JPH0959099A - Processing of layer substance material - Google Patents
Processing of layer substance materialInfo
- Publication number
- JPH0959099A JPH0959099A JP7216413A JP21641395A JPH0959099A JP H0959099 A JPH0959099 A JP H0959099A JP 7216413 A JP7216413 A JP 7216413A JP 21641395 A JP21641395 A JP 21641395A JP H0959099 A JPH0959099 A JP H0959099A
- Authority
- JP
- Japan
- Prior art keywords
- probe
- deposit
- substance
- processing
- scanning
- 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.)
- Granted
Links
Landscapes
- Inorganic Compounds Of Heavy Metals (AREA)
- Crystals, And After-Treatments Of Crystals (AREA)
- Superconductor Devices And Manufacturing Methods Thereof (AREA)
- Containers, Films, And Cooling For Superconductive Devices (AREA)
- Superconductors And Manufacturing Methods Therefor (AREA)
Abstract
Description
【０００１】[0001]
【発明の属する技術分野】本発明は、層状物質材料の加
工方法の改良に関するものである。さらに詳しくいえ
ば、本発明は、走査型トンネル顕微鏡を用いて層状物質
材料を加工するに際し、材料表面の劣化及び走査型トン
ネル顕微鏡探針の損傷をもたらすことなく、層状物質材
料の表面に効率よく微細加工を施す方法に関するもので
ある。TECHNICAL FIELD The present invention relates to an improvement in a method for processing a layered material. More specifically, the present invention efficiently processes the layered material material on the surface of the layered material material without causing deterioration of the material surface and damage of the scanning tunneling microscope probe when processing the layered material material using the scanning tunneling microscope. The present invention relates to a method for performing fine processing.
【０００２】[0002]
【従来の技術】超伝導体は温度が下がると電気抵抗が減
少し、ある有限の温度（臨界温度）で電気抵抗がゼロと
なる物質であるが、近年、このような性質を利用した超
伝導材料の応用研究が積極的になされており、例えば、
電磁石のコイルやジョセフソン素子などの電子デバイス
への利用がはかられている。2. Description of the Related Art A superconductor is a substance whose electric resistance decreases as the temperature lowers and becomes zero at a certain finite temperature (critical temperature). Applied research on materials is being actively conducted.
It is used for electronic devices such as coils of electromagnets and Josephson devices.
【０００３】ところで、超伝導材料を実用に供するに
は、できるだけ高い臨界温度を有するものが有利であ
り、このため、各種金属・合金系材料や酸化物材料など
が提案されているが、これらの中で、酸化物超伝導材料
は、金属・合金系超伝導材料よりも、臨界温度がはるか
に高いことから、実用性あるものとして注目されてい
る。In order to put the superconducting material into practical use, it is advantageous to use a material having a critical temperature as high as possible. Therefore, various metal / alloy-based materials and oxide materials have been proposed. Among them, the oxide superconducting material has attracted attention as a practical material because its critical temperature is much higher than that of the metal / alloy superconducting material.
【０００４】このような酸化物超伝導材料の実用化に際
しては、これを加工する必要があるが、この加工方法の
１つとして、走査型トンネル顕微鏡を用いる方法が知ら
れている。この走査型トンネル顕微鏡を用いて、酸化物
超伝導材料を加工する方法としては、これまで（１）探
針を加工すべき表面に機械的に当てて加工する機械的加
工（ミリング）法、（２）探針からの電子ビームにより
材料を変質させる電子ビームダメージ法、（３）高バイ
アス電圧、高トンネル電流による局所的な発熱で材料を
蒸発させる蒸発法、（４）二酸化炭素及び水分の存在す
る雰囲気中において、探針走査下の部位で化学反応を起
こして、エッチングする電気化学エッチング法、（５）
バイアス電圧及びトンネル電流により酸素を移動させ材
質を変質させる酸素の電気的移動法、（６）探針と材料
表面間に閾値以上のパルス及び連続的な電圧を加えるこ
とにより、表面原子を蒸発あるいは昇華させる電界蒸発
法、などが報告されている。In order to put such an oxide superconducting material into practical use, it is necessary to process it. As one of the processing methods, a method using a scanning tunneling microscope is known. As a method for processing an oxide superconducting material by using this scanning tunneling microscope, (1) a mechanical processing (milling) method in which a probe is mechanically applied to the surface to be processed, 2) Electron beam damage method that modifies the material by the electron beam from the probe, (3) Evaporation method that evaporates the material by local heat generation due to high bias voltage and high tunnel current, (4) Presence of carbon dioxide and water Electrochemical etching method in which a chemical reaction is caused in a portion under scanning of a probe in an atmosphere to perform etching to etch (5)
An electric transfer method of oxygen that changes oxygen by moving oxygen by bias voltage and tunnel current, (6) by applying a pulse and a continuous voltage above a threshold value between the probe and the surface of the material to evaporate surface atoms or A field evaporation method for sublimation has been reported.
