JP2622322B2 - Method of manufacturing probe for atomic force microscope - Google Patents
Method of manufacturing probe for atomic force microscopeInfo
- Publication number
- JP2622322B2 JP2622322B2 JP34451791A JP34451791A JP2622322B2 JP 2622322 B2 JP2622322 B2 JP 2622322B2 JP 34451791 A JP34451791 A JP 34451791A JP 34451791 A JP34451791 A JP 34451791A JP 2622322 B2 JP2622322 B2 JP 2622322B2
- Authority
- JP
- Japan
- Prior art keywords
- probe
- cantilever
- whisker
- force microscope
- atomic force
- 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 - Fee Related
Links
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- Length Measuring Devices With Unspecified Measuring Means (AREA)
Description
【０００１】[0001]
【産業上の利用分野】本発明は、原子間力顕微鏡（以後
ＡＦＭと記す）用探針の製造方法に関し、とりわけ先端
曲率が小さく、アスペクト比の大きい探針の製造方法に
関するものである。BACKGROUND OF THE INVENTION 1. Field of the Invention The present invention relates to a method of manufacturing a probe for an atomic force microscope (hereinafter, referred to as AFM), and more particularly to a method of manufacturing a probe having a small tip curvature and a large aspect ratio.
【０００２】[0002]
【従来の技術】近年、固体表面を原子オーダで観察でき
る装置としてＡＦＭが開発されている。ＡＦＭでは微小
な力を検出するために、図５に示すような探針１５を有
する長さ１００μｍから２００μｍ程度のカンチレバー
１６が必要である。従来、この探針としては、カンチレ
バー先端のエッジ部分を探針として用いたもの、結晶の
エッチピットを鋳型として利用し作製したもの、異方性
エッチングにより作製したもの等が使用されている。Ａ
ＦＭの分解能は前記探針の先端曲率半径に依存し、曲率
半径が小さいほど分解能は上がる。現在のところ２０ｎ
ｍから３０ｎｍの曲率の探針が作製され、このカンチレ
バーを用いてマイカ等の原子像が観察されている。2. Description of the Related Art In recent years, an AFM has been developed as a device capable of observing a solid surface in an atomic order. The AFM requires a cantilever 16 having a length of about 100 μm to 200 μm and having a probe 15 as shown in FIG. 5 in order to detect a small force. Conventionally, as the probe, a probe using the edge portion of the tip of the cantilever as a probe, a probe fabricated using a crystal etch pit as a template, and a probe fabricated by anisotropic etching have been used. A
The resolution of FM depends on the radius of curvature of the tip of the probe, and the smaller the radius of curvature, the higher the resolution. 20n at present
A probe having a curvature of m to 30 nm has been fabricated, and an atomic image of mica or the like has been observed using this cantilever.
【０００３】[0003]
【発明が解決しようとする課題】しかし、ＡＦＭの用途
としては、試料表面の原子レベルでの観察と同時に、ナ
ノメータあるいはミクロンオーダでの凹凸の大きな試料
観察がある。このような試料観察の場合、特にグレーテ
ィング等の深い溝形状を有する試料では、前記のような
探針では、探針が溝部の底まで届かず正確な形状測定が
困難であった。However, applications of the AFM include observation of a sample surface at an atomic level and observation of a sample having large irregularities on the order of nanometers or microns. In the case of such a sample observation, particularly in a sample having a deep groove shape such as a grating, it is difficult to accurately measure the shape with the above-described probe because the probe does not reach the bottom of the groove portion.
【０００４】したがって、このような用途においては、
探針の先端曲率が小さいのと同時に、溝部の底まで届く
ような、細長い形状の探針を有するカンチレバーが要望
されている。Therefore, in such an application,
There is a need for a cantilever having an elongated probe that has a small tip curvature and reaches the bottom of the groove at the same time.
