JPH0628992A - Transmission type electron microscope aperture and its manufacture - Google Patents
Transmission type electron microscope aperture and its manufactureInfo
- Publication number
- JPH0628992A JPH0628992A JP4206232A JP20623292A JPH0628992A JP H0628992 A JPH0628992 A JP H0628992A JP 4206232 A JP4206232 A JP 4206232A JP 20623292 A JP20623292 A JP 20623292A JP H0628992 A JPH0628992 A JP H0628992A
- Authority
- JP
- Japan
- Prior art keywords
- electron beam
- aperture
- opening
- electron microscope
- layer
- 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 abstract description 11
- 238000004519 manufacturing process Methods 0.000 title claims description 6
- 238000010894 electron beam technology Methods 0.000 claims abstract description 26
- 239000000463 material Substances 0.000 claims abstract description 14
- 238000005530 etching Methods 0.000 claims abstract description 6
- 230000000903 blocking effect Effects 0.000 claims description 15
- 238000000034 method Methods 0.000 claims description 12
- 239000013078 crystal Substances 0.000 claims description 2
- KRHYYFGTRYWZRS-UHFFFAOYSA-N Fluorane Chemical compound F KRHYYFGTRYWZRS-UHFFFAOYSA-N 0.000 description 6
- 229910001218 Gallium arsenide Inorganic materials 0.000 description 5
- 229910004298 SiO 2 Inorganic materials 0.000 description 5
- 239000010931 gold Substances 0.000 description 5
- NBIIXXVUZAFLBC-UHFFFAOYSA-N Phosphoric acid Chemical compound OP(O)(O)=O NBIIXXVUZAFLBC-UHFFFAOYSA-N 0.000 description 4
- 229910052782 aluminium Inorganic materials 0.000 description 4
- PCHJSUWPFVWCPO-UHFFFAOYSA-N gold Chemical compound [Au] PCHJSUWPFVWCPO-UHFFFAOYSA-N 0.000 description 4
- 229910052737 gold Inorganic materials 0.000 description 4
- 229910052751 metal Inorganic materials 0.000 description 4
- 239000002184 metal Substances 0.000 description 4
- XAGFODPZIPBFFR-UHFFFAOYSA-N aluminium Chemical compound [Al] XAGFODPZIPBFFR-UHFFFAOYSA-N 0.000 description 3
- 229910000147 aluminium phosphate Inorganic materials 0.000 description 2
- 125000004429 atom Chemical group 0.000 description 2
- 238000000206 photolithography Methods 0.000 description 2
- RTAQQCXQSZGOHL-UHFFFAOYSA-N Titanium Chemical compound [Ti] RTAQQCXQSZGOHL-UHFFFAOYSA-N 0.000 description 1
- 230000001133 acceleration Effects 0.000 description 1
- 239000003795 chemical substances by application Substances 0.000 description 1
- 238000010586 diagram Methods 0.000 description 1
- 238000009713 electroplating Methods 0.000 description 1
- 238000011156 evaluation Methods 0.000 description 1
- 229910052733 gallium Inorganic materials 0.000 description 1
- 125000005842 heteroatom Chemical group 0.000 description 1
- 238000003754 machining Methods 0.000 description 1
- 150000002739 metals Chemical class 0.000 description 1
- 238000001000 micrograph Methods 0.000 description 1
- 239000004065 semiconductor Substances 0.000 description 1
- 239000003362 semiconductor superlattice Substances 0.000 description 1
- 239000010936 titanium Substances 0.000 description 1
- 229910052719 titanium Inorganic materials 0.000 description 1
- 238000001947 vapour-phase growth Methods 0.000 description 1
Abstract
Description
【０００１】[0001]
【産業上の利用分野】本発明は、透過電子顕微鏡用アパ
ーチャおよびその製造法に関する。BACKGROUND OF THE INVENTION 1. Field of the Invention The present invention relates to an aperture for a transmission electron microscope and a method for manufacturing the aperture.
