JPH0792062A - In-situ preparation and observation method of thin film sample for transmission electron microscope and its apparatus - Google Patents
In-situ preparation and observation method of thin film sample for transmission electron microscope and its apparatusInfo
- Publication number
- JPH0792062A JPH0792062A JP5067341A JP6734193A JPH0792062A JP H0792062 A JPH0792062 A JP H0792062A JP 5067341 A JP5067341 A JP 5067341A JP 6734193 A JP6734193 A JP 6734193A JP H0792062 A JPH0792062 A JP H0792062A
- Authority
- JP
- Japan
- Prior art keywords
- electron microscope
- sample
- transmission electron
- thin film
- polishing
- 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.)
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Abstract
(57)【要約】
【目的】 透過型電子顕微鏡用の薄膜試料の特定局所領
域の薄膜化を該顕微鏡内で試料を観察しながらその場で
高精度に作製する。難加工材料の透過型電子顕微鏡試料
の作製を容易にして透過型電子顕微鏡の観察を効率化す
る。
【構成】 集束イオンビーム照射装置を透過型電子顕微
鏡の試料室の前方斜め上方から取付け、サブミクロンオ
ーダー領域の精密な研磨が可能になるようにビーム径は
約０．１５μｍまで絞る手段を設ける。電子顕微鏡で観
察しながら研磨できるように電子線とＦＩＢを試料上の
同一場所に来るように調整する手段を設ける。透過型電
子顕微鏡の走査系および２次電子検出器を集束イオンビ
ーム照射装置の試料の微細研磨加工手段に兼用する。
(57) [Abstract] [Purpose] A thin film sample for a transmission electron microscope is formed in a thin film in a specific local region with high precision on the spot while observing the sample in the microscope. It facilitates the preparation of a transmission electron microscope sample of a difficult-to-process material and makes the observation of the transmission electron microscope efficient. [Structure] A focused ion beam irradiation device is attached obliquely from above and forward of a sample chamber of a transmission electron microscope, and means for narrowing the beam diameter to about 0.15 μm is provided so as to enable precise polishing in a submicron order region. A means is provided for adjusting the electron beam and the FIB so as to come to the same place on the sample so that polishing can be performed while observing with an electron microscope. The scanning system of the transmission electron microscope and the secondary electron detector are also used as the means for finely polishing the sample of the focused ion beam irradiation apparatus.
Description
【産業上の利用分野】この発明は、透過型電子顕微鏡用
の薄膜試料の作製および観察方法並びにその装置に関す
るものである。さらに詳しくは、この発明は、これまで
経験に頼って行っていた試料の特定局所領域の薄膜化
を、該顕微鏡内で試料を観察しながらその場で高精度に
実施可能にしたもので、難加工材料の透過型電子顕微鏡
試料の作製を容易とすることのできる新しい方法とその
ための装置に関するものである。BACKGROUND OF THE INVENTION 1. Field of the Invention The present invention relates to a method for preparing and observing a thin film sample for a transmission electron microscope and an apparatus therefor. More specifically, the present invention makes it possible to perform thinning of a specific local region of a sample, which had been performed so far by experience, with high precision on the spot while observing the sample in the microscope, The present invention relates to a new method capable of facilitating the preparation of a transmission electron microscope sample of a processed material and an apparatus therefor.