【０００５】本発明は、このような従来の原子間力顕微
鏡用探針の問題を解決するため、深い溝形状を有するよ
うな試料でも、精度良く観察することが可能な、高アス
ペクト比でしかも先端曲率が極めて小さい原子間力顕微
鏡用探針の製造方法を提供することを目的とする。According to the present invention, in order to solve the problem of the conventional probe for an atomic force microscope, a sample having a deep groove shape can be observed with high accuracy and has a high aspect ratio. An object of the present invention is to provide a method of manufacturing a probe for an atomic force microscope having an extremely small tip curvature.
【０００６】[0006]
【課題を解決するための手段】前記目的を達成するた
め、本発明の原子間力顕微鏡用探針の第１の製造方法
は、成長途中のテトラポッド形状の酸化亜鉛ウィスカ
を、カンチレバー先端部に固着した後、前記の固着した
ウィスカをさらに成長させ、先端の尖ったウィスカに形
成するという構成を備えたものである。In order to achieve the above object, a first method for manufacturing a probe for an atomic force microscope according to the present invention is to provide a tetrapod-shaped zinc oxide whisker during growth at the tip of a cantilever. After the whisker is fixed, the whisker is further grown to form a whisker with a sharp tip.
【０００７】次に本発明の原子間力顕微鏡用探針の第２
の製造方法は、酸化亜鉛ウィスカを成長させる原料微粒
子を、カンチレバー先端部に固着した後、前記微粒子か
ら酸化亜鉛ウィスカを成長させるという構成を備えたも
のである。Next, the second embodiment of the probe for an atomic force microscope according to the present invention will be described.
The manufacturing method of (1) has a configuration in which raw material fine particles for growing zinc oxide whiskers are fixed to the tip of the cantilever, and then zinc oxide whiskers are grown from the fine particles.
【０００８】前記構成においては、カンチレバーがシリ
コン酸化膜であることが好ましい。また前記構成におい
ては、カンチレバーがシリコン窒化膜であることが好ま
しい。In the above structure, it is preferable that the cantilever is a silicon oxide film. In the above configuration, it is preferable that the cantilever is a silicon nitride film.
【０００９】[0009]
【作用】前記本発明の構成によれば、酸化亜鉛ウィスカ
は、先端部の曲率半径が５ｎｍ以下で、高アスペクト比
を有した針状単結晶であり、長さ１μｍから２０μｍ程
度のものまで容易に得られる。したがってこのウィスカ
を探針に用いれば、分解能の高いＡＦＭが得られる。ま
た、本発明の製造方法を用いて前記探針を作製すること
で、酸化亜鉛ウィスカをカンチレバーに固着する時に起
こるウィスカ先端部の損傷を防ぐことができる。すなわ
ち、本発明の第１及び第２製造方法によれば、いずれも
結晶成長させたウィスカをそのままの状態で探針として
用いることができるからである。According to the structure of the present invention, the zinc oxide whiskers are needle-like single crystals having a high radius of curvature of 5 nm or less at the tip and having a high aspect ratio. Is obtained. Therefore, if this whisker is used for a probe, an AFM with high resolution can be obtained. Further, by manufacturing the probe using the manufacturing method of the present invention, it is possible to prevent the tip of the whisker from being damaged when the zinc oxide whisker is fixed to the cantilever. That is, according to the first and second manufacturing methods of the present invention, it is possible to use the whisker on which the crystal has been grown as it is, as it is, as a probe.