【０００５】これらの加工方法のうち、数十ナノメート
ル以下のスケールでの微細加工が可能な方法は、前記
（１）の機械的加工法、（４）の電気化学エッチング法
及び（６）の電界蒸発法である。しかしながら、前記
（１）の機械的加工法は、探針を直接材料表面に当てる
ために、探針自体が損傷するのを免れないし、（４）の
電気化学エッチング法は、材料全体を水分を含む雰囲気
中に保持するため、材料表面が劣化しやすいという欠点
がある。また、（６）の電界蒸発法は、加工度の制御が
むずかしく、再現性の点で問題がある。Among these processing methods, the methods capable of fine processing on the scale of several tens of nanometers or less are the mechanical processing method of (1), the electrochemical etching method of (4) and the method of (6). It is a field evaporation method. However, the mechanical processing method of (1) above inevitably damages the probe itself because the probe directly contacts the surface of the material, and the electrochemical etching method of (4) keeps the entire material wet. Since it is held in an atmosphere containing it, there is a drawback that the material surface is likely to deteriorate. Further, in the field evaporation method (6), it is difficult to control the working degree and there is a problem in reproducibility.
【０００６】一方、前記の走査型トンネル顕微鏡を用い
る方法以外の酸化物超伝導材料を微細加工する方法とし
ては、集束イオンビームを用いる方法が知られており、
例えば（１）集束イオンビームを超伝導薄膜に打ち込ん
だのち、臭素を含むエタノール溶液により、照射部を増
幅エッチングする、（２）集束イオンビームを基板（例
えば酸化マグネシウム基板）に線状に打ち込んで、その
部位にダメージを与えたのち、超伝導薄膜を成長させ、
ダメージを与えた箇所を含む両側でジョセフソン接合を
形成させる、などの技術が報告されている。しかしなが
ら、このような集束イオンビームを用いる方法において
は、集束イオンビームの径が５０ｎｍ程度であるため、
数十ナノメートル以下の微細加工ができないという欠点
がある。On the other hand, a method using a focused ion beam is known as a method for finely processing an oxide superconducting material other than the method using the scanning tunneling microscope,
For example, (1) after implanting a focused ion beam into a superconducting thin film, the irradiation part is amplified and etched with an ethanol solution containing bromine. (2) A focused ion beam is linearly implanted into a substrate (eg, magnesium oxide substrate). , After damaging that part, grow a superconducting thin film,
Techniques such as forming Josephson junctions on both sides including the damaged portion have been reported. However, in the method using such a focused ion beam, since the diameter of the focused ion beam is about 50 nm,
There is a drawback that fine processing of several tens of nanometers or less cannot be performed.
【０００７】[0007]
【発明が解決しようとする課題】本発明は、このような
従来技術がもつ欠点を克服し、走査型トンネル顕微鏡を
用いて酸化物超伝導材料のような層状物質材料を加工す
るに際し、材料表面の劣化及び走査型トンネル顕微鏡探
針の損傷をもたらすことなく、層状物質材料の表面に、
幅が数十ナノメートル以下で、かつ深さが数ナノメート
ル程度の微細加工を効率よく施す方法を提供することを
目的としてなされたものである。SUMMARY OF THE INVENTION The present invention overcomes the above-mentioned drawbacks of the prior art, and when processing a layered material such as an oxide superconducting material using a scanning tunneling microscope, the material surface is On the surface of the layered material without degrading and damaging the scanning tunneling microscope probe,
The object of the present invention is to provide a method for efficiently performing fine processing with a width of several tens of nanometers or less and a depth of several nanometers.