【０００２】[0002]
【従来の技術】透過電子顕微鏡（ＴＥＭ）法は、金属や
半導体などの原子レベルでの構造観察が可能であり、半
導体超格子界面の評価などには不可欠な観察法である。
通常は、すべての回折スポットから像を構成する明視野
像の観察が行われるが、特定の回折スポットだけを選
び、これらのスポットで像を構成する観察法もしばしば
用いられる。ＧａＡｓ−ＡｌＡｓ超格子界面の観察を例
にとると、Ｇａ原子とＡｌ原子の散乱能の違いをよく反
映する回折線のみで像を構成することにより、より鮮明
な界面の像を得ることができる（N.Ikarashiほか、マテ
リアル・リサーチ・ソサエティ・シンポジウム・プロシ
ーディング，第183巻，187ページ，1990年［Materials
Research Society Symposium Proceedings 183(199
0)］）。このような観察を行う際は、特定の回折電子線
だけを選別するため、試料の後ろにアパーチャが挿入さ
れる。アパーチャは、金属の薄片に小孔を開けたもの
で、小孔の大きさは使用加速電圧にもよるが、直径数十
μｍ程度である。2. Description of the Related Art The transmission electron microscope (TEM) method allows observation of the structure of metals and semiconductors at the atomic level, and is an indispensable observation method for evaluation of semiconductor superlattice interfaces.
Normally, a bright field image forming an image is observed from all diffraction spots, but an observation method of selecting only a specific diffraction spot and forming an image with these spots is also often used. Taking the observation of the GaAs-AlAs superlattice interface as an example, a clearer image of the interface can be obtained by constructing the image only with diffraction lines that well reflect the difference in the scattering ability of Ga atoms and Al atoms. (N.Ikarashi et al., Material Research Society Symposium Proceedings, Volume 183, p. 187, 1990 [Materials
Research Society Symposium Proceedings 183 (199
0)]). When performing such an observation, an aperture is inserted behind the sample in order to select only a specific diffracted electron beam. The aperture is a thin piece of metal with a small hole, and the size of the small hole is about several tens of μm, although it depends on the accelerating voltage used.
【０００３】[0003]
【発明が解決しようとする課題】アパーチャ径の精度
は、例えばＳｉやＧａＡｓの観察において、隣合う回折
線を分離するために、±２μｍ以下である必要がある。
従来、アパーチャは、厚さ１０〜１００μｍ程度の金属
片に放電加工により小孔を開けて製作されてきた。この
手法では５μｍ以下の精度で小孔の直径を制御すること
は困難であった。金属片を薄くすることにより精度は向
上するが、強度的な問題から限界がある。また、アパー
チャの開口部形状は、円以外は製作不可能であった。本
発明は、このような従来の課題を解決して、高精度でか
つ開口部形状の自由度の高い透過電子顕微鏡用アパーチ
ャおよびその製造法を提供することを目的とする。The accuracy of the aperture diameter needs to be ± 2 μm or less in order to separate adjacent diffraction lines when observing Si or GaAs, for example.
Conventionally, an aperture has been manufactured by making a small hole in a metal piece having a thickness of about 10 to 100 μm by electric discharge machining. With this method, it was difficult to control the diameter of the small holes with an accuracy of 5 μm or less. The accuracy is improved by making the metal piece thin, but there is a limit due to the problem of strength. In addition, the shape of the aperture of the aperture could not be manufactured except for the circle. SUMMARY OF THE INVENTION It is an object of the present invention to solve such conventional problems and provide an aperture for a transmission electron microscope with high accuracy and a high degree of freedom in the shape of an opening, and a method for manufacturing the aperture.