【従来の技術とその装置】透過型電子顕微鏡用の薄膜試
料はこれまで電解研磨やイオン研磨などによって作製さ
れてきたが、これらの方法では試料研磨中は試料の観察
が出来ず、従って、試料の出来具合は経験に頼らざるを
得ず、また、研磨が終了して作製された薄膜試料を観察
のため電子顕微鏡内に挿入載置するまでに、該薄膜試料
は溶液や大気に必ず触れるため、表面の清浄な薄膜試料
を電子顕微鏡内に挿入設置することは大変困難であっ
た。一方、集束イオンビーム（Focused Ion Beam：ＦＩ
Ｂ）は、マスクレス注入やリソグラフィへの応用が図ら
れている。そしてこのＦＩＢの応用に際しては、ビーム
スポット内での研磨速度の差やスパッタ粒子の再デポジ
ッションにより、研磨周辺領域には複雑なミクロ組織変
化が起こるため、これらのミクロ組織変化を観察するこ
とが望まれていた。しかしながら、上記の通り、試料を
観察のために電子顕微鏡内に挿入設置する場合、薄膜試
料の表面は汚れるために観察は実際上困難であった。こ
の発明は、以上の通りの従来技術の問題点を一気に解決
するためになされたものであり、作製された薄膜試料が
溶液や大気に触れて汚染される心配をなくし、透過型電
子顕微鏡観察においてサブミクロンオーダーの高精度の
薄膜試料を効率よくＦＩＢで研磨して作製すると共にこ
れを観察することのできる、新しい方法とその装置を提
供することを目的としている。2. Description of the Related Art Thin film samples for transmission electron microscopes have been prepared by electrolytic polishing or ion polishing until now. However, these methods cannot observe the samples during polishing and therefore However, the thin film sample must be in contact with the solution or the atmosphere until it is inserted into the electron microscope for observation and the thin film sample prepared after polishing has been completed. It was very difficult to insert a thin film sample with a clean surface into an electron microscope. On the other hand, Focused Ion Beam (FI)
In B), application to maskless implantation and lithography is aimed at. When applying this FIB, a complicated microstructure change occurs in the polishing peripheral region due to the difference in the polishing rate within the beam spot and the redeposition of sputtered particles. Therefore, it is possible to observe these microstructure changes. Was wanted. However, as described above, when the sample is inserted and installed in the electron microscope for observation, the surface of the thin film sample is contaminated, and therefore observation is practically difficult. This invention has been made in order to solve the problems of the prior art as described above at a stroke, eliminates the risk of the produced thin film sample being touched by a solution or the atmosphere and being contaminated, and in observing with a transmission electron microscope. It is an object of the present invention to provide a new method and apparatus capable of efficiently producing a submicron-order high-precision thin film sample by polishing with FIB and observing the sample.
【課題を解決するための手段】上記の課題を解決するた
めに、この発明は、作製すべき試料を透過型電子顕微鏡
内に観察状態に挿入設置し、電子線を走査して試料を観
察しながら試料の観察領域に集束イオンビームを照射し
て該集束イオンビームで該試料面を研磨すると共にこれ
を観察する方法を提供する。また、この発明は、透過型
電子顕微鏡用の試料に電子顕微鏡内で研磨加工すること
ができるように集束イオンビーム照射装置を透過型電子
顕微鏡に設け、サブミクロンオーダー領域の精密な研磨
が可能になるようにビーム径は約０．１５μｍまで絞る
手段を設け、実際に電子顕微鏡で観察しながら研磨でき
るように電子線とＦＩＢを試料上の同一場所に来るよう
に調整する手段を設けた装置をも提供する。さらにま
た、集束イオンビーム照射装置を透過型電子顕微鏡の試
料室の前方斜め上方から透過型電子顕微鏡に取付け、透
過型電子顕微鏡の走査系および２次電子検出器を集束イ
オンビーム照射装置の試料の微細研磨加工手段に兼用す
ることとした装置をその一つの態様としてもいる。SUMMARY OF THE INVENTION In order to solve the above problems, the present invention inserts a sample to be prepared into a transmission electron microscope in an observing state, installs it, and scans an electron beam to observe the sample. While providing a method of irradiating the observation region of the sample with a focused ion beam, polishing the sample surface with the focused ion beam, and observing the surface. Further, according to the present invention, a focused ion beam irradiation device is provided in a transmission electron microscope so that a sample for a transmission electron microscope can be polished in the electron microscope, which enables precise polishing in a submicron order region. As shown in the figure, the beam diameter is reduced to about 0.15 μm, and the apparatus is equipped with a means for adjusting the electron beam and FIB to come to the same place on the sample so that polishing can be performed while actually observing with an electron microscope. Also provide. Furthermore, the focused ion beam irradiation apparatus is attached to the transmission electron microscope from diagonally above and in front of the sample chamber of the transmission electron microscope, and the scanning system of the transmission electron microscope and the secondary electron detector are attached to the sample of the focused ion beam irradiation apparatus. An apparatus which is also used as a fine polishing processing means is also one of its modes.