【００１０】[0010]
【実施例】以下、実施例を用いて本発明をさらに具体的
に説明する。 実施例１ 図１は、本発明の第１実施例におけるＡＦＭ用探針の製
造プロセスである。１μｍから１００μｍの亜鉛微粒子
表面を水中で酸化する。前記微粒子を乾燥後、酸素雰囲
気中で９２０℃に加熱し、テトラポッド形状の酸化亜鉛
ウィスカ１を途中まで成長させた後、前記ウィスカを銀
ペースト２を用いて、フォトリソグラフィーにより作製
した長さ１００μｍ、厚さ１．５μｍのＶ型のＳｉＯ2
薄膜カンチレバー３の先端部分に取り付ける。酸化亜鉛
ウィスカ１は、テトラポッド状であるから、３つの脚部
で安定して固着でき、かつ残りの先端部をカンチレバー
３から実質的に垂直方向に配向させることができる。EXAMPLES Hereinafter, the present invention will be described more specifically with reference to examples. Embodiment 1 FIG. 1 shows a manufacturing process of an AFM probe according to a first embodiment of the present invention. The surface of zinc fine particles of 1 μm to 100 μm is oxidized in water. After drying the fine particles, the particles were heated to 920 ° C. in an oxygen atmosphere to grow a zinc oxide whisker 1 in a tetrapod shape halfway, and then the whisker was formed by photolithography using a silver paste 2 to a length of 100 μm. V-type SiO 2 with a thickness of 1.5 μm
It is attached to the tip of the thin film cantilever 3. Since the zinc oxide whisker 1 has a tetrapod shape, it can be stably fixed by three legs, and the remaining tip can be oriented substantially vertically from the cantilever 3.
【００１１】その後、再び酸素雰囲気中で９２０℃に加
熱し、テトラポッド形状の酸化亜鉛ウィスカ４を完全に
成長させる。成長した酸化亜鉛ウィスカの各脚の長さは
５μｍから２０μｍであった。また、酸化亜鉛ウィスカ
の脚の先端部は透過電子顕微鏡により観察した結果５ｎ
ｍ以下の曲率半径を有していた。ＡＦＭ用探針には、カ
ンチレバー主面に垂直方向に成長したウィスカの脚を用
いる。この製造プロセスではカンチレバーに接着後、ウ
ィスカ先端部を成長させるため、カンチレバーとウィス
カの接着時に起こるウィスカ先端部の損傷を防ぐことが
できる。Thereafter, the substrate is again heated to 920 ° C. in an oxygen atmosphere to completely grow the tetrapod-shaped zinc oxide whiskers 4. The length of each leg of the grown zinc oxide whiskers was 5 μm to 20 μm. The tip of the leg of the zinc oxide whisker was observed by a transmission electron microscope to be 5n.
m or less. As the AFM probe, a whisker leg grown in a direction perpendicular to the main surface of the cantilever is used. In this manufacturing process, since the tip of the whisker is grown after bonding to the cantilever, damage to the tip of the whisker that occurs when the cantilever and the whisker are bonded can be prevented.
【００１２】実施例２ 第２実施例におけるＡＦＭ用探針の製造プロセスを図２
に示す。まず、１μｍから１００μｍの亜鉛微粒子表面
を水中で酸化する。前記微粒子５を乾燥後、銀ペースト
６を用いて、フォトリソグラフィー技術により作製した
厚さ０．６μｍ、長さ１００μｍのＶ型のＳｉ3 Ｎ4 薄
膜カンチレバー７の先端部分に取り付ける。その後、酸
素雰囲気中で９２０℃に加熱し、酸化亜鉛ウィスカ８を
成長させる。この製造プロセスでは、第１実施例と同様
に、カンチレバーに接着後、ウィスカを成長させるた
め、カンチレバーとウィスカの接着時に起こるウィスカ
先端部の損傷を防ぐことができる。Embodiment 2 FIG. 2 shows a manufacturing process of an AFM probe according to a second embodiment.
Shown in First, the surface of zinc fine particles of 1 μm to 100 μm is oxidized in water. After the fine particles 5 are dried, they are attached to the tip of a V-type Si 3 N 4 thin film cantilever 7 having a thickness of 0.6 μm and a length of 100 μm manufactured by photolithography using a silver paste 6. Thereafter, the substrate is heated to 920 ° C. in an oxygen atmosphere to grow zinc oxide whiskers 8. In this manufacturing process, as in the first embodiment, the whisker is grown after bonding to the cantilever, so that damage to the tip of the whisker that occurs when the cantilever and the whisker are bonded can be prevented.