【０００８】[0008]
【課題を解決するための手段】本発明者らは、前記目的
を達成するために鋭意研究を重ねた結果、堆積用物質を
付着させた探針を走査して、加工すべき層状物質材料表
面上の所定部位に該堆積用物質を堆積し、該表面の層状
物質材料の一部を堆積物に付着させたのち、探針を走査
してこの堆積物を取り除くことにより、その目的を達成
しうることを見出し、この知見に基づいて本発明を完成
するに至った。Means for Solving the Problems As a result of intensive studies to achieve the above-mentioned object, the present inventors have found that a probe having a deposition substance attached thereto is scanned and the surface of a layered substance material to be processed is scanned. The object is achieved by depositing the depositing substance on a predetermined portion above and adhering a part of the layered substance material on the surface to the deposit, and then scanning the probe to remove the deposit. Based on this finding, the present invention has been completed.
【０００９】すなわち、本発明は、探針を備えた走査型
トンネル顕微鏡を用いて、層状物質材料の表面を加工す
るに当り、堆積用物質を付着させた探針を走査して、加
工すべき材料表面上の所定部位に該堆積用物質を堆積
し、該表面の層状物質材料の一部を堆積物に付着させた
のち、探針を走査してこの堆積物を取り除くことを特徴
とする層状物質材料の加工方法を提供するものである。That is, according to the present invention, when a surface of a layered substance material is processed by using a scanning tunnel microscope equipped with a probe, the probe to which a deposition substance is attached should be scanned and processed. A layered structure characterized in that the depositing substance is deposited at a predetermined site on a material surface, a part of the layered substance material on the surface is attached to the deposit, and then the probe is scanned to remove the deposit. A method of processing a material is provided.
【００１０】ここで層状物質材料とは、酸化物超伝導材
料のほか、Ｋ2ＮｉＦ4構造、Ｓｒ3Ｔｉ2Ｏ7構造、Ｂｉ4
Ｔｉ3Ｏ12構造を含む層状ペロブスカイト型の化合物の
中で電気伝導性を有するものや、遷移金属ダイカルコゲ
ナイド、ハロゲン化金属、グラファイトなどの層状構造
を有し、物理的な力により表面部分が剥離可能な物質か
ら成る材料を意味する。The layered material here means an oxide superconducting material, a K 2 NiF 4 structure, a Sr 3 Ti 2 O 7 structure, and a Bi 4 material.
A layered perovskite-type compound containing a Ti 3 O 12 structure that has electrical conductivity, a layered structure of transition metal dichalcogenide, metal halide, graphite, etc., and the surface part is peeled off by physical force. A material composed of possible substances.
【００１１】また、本発明によれば加工すべき材料表面
上の所定部位において、この材料表面と堆積用物質を付
着させた探針との間に、走査型トンネル顕微鏡像を得る
際に設定されるバイアス電圧よりもプラス側又はマイナ
ス側に高い電圧をパルス的又は連続的に印加して、該堆
積用物質を堆積させ、次いで、走査型トンネル顕微鏡像
を得る際に設定されるバイアス電圧及びトンネル電流値
と同じバイアス電圧及びトンネル電流値、又はそれより
低いバイアス電圧及び高いトンネル電流値にて走査を繰
り返して、堆積物を取り除くことにより層状物質材料を
加工することができる。Further, according to the present invention, at a predetermined portion on the surface of the material to be processed, it is set when a scanning tunneling microscope image is obtained between the material surface and the probe to which the deposition substance is attached. The bias voltage and the tunnel which are set when a scanning tunneling microscope image is obtained by applying a voltage higher or more positively than the bias voltage in a pulsed or continuous manner to deposit the deposition material. The layered material can be processed by repeating the scan at the same bias voltage and tunnel current value as the current value, or at a lower bias voltage and higher tunnel current value to remove the deposit.
【００１２】[0012]
【発明の実施の形態】本発明方法において用いられる層
状物質材料の種類については特に制限はなく、従来公知
のもの、例えばランタン系、イットリウム系、ビスマス
系、タリウム系などの酸化物超伝導材料、いずれも使用
することができる。また、伝導性を有する層状ペロブス
カイト化合物、遷移金属ダイカルコゲナイド、ハロゲン
化金属、グラファイトなどから成る層状物質材料も用い
ることができる。The type of the layered material used in the method of the present invention is not particularly limited, and conventionally known materials such as lanthanum-based, yttrium-based, bismuth-based, and thallium-based oxide superconducting materials, Either can be used. Further, a layered material material composed of a conductive layered perovskite compound, a transition metal dichalcogenide, a metal halide, graphite, or the like can also be used.