【作用】すなわち、この発明は透過型電子顕微鏡の中で
電子顕微鏡用試料を観察しながら研磨するという、斬新
な発想に基いて行われたものであり、これまで類をみな
いほどの微小領域を研磨することを可能とし、高精度の
薄膜試料の作製および観察並びに、透過型顕微鏡内に載
置された薄膜試料を汚染されることなく清浄に保つこと
を可能としている。In other words, the present invention was carried out based on the novel idea of polishing while observing a sample for an electron microscope in a transmission electron microscope. It makes it possible to polish and observe a thin film sample with high accuracy, and to keep the thin film sample placed in the transmission microscope clean without being contaminated.
【実施例】図１は、この発明の装置の一例を示したもの
である。この図１において、２００ｋＶの走査透過型電
子顕微鏡（ＪＥＭ−２００ＣＸ）の試料室の前面斜め上
方に２５ｋＶのＦＩＢカラム（１）を取付け、走査透過
型電子顕微鏡の対物ポールピース（２）の斜め上方から
試料位置にたとえばＧａビームを導入できる構造とす
る。走査透過型電子顕微鏡の分解能を低下させないよう
に配慮して、ＦＩＢカラム（１）の取付け角度は水平面
から５５度斜め上方とした。この結果、ＦＩＢの作動距
離は９７．５mmとなった。ＦＩＢによる描画は走査透過
型電子顕微鏡の走査系・二次電子検出器を兼用する構成
とする。ついで、上記図１の構成とした走査透過型顕微
鏡の試料室にイオン研磨して予め作製したＳｉの単結晶
薄膜を設置し、Ｓｉの単結晶薄膜に電子線を照射してリ
アルタイムで観察しながら観察下にあるＳｉの単結晶薄
膜に前方斜め上方のＦＩＢカラム（１）から２５ｋｅＶ
のＧａ−ＦＩＢを照射し、該ＦＩＢのビーム径（最小
０．１５μｍ ）を調節することで研磨領域を自由に設
定し、スキャン速度を調節することで研磨速度を自由に
調節して、試料面を高精度に微細に研磨して観察可能な
領域を増やすことに成功した。この場合、ＦＩＢの作動
距離からビーム径は約０．１５μｍであり、２５ｋｅＶ
での動作では、対物ポールピース（２）中で磁場の影響
はほとんど無かった。図２は、実際にＳｉ（１００）を
Ｇａ−ＦＩＢで研磨した透過型電子顕微鏡用の薄膜試料
の全体の電子顕微鏡像を示したものである。図２（ａ）
はａｒｅａ・ｓｃａｎをして観察に適した薄い領域を作
りだしたところであり、図２（ｂ）はｌｉｎｅ・ｓｃａ
ｎをして観察領域のごく一部（幅０．１５μｍ程度）だ
けを研磨したものである。DESCRIPTION OF THE PREFERRED EMBODIMENTS FIG. 1 shows an example of the device of the present invention. In FIG. 1, a 25 kV FIB column (1) is attached diagonally above the front of the sample chamber of a 200 kV scanning transmission electron microscope (JEM-200CX), and diagonally above the objective pole piece (2) of the scanning transmission electron microscope. Therefore, the structure is such that a Ga beam can be introduced into the sample position. The mounting angle of the FIB column (1) was set at an angle of 55 degrees above the horizontal plane so as not to reduce the resolution of the scanning transmission electron microscope. As a result, the working distance of the FIB was 97.5 mm. The drawing by the FIB is configured so that the scanning system and the secondary electron detector of the scanning transmission electron microscope are also used. Next, a Si single crystal thin film prepared by ion polishing in advance is placed in the sample chamber of the scanning transmission microscope configured as shown in FIG. 1, and the Si single crystal thin film is irradiated with an electron beam and observed in real time. 25 keV from the FIB column (1) diagonally forward and upward to the Si single crystal thin film under observation
Of Ga-FIB and the beam diameter (0.15 μm minimum) of the FIB is adjusted to freely set the polishing region, and the scanning speed is adjusted to freely adjust the polishing rate to obtain the sample surface. We succeeded in increasing the observable area by finely polishing the surface with high precision. In this case, the beam diameter is about 0.15 μm from the working distance of the FIB, and 25 keV
In the operation at 1, there was almost no influence of the magnetic field in the objective pole piece (2). FIG. 2 shows an electron microscope image of an entire thin film sample for a transmission electron microscope in which Si (100) was actually polished by Ga-FIB. Figure 2 (a)
Is a area where a thin area suitable for observation has been created by performing area scan, and FIG. 2B shows line scan
n is used to polish only a small part of the observation region (width of about 0.15 μm).