【００１３】このカンチレバーを原子間力顕微鏡に取り
付け、深さ１μｍ、幅１μｍの溝形状を有する試料の観
察を行い、Ｓｉのエッチピットを鋳型としてＳｉ3 Ｎ4
で探針を作製した従来のカンチレバーとの比較を行っ
た。従来のカンチレバーの場合、探針形状は、Ｓｉ（１
００）面のエッチピット形状で決定され、頂角が約７０
度のピラミッド形状となる。従ってこの探針を有するカ
ンチレバーで溝部を矢印の方向へ走査すれば、図３に示
すように、探針９が溝の底まで届かず、破線で示したよ
うな実際の試料１０の表面形状とは異なる像１１が得ら
れた。一方、ウィスカを探針として有するカンチレバー
では、図４に示すように、ウィスカの探針１２が溝の底
まで達し、試料１３の表面形状に忠実な像１４が得られ
た。The cantilever was attached to an atomic force microscope, a sample having a groove shape of 1 μm in depth and 1 μm in width was observed, and Si 3 N 4 was used with the Si etch pit as a template.
A comparison was made with a conventional cantilever in which a probe was manufactured. In the case of a conventional cantilever, the probe shape is Si (1
Determined by the shape of the etch pit on the (00) plane, the apex angle is about 70
Pyramid shape of degree. Therefore, if the groove is scanned in the direction of the arrow with the cantilever having the probe, the probe 9 does not reach the bottom of the groove as shown in FIG. A different image 11 was obtained. On the other hand, in the cantilever having a whisker as a probe, as shown in FIG. 4, the probe 12 of the whisker reached the bottom of the groove, and an image 14 faithful to the surface shape of the sample 13 was obtained.
【００１４】なお、酸化亜鉛ウィスカを作製すること自
体は、たとえば亜鉛微粒子表面を水中で酸化後、酸素雰
囲気中で加熱する方法［ジャーナル・オブ・クリスタル
・グロース102(1990年) 第965 頁から第973 頁（J. Cry
stal Growth 102,965-973,1990）］などが知られている
が、本発明方法はこのような公知の技術を広く応用する
こともできる。The production of the zinc oxide whisker itself is performed, for example, by oxidizing the surface of the zinc fine particles in water and then heating it in an oxygen atmosphere [Journal of Crystal Growth 102 (1990), p. Page 973 (J. Cry
stal Growth 102, 965-973, 1990)], and the method of the present invention can also widely apply such known techniques.
【００１５】[0015]
【発明の効果】以上述べたところから明らかなように、
本発明によれば、従来、作製困難であった５ｎｍ以下の
先端曲率半径を有し、しかも高アスペクト比のＡＦＭ用
探針を容易に作製することが可能となった。また前記探
針を用いることで、分解能が非常に高く、安定に、再現
性よく試料表面を原子オーダで観察することが可能にな
った。またグレーティング等の深い溝形状を有する試料
を精度よく測定することが可能になった。As is apparent from the above description,
According to the present invention, it has become possible to easily manufacture an AFM probe having a tip curvature radius of 5 nm or less, which has been conventionally difficult to manufacture, and a high aspect ratio. In addition, the use of the probe makes it possible to observe the sample surface in an atomic order with extremely high resolution, stably, and with good reproducibility. In addition, it is possible to accurately measure a sample having a deep groove shape such as a grating.
【図１】本発明の実施例１の原子間力顕微鏡用探針の製
造方法を示すプロセス図である。FIG. 1 is a process diagram showing a method for manufacturing a probe for an atomic force microscope according to a first embodiment of the present invention.
【図２】本発明の実施例２の原子間力顕微鏡用探針の製
造方法を示すプロセス図である。FIG. 2 is a process diagram showing a method for manufacturing a probe for an atomic force microscope according to a second embodiment of the present invention.
【図３】従来の製造方法で作製されたカンチレバーで得
られたＡＦＭ像の説明図である。FIG. 3 is an explanatory diagram of an AFM image obtained by a cantilever manufactured by a conventional manufacturing method.
【図４】本発明の実施例により作製されたカンチレバー
で得られたＡＦＭ像の説明図である。FIG. 4 is an explanatory diagram of an AFM image obtained by a cantilever manufactured according to an example of the present invention.