【００１３】本発明方法においては、探針を備えた走査
型トンネル顕微鏡を用いて、層状物質材料を加工する
が、該探針として、堆積用物質を付着させたものが用い
られる。探針の材質としては例えばイリジウム含有量が
１０〜２０重量％の白金−イリジウム合金、白金、タン
グステン、金などが挙げられる。また、探針の先端は、
電界研磨処理などを施し、曲率半径が２０〜１００ｎｍ
程度の形状にしておくのが望ましい。In the method of the present invention, a layered substance material is processed by using a scanning tunneling microscope equipped with a probe, and the probe to which a deposition substance is attached is used as the probe. Examples of the material of the probe include a platinum-iridium alloy having an iridium content of 10 to 20% by weight, platinum, tungsten, gold and the like. Also, the tip of the probe is
The radius of curvature is 20 to 100 nm after being subjected to electropolishing
It is desirable to keep the shape.
【００１４】この探針に付着させる堆積用物質として
は、例えば、炭化水素化合物、水、加工すべき層状物質
材料の構成元素又はその化合物が用いられる。これらの
堆積用物質は単独で用いてもよいし、２種以上組み合せ
て用いてもよい。炭化水素化合物や水を探針に付着させ
る方法としては、例えば炭化水素化合物や水を含む雰囲
気中に探針を放置しておく方法、炭化水素化合物や水を
含む雰囲気中に放置した金属板の表面を、走査型トンネ
ル顕微鏡像を得る条件で走査して付着させる方法、ある
いは真空中、炭化水素化合物や水を含む雰囲気下で探針
に電子線を照射して付着させる方法などを用いることが
できる。As the deposition substance attached to the probe, for example, a hydrocarbon compound, water, a constituent element of the layered material to be processed or its compound is used. These depositing substances may be used alone or in combination of two or more kinds. As a method of attaching the hydrocarbon compound or water to the probe, for example, a method of leaving the probe in an atmosphere containing a hydrocarbon compound or water, or a method of using a metal plate left in an atmosphere containing a hydrocarbon compound or water It is possible to use a method of scanning and adhering the surface under the condition of obtaining a scanning tunneling microscope image, or a method of irradiating the probe with an electron beam in an atmosphere containing a hydrocarbon compound and water in vacuum to adhere the surface. it can.
【００１５】また、層状物質材料の構成元素やその化合
物を探針に付着させる方法としては、例えば酸化物超伝
導材料の表面を、走査型トンネル顕微鏡像を得る条件で
走査する方法、あるいは蒸着法などを用いることができ
る。As a method of adhering the constituent elements of the layered material or its compound to the probe, for example, the surface of the oxide superconducting material is scanned under the condition of obtaining a scanning tunneling microscope image, or the vapor deposition method. Etc. can be used.
【００１６】本発明方法においては、まず、このように
して堆積用物質を付着させた探針を走査して、加工すべ
き層状物質材料表面上の部位に該堆積用物質を堆積させ
る。この堆積方法としては、例えば材料表面と堆積用物
質を付着させた探針との間に、走査型トンネル顕微鏡像
を得る際に設定されるバイアス電圧よりもプラス側又は
マイナス側に高い電圧をパルス的又は連続的に印加する
ことにより、材料表面上の加工すべき部位に堆積用物質
を堆積させる方法が、一般的に用いられる。この際、バ
イアス電圧は、探針に対して、例えば−２．５ボルトよ
りも大きくマイナス側に印加するか、あるいは＋３ボル
トよりも大きくプラス側に印加するのがよい。パルスの
印加時間は、通常数マイクロ秒ないし数十ミリ秒の範囲
で選ばれる。このようにして堆積された堆積物は、層状
物質材料の表面上に、通常数十ナノメートル以下の半径
をもった面積を有している。In the method of the present invention, first, the probe having the depositing substance thus attached is scanned to deposit the depositing substance at a site on the surface of the layered substance material to be processed. As this deposition method, for example, a voltage higher than the bias voltage set when obtaining a scanning tunneling microscope image is applied between the surface of the material and the probe to which the material for deposition is attached to the positive side or the negative side. A method of depositing a deposition substance on a surface of a material to be processed by applying the deposition material continuously or continuously is generally used. At this time, the bias voltage is preferably applied to the probe on the minus side by more than -2.5 volts or on the plus side by more than +3 volts. The pulse application time is usually selected in the range of several microseconds to several tens of milliseconds. The deposit thus deposited has an area on the surface of the layered material which usually has a radius of a few tens of nanometers or less.