【０００４】[0004]
【課題を解決するための手段】本発明は、第１の材質か
らなる電子線阻止層と、第２の材質からなる支持層との
２層構造を少なくとも有し、前記電子線阻止層に形成さ
れた第１の開口部と、前記支持層に形成されて前記第１
の開口部を見通し、かつ該第１の開口部よりも面積の大
きな第２の開口部とからなる開口部を備えてなることを
特徴とする電子顕微鏡用アパーチャである。また本発明
によれば、開口部を複数個備え、該開口部が被観察結晶
の逆格子点を電子線照射方向に投影した点のいずれかの
位置に設けられている透過電子顕微鏡用アパーチャが提
供される。本発明による透過電子顕微鏡用アパーチャの
製造法は、所定の位置に開口部を有し、後記する第２の
材質のエッチング剤によりエッチングされない第１の材
質からなる電子線阻止層を第２の材質からなる支持層上
に形成する工程と、前記電子線阻止層をマスクとして前
記支持層をエッチングし、前記支持層に貫通孔を形成す
る工程とからなることを特徴とする。The present invention has at least a two-layer structure of an electron beam blocking layer made of a first material and a support layer made of a second material, and is formed in the electron beam blocking layer. And a first opening formed in the support layer.
The aperture for the electron microscope is characterized in that it includes an opening that is in front of the first opening and has a second opening having a larger area than the first opening. Further, according to the present invention, there is provided an aperture for a transmission electron microscope, which comprises a plurality of openings, the openings being provided at any position of the points where the reciprocal lattice points of the crystal to be observed are projected in the electron beam irradiation direction. Provided. A method of manufacturing an aperture for a transmission electron microscope according to the present invention includes an electron beam blocking layer made of a first material, which has an opening at a predetermined position and is not etched by an etching agent of a second material, which will be described later. And a step of forming a through hole in the support layer by etching the support layer using the electron beam blocking layer as a mask.
【０００５】[0005]
【作用】本発明によれば、アパーチャの機械的強度は支
持層の厚さで決まる。このため、電子線阻止層の厚さを
電子線が透過しない程度まで薄くすることができる。例
えばアルミニウムを阻止層に用いた場合、加速電圧４０
０ｋＶの電子線に対する透過能はμ-1＝２０００Ａ程度
であるから、１μｍ以上の厚さであれば電子線阻止層と
して十分機能する。金やチタンを阻止層に用いれば、厚
さをさらに薄くすることができる。開口部を形成する際
の精度は、電子線阻止層の厚さと同程度かそれ以下であ
るから、本発明によるアパーチャの開口部精度は１μｍ
以下となる。また、フォトリソグラフィー技術を用いれ
ば、開口部形状やその数を任意のものとすることができ
る。According to the present invention, the mechanical strength of the aperture is determined by the thickness of the support layer. Therefore, the thickness of the electron beam blocking layer can be reduced to such an extent that the electron beam does not pass therethrough. For example, when aluminum is used as the blocking layer, an acceleration voltage of 40
Since the transmissivity for an electron beam of 0 kV is about μ −1 = 2000 A, a thickness of 1 μm or more sufficiently functions as an electron beam blocking layer. If gold or titanium is used for the blocking layer, the thickness can be further reduced. Since the accuracy in forming the opening is equal to or less than the thickness of the electron beam blocking layer, the opening accuracy of the aperture according to the present invention is 1 μm.
It becomes the following. Further, by using the photolithography technique, the shape of the openings and the number thereof can be made arbitrary.