【図５】従来の原子間力顕微鏡用カンチレバーの概略図
である。FIG. 5 is a schematic view of a conventional cantilever for an atomic force microscope.
１ 成長途中の酸化亜鉛ウィスカ ２、６ 銀ペースト ３ ＳｉＯ2 薄膜カンチレバー ４、８ 酸化亜鉛ウィスカ ５ 表面を酸化した亜鉛微粒子 ７ Ｓｉ3 Ｎ4 薄膜カンチレバー ４、８ 酸化亜鉛ウィスカ ９ Ｓｉ3 Ｎ4 探針 １０、１３ 試料 １１、１４ ＡＦＭ像 １２ ＺｎＯウィスカ探針 １５ 探針 １６ カンチレバーReference Signs List 1 zinc oxide whisker during growth 2, 6 silver paste 3 SiO 2 thin film cantilever 4, 8 zinc oxide whisker 5 zinc fine particles with oxidized surface 7 Si 3 N 4 thin film cantilever 4, 8 zinc oxide whisker 9 Si 3 N 4 probe 10, 13 sample 11, 14 AFM image 12 ZnO whisker probe 15 probe 16 cantilever
Claims (4)
ウィスカを、カンチレバー先端部に固着した後、前記の
固着したウィスカをさらに成長させ、先端の尖ったウィ
スカに形成する原子間力顕微鏡用探針の製造方法。1. An atomic force microscope probe in which a growing tetrapod-shaped zinc oxide whisker is fixed to the tip of a cantilever, and the fixed whisker is further grown to form a whisker with a sharp tip. Manufacturing method.
子を、カンチレバー先端部に固着した後、前記微粒子か
ら酸化亜鉛ウィスカを成長させる原子間力顕微鏡用探針
の製造方法。2. A method of manufacturing a probe for an atomic force microscope, wherein raw material fine particles for growing zinc oxide whiskers are fixed to the tip of a cantilever, and then zinc oxide whiskers are grown from the fine particles.
求項１または２に記載の原子間力顕微鏡用探針の製造方
法。3. The method of manufacturing a probe for an atomic force microscope according to claim 1, wherein the cantilever is a silicon oxide film.
求項１または２に記載の原子間力顕微鏡用探針の製造方
法。4. The method of manufacturing a probe for an atomic force microscope according to claim 1, wherein the cantilever is a silicon nitride film.
Priority Applications (4)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| JP34451791A JP2622322B2 (en) | 1991-12-26 | 1991-12-26 | Method of manufacturing probe for atomic force microscope |
| DE69208979T DE69208979T2 (en) | 1991-07-15 | 1992-07-14 | Cantilever cantilever for atomic force microscope and method for its production |
| EP92111956A EP0530473B1 (en) | 1991-07-15 | 1992-07-14 | Cantilever for atomic force microscope and method of manufacturing the same |
| US08/201,087 US5357787A (en) | 1991-07-15 | 1994-02-24 | Cantilever for atomic force microscope and method of manufacturing the same |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| JP34451791A JP2622322B2 (en) | 1991-12-26 | 1991-12-26 | Method of manufacturing probe for atomic force microscope |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| JPH05172561A JPH05172561A (en) | 1993-07-09 |
| JP2622322B2 true JP2622322B2 (en) | 1997-06-18 |
Family
ID=18369890
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| JP34451791A Expired - Fee Related JP2622322B2 (en) | 1991-07-15 | 1991-12-26 | Method of manufacturing probe for atomic force microscope |
Country Status (1)
| Country | Link |
|---|---|
| JP (1) | JP2622322B2 (en) |
Families Citing this family (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US7408366B2 (en) * | 2006-02-13 | 2008-08-05 | Georgia Tech Research Corporation | Probe tips and method of making same |
-
1991
- 1991-12-26 JP JP34451791A patent/JP2622322B2/en not_active Expired - Fee Related
Also Published As
| Publication number | Publication date |
|---|---|
| JPH05172561A (en) | 1993-07-09 |
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| Date | Code | Title | Description |
|---|---|---|---|
| LAPS | Cancellation because of no payment of annual fees |