【００１７】次に、前記堆積物を探針を走査して取り除
くが、この堆積物を取り除く方法としては、例えば走査
型トンネル顕微鏡像を得る際に設定されるバイアス電圧
及びトンネル電流値と同じバイアス電圧及びトンネル電
流値、又はそれより低いバイアス電圧及び高いトンネル
電流値にて走査を繰り返すことにより、該堆積物を取り
除く方法が、一般的に用いられる。この際、探針は材料
表面に十分近づいて走査されるので、この走査を繰り返
すと、探針が堆積物のある部分で、堆積物に微弱に機械
的に接触し、堆積物がその箇所から取り除かれる。この
堆積物は堆積された箇所の材料表面をはぎ取るようにし
て取り除かれるので、結果として堆積面積とほぼ同じ面
積で加工が施されることになる。Next, the deposit is removed by scanning with a probe. As a method for removing this deposit, for example, the same bias voltage and tunnel current value that are set when obtaining a scanning tunneling microscope image are used. A method of removing the deposit by repeating scanning at a voltage and a tunnel current value, or a bias voltage and a lower tunnel current value is generally used. At this time, the probe is scanned sufficiently close to the material surface, so if this scanning is repeated, the probe will weakly mechanically contact the deposit at the part where the deposit is present, and the deposit will be removed from that part. To be removed. This deposit is removed by stripping off the material surface at the deposited portion, and as a result, processing is performed in an area approximately the same as the deposition area.
【００１８】このようにして、材料表面の劣化及び走査
型トンネル顕微鏡探針の損傷をもたらすことなく、層状
物質材料の表面に幅が数十ナノメートル以下で、かつ深
さが数ナノメートル程度の微細加工が施される。In this manner, the width of the layered material is several tens of nanometers or less and the depth is about several nanometers without causing deterioration of the material surface and damage of the scanning tunneling microscope probe. Fine processing is applied.
【００１９】図１（ａ）ないし（ｄ）は本発明方法を実
施するための手順を示す説明図であって、まず、層状物
質材料１の表面の目的位置まで、堆積用物質３が付着し
た探針２を移動させる［（ａ）図］。次いで、電圧パル
ス印加により、材料１の表面に堆積用物質３を堆積させ
る［（ｂ）図］。次に探針を走査し、該探針と堆積物と
の機械的作用により、堆積物とそれに付着した超伝導材
料を除去する［（ｃ）図］。このようにして、ナノメー
トルスケールの微細加工４が、層状物質材料１の表面上
に施される（ｄ）。FIGS. 1 (a) to 1 (d) are explanatory views showing the procedure for carrying out the method of the present invention. First, the deposition substance 3 adheres to the target position on the surface of the layered substance material 1. The probe 2 is moved [Fig. (A)]. Then, the deposition substance 3 is deposited on the surface of the material 1 by applying a voltage pulse [FIG. (B)]. Next, the probe is scanned, and the deposit and the superconducting material adhering thereto are removed by the mechanical action of the probe and the deposit [Fig. (C)]. In this way, nanometer-scale microfabrication 4 is performed on the surface of the layered material 1 (d).
【００２０】[0020]
【発明の効果】本発明方法によると、走査型トンネル顕
微鏡を用いて層状物質材料を加工するに際し、材料表面
の劣化及び走査型トンネル顕微鏡探針の損傷をもたらす
ことなく、層状物質材料の表面に効率よく微細加工を施
すことができる。According to the method of the present invention, when a layered material is processed by using a scanning tunneling microscope, the surface of the layered material is not deteriorated and the surface of the layered material is damaged without causing deterioration of the material surface and damage of the scanning tunneling microscope probe. Fine processing can be performed efficiently.
【００２１】[0021]
【実施例】次に、本発明を実施例によりさらに詳細に説
明するが、本発明は、これらの例によって何ら限定され
るものではない。EXAMPLES Next, the present invention will be described in more detail with reference to examples, but the present invention is not limited to these examples.
