３．１４が設けられて
いる。There is an ion pump in the acceleration tube 1, and a differential pumping system consisting of an oil diffusion pump 9, a main pumping system pump 10, and a pump 11 on the side of the objective lens gap is configured directly below the ion pump, and a vacuum gauge 12 is attached to each pump. .13.14 are provided.
さらに対物レンズポールピース４の側面にはガス導入口
１８が設けられておりガス導入用微調整バルブが取付け
られている。Furthermore, a gas introduction port 18 is provided on the side surface of the objective lens pole piece 4, and a gas introduction fine adjustment valve is attached thereto.
試料３を観察するには、トップエントリ一方式の通常観
察法により、試料を収容し、次いでカップ型隔壁８でこ
れを覆う。In order to observe the sample 3, the sample is accommodated using a top-entry one-way normal observation method, and then covered with a cup-shaped partition wall 8.
加熱時の熱電対等のリード線はこのカップ型隔壁８に設
けられた細孔を通してセットされる。Lead wires for thermocouples and the like during heating are set through the pores provided in the cup-shaped partition wall 8.
各ポンプを作動させると、各部の真空度は１０ ”Ｔ
ｏｒｒに達する。When each pump is operated, the degree of vacuum in each part is 10”T.
Reach orr.
鏡体内をアルゴン洗浄して不良残留ガス量を減じたのち
、ガス導入口１８より目的の反応ガスを導入する。After cleaning the inside of the mirror body with argon to reduce the amount of defective residual gas, the target reaction gas is introduced through the gas inlet 18.
このとき試料３の近傍をＩ×ＩＯ ’Ｔｏｒｒにする
と鏡体２の真空度は５×１０ ’Ｔｏｒｒとなるが、
電子鏡部はＩ×ＩＯ−６Ｔｏｒｒ、加速管部１は１×１
０−７Ｔｏｒｒであり、真空度の低下は起らない。At this time, if the vicinity of the sample 3 is set to I×IO' Torr, the degree of vacuum of the mirror body 2 becomes 5×10' Torr.
The electronic mirror section is I x IO-6 Torr, and the acceleration tube section 1 is 1 x 1
The pressure is 0-7 Torr, and the degree of vacuum does not decrease.
金属薄膜試料の高温ガス反応実験におけるガス圧はＩ
× １０ ” Ｔｏｒｒもあれば充分であり、これ以
上多量のガスを導入すると反応が早く観測が出来ないば
かりか、不純ガスによる悪影響のみが観測される結果に
なる。The gas pressure in the high temperature gas reaction experiment of the metal thin film sample is I
× 10” Torr is sufficient, and if a larger amount of gas is introduced, the reaction will be too fast and observation will not be possible, and only the adverse effects of the impure gas will be observed.
Ｉ×ＩＯ ’Ｔｏｒｒ ，８００〜９００℃の実験で
はガスの拡散速度にもよるが一般的には士数分で反応が
終るようである。In experiments at I×IO' Torr of 800 to 900° C., the reaction generally seems to end in a few minutes, although it depends on the gas diffusion rate.
一例を次に示す。An example is shown below.
Ｉ×ＩＯ ”Ｔｏｒｒ，の窒素ガス中にＦｅ−０．３
％Ａ／合金の薄膜を入れ、８００℃，１０分の処理で窒
化アルミニウムが析出することを確認した。Fe-0.3 in nitrogen gas at I×IO” Torr.
It was confirmed that aluminum nitride was precipitated by adding a thin film of %A/alloy and treating at 800° C. for 10 minutes.
さらに長時間観測を続けると内部構造的には大きな変化
は見られなかったが、残留酸素のために表面銹がはげし
くなる傾向を示した。When the observation was continued for an even longer period of time, no major changes were observed in the internal structure, but the surface rust tended to become more severe due to residual oxygen.
以上説明したように本発明装置は真空内で低圧のガス反
応を行う電子顕微鏡において、差動排気用の有効隔壁の
１つをカップ型のものを用いることにより通常状態のト
ップエントリ一方式の試料ホルダーによってガス反応実
験ができその効果は極めて大きい。As explained above, the apparatus of the present invention can be used for electron microscopes that perform low-pressure gas reactions in vacuum. The holder allows gas reaction experiments to be carried out, which is extremely effective.
第１図は本発明の要部を示す側面略図である。
１・・・・・・加速管、２・・・・・・鏡体、３・・・
・・・試料、４・・・・・・対物レンズポールピース、
５，６．７・・・・・・有孔隔壁、８・・・・・・カッ
プ型有孔隔壁、９・・・・・・電子鏡直下に設けた真空
ポンプ、１０・・・・・・主排気系に設けた真空ポンプ
、１１・・・・・・対物レンズギャップに設けた真空ポ
ンプ、１２・・・・・・電子鏡に設けた真空計、１３・
・・・・・主排気系に設けた真空計、１４・・・・・・
対物レンズギャップに設けた真空計、１５・・・・・・
集束レンズ、１６・・・・・・対物レンズ、１７・・・
・・・中間レンズ、１８・・・・・・ガス導入口、１９
・・・・・・試料台。FIG. 1 is a schematic side view showing the main parts of the present invention. 1...Acceleration tube, 2...Mirror body, 3...
...Sample, 4...Objective lens pole piece,
5, 6.7... Perforated partition wall, 8... Cup-shaped perforated partition wall, 9... Vacuum pump installed directly below the electronic mirror, 10...・Vacuum pump provided in the main exhaust system, 11... Vacuum pump provided in the objective lens gap, 12... Vacuum gauge provided in the electronic mirror, 13.
...Vacuum gauge installed in the main exhaust system, 14...
Vacuum gauge installed in the objective lens gap, 15...
Focusing lens, 16...Objective lens, 17...
...Intermediate lens, 18...Gas inlet, 19
...Sample stand.
Claims (1)
壁を設け、該隔壁に細孔を設けるとともに、通常の試料
ホルダーを試料室にセットした後、該試料ホルダーを細
孔を穿ったカップ型の隔壁で被覆することを特徴とする
電子顕微鏡用カプセル装置。1. Fixed partitions are provided above and below the focusing lens and at the bottom of the objective lens, and pores are provided in the partitions. After setting a normal sample holder in the sample chamber, the sample holder is attached to a cup-shaped partition with pores. A capsule device for an electron microscope characterized by being coated with.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| JP51131261A JPS586268B2 (en) | 1976-11-02 | 1976-11-02 | Capsule device for electron microscope |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| JP51131261A JPS586268B2 (en) | 1976-11-02 | 1976-11-02 | Capsule device for electron microscope |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| JPS5356962A JPS5356962A (en) | 1978-05-23 |
| JPS586268B2 true JPS586268B2 (en) | 1983-02-03 |
Family
ID=15053778
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| JP51131261A Expired JPS586268B2 (en) | 1976-11-02 | 1976-11-02 | Capsule device for electron microscope |
Country Status (1)
| Country | Link |
|---|---|
| JP (1) | JPS586268B2 (en) |
Families Citing this family (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JPH0719556B2 (en) * | 1983-02-07 | 1995-03-06 | 株式会社トプコン | Scanning electron microscope |
| JP2009152087A (en) * | 2007-12-21 | 2009-07-09 | Jeol Ltd | Transmission electron microscope |
-
1976
- 1976-11-02 JP JP51131261A patent/JPS586268B2/en not_active Expired
Also Published As
| Publication number | Publication date |
|---|---|
| JPS5356962A (en) | 1978-05-23 |
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