【０００６】[0006]
【実施例】以下、本発明の実施例について、図面を用い
て詳細に説明する。図１は、電子線阻止層に金、支持層
にアルミニウムを用いた本発明によるアパーチャの形成
工程を示す図である。厚さ２００μｍのアルミニウム１
０１上に、気相成長法で酸化膜（ＳｉＯ2）を２μｍ堆
積させた。次に図１（ａ）に示すようにフォトリソグラ
フィー技術により１０μｍ径の円状にＳｉＯ2１０２を
残し、残りをバッファードフッ酸で取り去る。この後、
図１（ｂ）に示すように電解メッキにより金１０３を厚
さ２μｍメッキする。ＳｉＯ2１０２が残された部分は
メッキされないため、結果として１０μｍ径の小孔が形
成される。ＳｉＯ2１０２をバッファードフッ酸により
取り去り第１の開口部を形成した後、リン酸系エッチン
グ液を用いてＡｌをエッチングして第２の開口部を形成
し、、図１（ｃ）に示すように第１の開口部と第２の開
口部よりなる開口部１０４を形成する。金はバッファー
ドフッ酸やリン酸に侵されないため、開口部の面積はメ
ッキされたときのものと同一となる。Embodiments of the present invention will be described in detail below with reference to the drawings. FIG. 1 is a diagram showing a process of forming an aperture according to the present invention in which gold is used for an electron beam blocking layer and aluminum is used for a support layer. 200 μm thick aluminum 1
An oxide film (SiO 2 ) having a thickness of 2 μm was deposited on No. 01 by a vapor phase growth method. Next, as shown in FIG. 1A, the SiO 2 102 is left in a circular shape having a diameter of 10 μm by a photolithography technique, and the rest is removed with buffered hydrofluoric acid. After this,
As shown in FIG. 1B, gold 103 is plated to a thickness of 2 μm by electrolytic plating. Since the portion where the SiO 2 102 is left is not plated, a small hole having a diameter of 10 μm is formed as a result. After removing SiO 2 102 with buffered hydrofluoric acid to form a first opening, Al is etched with a phosphoric acid-based etching solution to form a second opening, as shown in FIG. 1 (c). Thus, the opening 104 including the first opening and the second opening is formed. Since gold is not attacked by buffered hydrofluoric acid or phosphoric acid, the area of the opening is the same as when plated.
【０００７】上記の形成方法を用い、ＧａＡｓの［１０
０］方向に対する逆格子点のうち、（００）、（１
０）、（１１）に対応する位置に開口部が設けられたア
パーチャを作製した。これらの回折電子線のみで結ばれ
た電子顕微鏡像はＧａとＡｌに対するコントラストが通
常の明視野像よりも高くなることが報告されている（N.
Ikarashiほか、マテリアル・リサーチ・ソサエティ・シ
ンポジウム・プロシーディング，第183巻，187ページ，
1990年［Materials Research Society Symposium Proce
edings 183(1990)］）。本アパーチャを加速電圧２００
ｋＶの透過電子顕微鏡に装着し、ＧａＡｓ（１００）上
に形成されたＧａＡｓ／ＡｌＡｓ量子井戸構造を［１０
０］方向から観察した。その結果、開口部以外の部分に
入射した電子線は電子線阻止層により透過しないことが
確認された。また長時間の使用に際しても、開口部形状
の変形等はみられず、機械的にも十分な強度を持つこと
が明らかとなった。また本アパーチャにより、従来のも
のに比べコントラストの高いＧａＡｓ／ＡｌＡｓヘテロ
界面の像が得られた。本実施例では開口部形状が円のも
のについて述べたが、その他の形状についても同様の結
果が得られることは明らかである。Using the above forming method, GaAs [10
Of the reciprocal lattice points for the [0] direction, (00), (1
Apertures having openings provided at positions corresponding to 0) and (11) were produced. It has been reported that the contrast of Ga and Al in an electron microscope image formed only by these diffracted electron beams is higher than that in a normal bright field image (N.
Ikarashi et al., Material Research Society Symposium Proceedings, Volume 183, 187 pages,
1990 [Materials Research Society Symposium Proce
edings 183 (1990)]). Accelerating voltage of 200 for this aperture
The GaAs / AlAs quantum well structure formed on GaAs (100) was attached to a transmission electron microscope of kV [10
It was observed from the [0] direction. As a result, it was confirmed that the electron beam incident on the portion other than the opening was not transmitted by the electron beam blocking layer. In addition, it was revealed that the shape of the opening was not deformed even when it was used for a long time, and that it had sufficient mechanical strength. In addition, the image of the GaAs / AlAs hetero interface having a higher contrast than that of the conventional one was obtained by this aperture. In the present embodiment, the shape of the opening is circular, but it is clear that similar results can be obtained with other shapes.
【０００８】[0008]
【発明の効果】以上説明したように、本発明によれば開
口部の加工精度の高い透過電子顕微鏡用アパーチャを得
ることができる。また得られたアパーチャは十分な機械
強度をもち、しかも開口部の形状に対する自由度が高い
ものである。As described above, according to the present invention, it is possible to obtain an aperture for a transmission electron microscope having a high processing accuracy of the opening. The obtained aperture has sufficient mechanical strength and has a high degree of freedom with respect to the shape of the opening.