【００２２】実施例 超高真空走査型トンネル顕微鏡を用いて、Ｂｉ2Ｓｒ2Ｃ
ａＣｕ2Ｏ8+x単結晶からなる酸化物超伝導材料の加工を
行った。 （１）探針への堆積用物質の付着処理 イリジウム含有量１５重量％の白金−イリジウム合金か
ら成る探針に、以下に示す方法により、炭化水素を付着
させた。すなわち、塩化カルシウムと塩酸を含む溶液中
で電界研摩法により作製した探針を１０日間大気中で保
管した後、真空中で電子線を照射しながら大気中に１０
日間保管してあったステンレス鋼板上を走査型トンネル
顕微鏡により１時間走査してＣ2〜Ｃ8炭化水素混合物を
付着させた。Example Using an ultra-high vacuum scanning tunneling microscope, Bi 2 Sr 2 C was used.
An oxide superconducting material made of aCu 2 O 8 + x single crystal was processed. (1) Adhesion treatment of deposition material to a probe Hydrocarbon was attached to a probe made of a platinum-iridium alloy having an iridium content of 15% by weight by the method described below. That is, a probe manufactured by the electric field polishing method in a solution containing calcium chloride and hydrochloric acid was stored in the atmosphere for 10 days, and then the probe was exposed to the electron beam in a vacuum and exposed to the atmosphere for 10 days.
Scans 1 hour on a stainless steel plate had been stored days with a scanning tunneling microscope was deposited C 2 -C 8 hydrocarbon mixture.
【００２３】（２）試料の準備 Ｂｉ2Ｓｒ2ＣａＣｕ2Ｏ8+x単結晶試料の裏面を、銀ペー
ストで試料ホルダーに接着したのち、この試料に粘着テ
ープを貼り付けた。次いで、これを試料準備用超高真空
チャンバーに導入したのち、チャンバー内の真空度を１
０-8Ｐａ台に保持し、試料に貼り付けた粘着テープを剥
がした。粘着テープの剥離は、超高真空中で動作するス
ティックを用いてテープの端をつかみ、試料からテープ
を引き離すように動作させることにより行った。これに
より、Ｂｉ2Ｓｒ2ＣａＣｕ2Ｏ8+x単結晶はへき開され、
清浄表面を得ることができた。(2) Preparation of Sample After the back surface of the Bi 2 Sr 2 CaCu 2 O 8 + x single crystal sample was adhered to the sample holder with silver paste, an adhesive tape was adhered to this sample. Then, after introducing this into an ultra-high vacuum chamber for sample preparation, the degree of vacuum in the chamber was set to 1
The pressure-sensitive adhesive tape stuck to the sample was peeled off by holding it on the 0-8 Pa level. Peeling of the adhesive tape was performed by grabbing the end of the tape with a stick operating in ultra-high vacuum and operating to pull the tape away from the sample. As a result, the Bi 2 Sr 2 CaCu 2 O 8 + x single crystal is cleaved,
A clean surface could be obtained.
【００２４】（３）走査型トンネル顕微鏡像の観察 このようにして、準備した清浄表面をもつ単結晶試料
を、超高真空走査型トンネル顕微鏡を有し、真空度が１
０-8Ｐａ台に保持された測定用チャンバーに移動させ、
該顕微鏡の試料ステージに取り付けた。なお、試料準備
用チャンバーから測定用チャンバーまでの移動中試料は
３×１０-8Ｐａの真空度に保持した。次に、試料表面の
走査型トンネル顕微鏡像を観察した。なお、観察条件
は、トンネル電圧を探針に対して試料側に１．２ボルト
印加したとき、トンネル電流が０．３ｎＡ流れるように
設定した。また、走査型トンネル顕微鏡像を観察してい
る間は、前記観察条件の電流値が常に一定に保たれるよ
うに、測定器でフィードバックをかけた。このフィード
バックは、探針を取り付けているピエゾ素子への印加電
圧を制御することにより、ピエゾ素子の伸縮を調整し、
これにより探針と試料表面の距離の微調整を行った。(3) Observation of Scanning Tunnel Microscope Image The thus prepared single crystal sample having a clean surface was provided with an ultrahigh vacuum scanning tunnel microscope and the degree of vacuum was 1.
Move to the measurement chamber held on the 0-8 Pa level,
It was attached to the sample stage of the microscope. The sample was kept moving from the sample preparation chamber to the measurement chamber at a vacuum degree of 3 × 10 −8 Pa. Next, a scanning tunneling microscope image of the sample surface was observed. The observation conditions were set so that a tunnel current of 0.3 nA would flow when a tunnel voltage of 1.2 V was applied to the sample side of the probe. Further, while observing the scanning tunneling microscope image, feedback was applied by a measuring instrument so that the current value under the above observation conditions was always kept constant. This feedback adjusts the expansion and contraction of the piezo element by controlling the voltage applied to the piezo element to which the probe is attached,
Thereby, the distance between the probe and the sample surface was finely adjusted.