【発明の効果】これまでの電子顕微鏡用試料製作方法で
は、試料を電子顕微鏡の中に挿入するまでに必ず大気中
あるいは溶液中にさらす瞬間があるため、清浄な表面を
得ることはほぼ不可能であった。しかしながら、この発
明は走査透過型電子顕微鏡に試料を挿入してから研磨を
行うので表面が汚染されていた試料でも観察する直前に
削り取ってしまうことができる。また、研磨の精度とし
て、従来では作製された薄膜試料の状態は実際に電子顕
微鏡で観察してみなければわからず、それで失敗すれば
終わりであったが、この発明では、試料を電子顕微鏡内
に設置して電子顕微鏡で実際に観察しながら研磨するの
で、たとえ電子顕微鏡外で作るのに失敗した試料でも製
作者自身の希望する試料の局所場所あるいは形状にサブ
ミクロンのオーダーで研磨することが可能となる。以上
の長所を持つ本装置は微小領域研磨装置として広く普及
することが期待される。According to the conventional method for producing a sample for an electron microscope, it is almost impossible to obtain a clean surface because the sample is always exposed to the atmosphere or solution before being inserted into the electron microscope. Met. However, in the present invention, since the sample is inserted into the scanning transmission electron microscope and then the polishing is performed, even a sample whose surface is contaminated can be scraped off immediately before observation. Further, as the polishing accuracy, the state of the thin film sample prepared in the past cannot be known unless actually observed with an electron microscope, and if it fails, it ends. Since it is installed on the surface and polished while actually observing with an electron microscope, even a sample that could not be made outside the electron microscope can be polished in the sub-micron order at the local location or shape of the sample desired by the manufacturer himself. It will be possible. It is expected that the present apparatus having the above advantages will be widely spread as a fine area polishing apparatus.
【図１】ＦＩＢカラムを取り付けた２００ｋＶ走査透過
型電子顕微鏡の試料室の概要を示す構成図である。斜め
上方５５度に集束イオンビームカラムを取付、試料まで
の距離を９７．５ｍｍとした。FIG. 1 is a configuration diagram showing an outline of a sample chamber of a 200 kV scanning transmission electron microscope equipped with a FIB column. A focused ion beam column was attached at an angle of 55 degrees obliquely above, and the distance to the sample was set to 97.5 mm.
【図２】Ｇａ−ＦＩＢでＳｉ（１００）の微小領域を研
磨した透過型電子顕微鏡用の薄膜を表わした図面に代わ
る写真である。ａ）はａｒｅａ ｓｃａｎしたもので、
ｂ）はｌｉｎｅ ｓｃａｎしたものである。Ｓｉ薄膜表
面は均一に研磨されており、Ｌｉｎｅ走査モードでの微
細加工線幅は最小で０．１５μｍ程度である。FIG. 2 is a photograph replacing a drawing showing a thin film for a transmission electron microscope in which a minute region of Si (100) is polished by Ga-FIB. a) is an area scan,
b) is a line scan. The surface of the Si thin film is uniformly polished, and the minimum line width for fine processing in the Line scanning mode is about 0.15 μm.