【図１】本発明による電子顕微鏡用アパーチャの製造法
を工程順に示す断面図である。FIG. 1 is a cross-sectional view showing a method of manufacturing an aperture for an electron microscope according to the present invention in the order of steps.
１０１ Ａｌ １０２ ＳｉＯ2 １０３ Ａｕ １０４ 開口部101 Al 102 SiO 2 103 Au 104 Opening
Claims (3)
２の材質からなる支持層との２層構造を少なくとも有
し、前記電子線阻止層に形成された第１の開口部と、前
記支持層に形成されて前記第１の開口部を見通し、かつ
該第１の開口部よりも面積の大きな第２の開口部とから
なる開口部を備えてなることを特徴とする電子顕微鏡用
アパーチャ。1. A first opening formed in the electron beam blocking layer, which has at least a two-layer structure of an electron beam blocking layer made of a first material and a support layer made of a second material. An electron microscope, comprising: an opening formed in the support layer, which is in front of the first opening, and which has a second opening having an area larger than that of the first opening. Aperture.
結晶の逆格子点を電子線照射方向に投影した点のいずれ
かの位置に設けられている請求項１記載の透過電子顕微
鏡用アパーチャ。2. The transmission electron microscope according to claim 1, wherein a plurality of openings are provided, and the openings are provided at any positions of the points where the reciprocal lattice points of the crystal to be observed are projected in the electron beam irradiation direction. Aperture.
２の材質のエッチング剤によりエッチングされない第１
の材質からなる電子線阻止層を第２の材質からなる支持
層上に形成する工程と、前記電子線阻止層をマスクとし
て前記支持層をエッチングし、前記支持層に貫通孔を形
成する工程とからなることを特徴とする電子顕微鏡用ア
パーチャの製造法。3. A first device which has an opening at a predetermined position and is not etched by an etching agent of a second material described later.
Forming an electron beam blocking layer made of the above material on a support layer made of a second material, and etching the support layer using the electron beam blocking layer as a mask to form a through hole in the support layer. A method for manufacturing an aperture for an electron microscope, which comprises:
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| JP4206232A JPH0628992A (en) | 1992-07-10 | 1992-07-10 | Transmission type electron microscope aperture and its manufacture |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| JP4206232A JPH0628992A (en) | 1992-07-10 | 1992-07-10 | Transmission type electron microscope aperture and its manufacture |
Publications (1)
| Publication Number | Publication Date |
|---|---|
| JPH0628992A true JPH0628992A (en) | 1994-02-04 |
Family
ID=16519950
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| JP4206232A Pending JPH0628992A (en) | 1992-07-10 | 1992-07-10 | Transmission type electron microscope aperture and its manufacture |
Country Status (1)
| Country | Link |
|---|---|
| JP (1) | JPH0628992A (en) |
Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| WO2009081897A1 (en) * | 2007-12-21 | 2009-07-02 | Daiwa Techno Systems Co., Ltd. | Filming treatment jig, plasma cvd apparatus, and metal plate and osmium film forming method |
| JP2013083006A (en) * | 2012-12-17 | 2013-05-09 | Utec:Kk | Metal plate, and film deposition method of osmium film |
-
1992
- 1992-07-10 JP JP4206232A patent/JPH0628992A/en active Pending
Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| WO2009081897A1 (en) * | 2007-12-21 | 2009-07-02 | Daiwa Techno Systems Co., Ltd. | Filming treatment jig, plasma cvd apparatus, and metal plate and osmium film forming method |
| JP2009149949A (en) * | 2007-12-21 | 2009-07-09 | Utec:Kk | Tool for film deposition treatment, plasma cvd system, metal plate, and osmium film deposition method |
| US9714468B2 (en) | 2007-12-21 | 2017-07-25 | Daiwa Techno Systems Co., Ltd. | Film-forming method of an osmium film |
| JP2013083006A (en) * | 2012-12-17 | 2013-05-09 | Utec:Kk | Metal plate, and film deposition method of osmium film |
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