【００２５】（４）試料表面の加工 測定器のディスプレイに表示された走査型トンネル顕微
鏡像を確認して、探針を画像の所定の点に移動させ、ト
ンネル電圧を１．２ボルトに保持したまま、トンネル電
流を新たに設定した電流値（例えば０．３ｎＡ）になる
ように調整した。なお、トンネル電流値を大きくすると
探針は試料表面に近づく。次いで、ピエゾ素子にかけて
いるフィードバックを遮断し、探針と試料表面間の距離
を一定に保持したのち、探針と試料表面間に４ボルトの
パルス電圧を５ミリ秒間印加した。図２に探針からの堆
積用物質の堆積が可能な条件を示す。図２において、横
軸にパルス電圧が、縦軸にパルス電圧を印加する前に設
定したトンネル電流値が示されており、斜線部分の領域
が堆積可能な条件を示している。次に、パルス電圧の印
加を終了すると同時に、フィードバック回路を回復し、
走査型トンネル顕微鏡像の観察条件であるトンネル電圧
及びトンネル電流値で試料表面を観察したところ、探針
に付着していた堆積用物質が、試料表面に堆積している
のが確認された。その後、この観察条件で観察走査を連
続して繰り返すことにより、堆積物を徐々に取り除い
た。堆積物が取り除かれた跡に、表面が凹に加工されて
いることが確認された。鮮明に凹が確認されたところで
走査を終了した。図３に、このようにして施された試料
表面の微細加工の形状をグラフで示す。横軸は微細加工
の両端Ａ，Ｂ間の距離を示し、縦軸は深さを示す。(4) Processing of sample surface Confirming the scanning tunneling microscope image displayed on the display of the measuring instrument, the probe was moved to a predetermined point on the image and the tunnel voltage was kept at 1.2 V. As it was, the tunnel current was adjusted to a newly set current value (for example, 0.3 nA). Note that when the tunnel current value is increased, the probe approaches the sample surface. Then, the feedback applied to the piezo element was cut off, the distance between the probe and the sample surface was kept constant, and then a pulse voltage of 4 V was applied between the probe and the sample surface for 5 milliseconds. FIG. 2 shows conditions under which the deposition material can be deposited from the probe. In FIG. 2, the horizontal axis shows the pulse voltage and the vertical axis shows the tunnel current value set before the pulse voltage is applied, and the shaded area shows the conditions under which deposition is possible. Next, at the same time as ending the application of the pulse voltage, the feedback circuit is recovered,
When the sample surface was observed at the tunnel voltage and tunnel current values, which are the observation conditions of the scanning tunneling microscope image, it was confirmed that the deposition material attached to the probe was deposited on the sample surface. Thereafter, the observation scan was continuously repeated under these observation conditions to gradually remove the deposit. It was confirmed that the surface was processed to be concave after the deposit was removed. The scanning was stopped when a sharp depression was confirmed. FIG. 3 is a graph showing the shape of the microfabrication of the sample surface thus obtained. The horizontal axis represents the distance between both ends A and B of the fine processing, and the vertical axis represents the depth.
【図１】 本発明方法を実施するための工程概略図。FIG. 1 is a process schematic diagram for carrying out the method of the present invention.
【図２】 本発明方法において、材料表面への堆積用物
質の堆積が可能な条件の１例を示す図。FIG. 2 is a diagram showing an example of conditions under which a deposition substance can be deposited on a material surface in the method of the present invention.
【図３】 本発明方法による微細加工の形状の１例を示
すグラフ。FIG. 3 is a graph showing an example of a finely processed shape according to the method of the present invention.