１ ＦＩＢカラム ２ 対物ポールピース 1 FIB column 2 Objective pole piece
─────────────────────────────────────────────────────
─────────────────────────────────────────────────── ───
【手続補正書】[Procedure amendment]
【提出日】平成６年２月７日[Submission date] February 7, 1994
【手続補正１】[Procedure Amendment 1]
【補正対象書類名】明細書[Document name to be amended] Statement
【補正対象項目名】発明の名称[Name of item to be amended] Title of invention
【補正方法】変更[Correction method] Change
【補正内容】[Correction content]
【発明の名称】 透過型電子顕微鏡用薄膜試料のその
場作製および観察方法並びにその装置Title: In-situ preparation and observation method of thin film sample for transmission electron microscope and its apparatus
【手続補正１】[Procedure Amendment 1]
【補正対象書類名】図面[Document name to be corrected] Drawing
【補正対象項目名】全図[Correction target item name] All drawings
【補正方法】変更[Correction method] Change
【補正内容】[Correction content]
【図１】 [Figure 1]
【図２】 [Fig. 2]
Claims (3)
集束イオンビームを照射し、該試料の特定の局所領域を
研磨すると同時に観察することを特徴とする透過型電子
顕微鏡用の薄膜試料のその場作製および観察方法。1. A thin film sample for a transmission electron microscope, which comprises irradiating a sample under observation with a transmission electron microscope with a focused ion beam, polishing a specific local region of the sample, and simultaneously observing the sample. In-situ fabrication and observation method.
ように集束イオンビーム照射装置を透過型電子顕微鏡に
取付け、電子線と集束イオンビームを試料上の同一場所
に照射し、薄膜試料を観察しながら研磨することを特徴
とする透過型電子顕微鏡用の薄膜試料のその場作製およ
び観察装置。2. A thin film sample is observed by irradiating a focused ion beam irradiation device on a transmission electron microscope so that a thin film sample is finely polished in the electron microscope, and irradiating an electron beam and a focused ion beam at the same place on the sample. An in-situ preparation and observation apparatus for a thin film sample for a transmission electron microscope, which is characterized by polishing while performing polishing.
顕微鏡の試料室の前方斜め上方から透過型電子顕微鏡に
取付け、透過型電子顕微鏡の走査系および２次電子検出
器を集束イオンビーム照射装置の試料の微細研磨加工手
段に兼用することを特徴とする請求項２の透過型電子顕
微鏡用の薄膜試料のその場作製および観察装置。3. A focused ion beam irradiation device is attached to a transmission electron microscope from diagonally above and in front of a sample chamber of the transmission electron microscope, and a scanning system and a secondary electron detector of the transmission electron microscope are installed in the focused ion beam irradiation device. The in-situ preparation and observation apparatus for a thin film sample for a transmission electron microscope according to claim 2, which is also used as a means for finely polishing a sample.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| JP5067341A JP2987417B2 (en) | 1993-03-04 | 1993-03-04 | In-situ preparation and observation method of thin film sample for transmission electron microscope and its apparatus |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| JP5067341A JP2987417B2 (en) | 1993-03-04 | 1993-03-04 | In-situ preparation and observation method of thin film sample for transmission electron microscope and its apparatus |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| JPH0792062A true JPH0792062A (en) | 1995-04-07 |
| JP2987417B2 JP2987417B2 (en) | 1999-12-06 |
Family
ID=13342232
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| JP5067341A Expired - Lifetime JP2987417B2 (en) | 1993-03-04 | 1993-03-04 | In-situ preparation and observation method of thin film sample for transmission electron microscope and its apparatus |
Country Status (1)
| Country | Link |
|---|---|
| JP (1) | JP2987417B2 (en) |
Cited By (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| WO1997005644A1 (en) * | 1995-07-25 | 1997-02-13 | Nmi Naturwissenschaftliches Und Medizinisches Institut An Der Universität Tübingen In Reutlingen | Process and device for ion thinning in a high-resolution transmission electron microscope |
| KR20010006414A (en) * | 1998-03-03 | 2001-01-26 | 게스레이 마크 | Electron-beam microcolumn as a general purpose scanning electron microscope |
| KR100671156B1 (en) * | 2004-12-24 | 2007-01-17 | 동부일렉트로닉스 주식회사 | Assembly of detector basic unit and optical amplifier tube of scanning electron microscope |
| US7928377B2 (en) | 2004-10-27 | 2011-04-19 | Hitachi High-Technologies Corporation | Charged particle beam apparatus and sample manufacturing method |
| CN112730006A (en) * | 2021-02-05 | 2021-04-30 | 上海市计量测试技术研究院 | Preparation method of pore surface ion channel contrast sample |
Citations (7)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JPS5299495A (en) * | 1976-02-18 | 1977-08-20 | Hitachi Ltd | Machining apparatus in use of ion beam |
| JPS60185352A (en) * | 1984-01-19 | 1985-09-20 | デユビリエ ピ−エルシ− | Charged particle optical system |
| JPS61176764U (en) * | 1985-04-24 | 1986-11-04 | ||
| JPS6312153U (en) * | 1986-07-08 | 1988-01-26 | ||
| JPH02132345A (en) * | 1988-11-14 | 1990-05-21 | Mitsubishi Electric Corp | Manufacture of thin film specimen |
| JPH0623172A (en) * | 1992-07-09 | 1994-02-01 | Mamoru Shimizu | Coincident edge part holding method for stereoscopic sewing |
| JPH06231719A (en) * | 1993-02-03 | 1994-08-19 | Seiko Instr Inc | Charged beam device for sectional working observation and working method |
-
1993
- 1993-03-04 JP JP5067341A patent/JP2987417B2/en not_active Expired - Lifetime
Patent Citations (7)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JPS5299495A (en) * | 1976-02-18 | 1977-08-20 | Hitachi Ltd | Machining apparatus in use of ion beam |
| JPS60185352A (en) * | 1984-01-19 | 1985-09-20 | デユビリエ ピ−エルシ− | Charged particle optical system |
| JPS61176764U (en) * | 1985-04-24 | 1986-11-04 | ||
| JPS6312153U (en) * | 1986-07-08 | 1988-01-26 | ||
| JPH02132345A (en) * | 1988-11-14 | 1990-05-21 | Mitsubishi Electric Corp | Manufacture of thin film specimen |
| JPH0623172A (en) * | 1992-07-09 | 1994-02-01 | Mamoru Shimizu | Coincident edge part holding method for stereoscopic sewing |
| JPH06231719A (en) * | 1993-02-03 | 1994-08-19 | Seiko Instr Inc | Charged beam device for sectional working observation and working method |
Cited By (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| WO1997005644A1 (en) * | 1995-07-25 | 1997-02-13 | Nmi Naturwissenschaftliches Und Medizinisches Institut An Der Universität Tübingen In Reutlingen | Process and device for ion thinning in a high-resolution transmission electron microscope |
| US6218663B1 (en) | 1995-07-25 | 2001-04-17 | Nmi Naturwissenschaftliches Und Medizinisches | Process and device for ion thinning in a high resolution transmission electron microscope |
| KR20010006414A (en) * | 1998-03-03 | 2001-01-26 | 게스레이 마크 | Electron-beam microcolumn as a general purpose scanning electron microscope |
| US7928377B2 (en) | 2004-10-27 | 2011-04-19 | Hitachi High-Technologies Corporation | Charged particle beam apparatus and sample manufacturing method |
| KR100671156B1 (en) * | 2004-12-24 | 2007-01-17 | 동부일렉트로닉스 주식회사 | Assembly of detector basic unit and optical amplifier tube of scanning electron microscope |
| CN112730006A (en) * | 2021-02-05 | 2021-04-30 | 上海市计量测试技术研究院 | Preparation method of pore surface ion channel contrast sample |
Also Published As
| Publication number | Publication date |
|---|---|
| JP2987417B2 (en) | 1999-12-06 |
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