１ 酸化物超伝導材料 ２ 探針 ３ 堆積用物質 ４ 微細加工 1 oxide superconducting material 2 probe 3 deposition material 4 microfabrication
───────────────────────────────────────────────────── フロントページの続き (51)Int.Cl.6 識別記号 庁内整理番号 ＦＩ 技術表示箇所 Ｈ０１Ｌ 39/24 ＺＡＡ Ｈ０１Ｌ 39/24 ＺＡＡＦ (72)発明者 徳本 洋志 茨城県つくば市東１−１−４ 産業技術融 合領域研究所内 アトムテクノロジー研究 体─────────────────────────────────────────────────── ─── Continuation of the front page (51) Int.Cl. 6 Identification code Internal reference number FI Technical display location H01L 39/24 ZAA H01L 39/24 ZAAF (72) Inventor Hiroshi Tokumoto 1-1, East Tsukuba, Ibaraki Prefecture 4 Atom Technology Research Institute in the Institute for Industrial Technology Integration
Claims (4)
いて、層状物質材料の表面を加工するに当り、堆積用物
質を付着させた探針を走査して、加工すべき材料表面上
の所定部位に該堆積用物質を堆積し、該表面の層状物質
材料の一部を堆積物に付着させたのち探針を走査してこ
の堆積物を取り除くことを特徴とする層状物質材料の加
工方法。1. When a surface of a layered material is processed by using a scanning tunneling microscope equipped with a probe, the probe having a deposition substance attached thereto is scanned and the surface of the material to be processed is scanned. A method for processing a layered material, comprising depositing the depositing material on a predetermined site, adhering a part of the layered material on the surface to the deposit, and then scanning the probe to remove the deposit. .
て、この材料表面と堆積用物質を付着させた探針との間
に、走査型トンネル顕微鏡像を得る際に設定されるバイ
アス電圧よりもプラス側又はマイナス側に高い電圧をパ
ルス的又は連続的に印加して、該堆積用物質を堆積さ
せ、次いで、走査型トンネル顕微鏡像を得る際に設定さ
れるバイアス電圧及びトンネル電流値と同じバイアス電
圧及びトンネル電流値、又はそれより低いバイアス電圧
及び高いトンネル電流値にて走査を繰り返し、堆積物を
取り除くことを特徴とする請求項１記載の層状物質材料
の加工方法。2. A bias voltage set at the time of obtaining a scanning tunneling microscope image between a surface of a material to be processed and a probe having a deposition substance attached thereto at a predetermined portion on the surface of the material to be processed. A high voltage is applied to the positive side or the negative side in a pulsed or continuous manner to deposit the deposition material, and then the bias voltage and the bias that are the same as the tunnel current value set when obtaining the scanning tunneling microscope image. 2. The method for processing a layered material according to claim 1, wherein the deposit is removed by repeating scanning at a voltage and a tunnel current value, or a bias voltage and a lower tunnel current value lower than that.
すべき酸化物超伝導材料の構成元素又はその化合物の中
から選ばれた少なくとも１種である請求項１又は２記載
の層状物質材料の加工方法。3. The layered material according to claim 1, wherein the depositing substance is at least one selected from a hydrocarbon compound, water, a constituent element of an oxide superconducting material to be processed, or a compound thereof. Processing method.
積物と探針とが機械的な接触を繰り返す請求項１、２又
は３記載の層状物質材料の加工方法。4. The method for processing a layered material according to claim 1, 2 or 3, wherein the deposit and the probe repeat mechanical contact with each other during scanning when removing the deposit.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| JP21641395A JP3721440B2 (en) | 1995-08-24 | 1995-08-24 | Processing method for layered material |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| JP21641395A JP3721440B2 (en) | 1995-08-24 | 1995-08-24 | Processing method for layered material |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| JPH0959099A true JPH0959099A (en) | 1997-03-04 |
| JP3721440B2 JP3721440B2 (en) | 2005-11-30 |
Family
ID=16688178
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| JP21641395A Expired - Lifetime JP3721440B2 (en) | 1995-08-24 | 1995-08-24 | Processing method for layered material |
Country Status (1)
| Country | Link |
|---|---|
| JP (1) | JP3721440B2 (en) |
Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JP2011198824A (en) * | 2010-03-17 | 2011-10-06 | Yukio Watabe | Method of manufacturing hetero structure including metal oxide, and method of manufacturing the metal oxide |
| JP2013075356A (en) * | 2011-09-14 | 2013-04-25 | Yukio Watabe | Structure having heterojunction including metal oxide |
Citations (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JPS63109A (en) * | 1986-06-19 | 1988-01-05 | Nec Corp | Semiconductor and manufacture thereof |
| JPS6360196A (en) * | 1986-08-29 | 1988-03-16 | Nec Corp | Surface treatment |
| JPH02173278A (en) * | 1988-12-26 | 1990-07-04 | Hitachi Ltd | Method and device for fine processing |
| JPH03238744A (en) * | 1989-11-07 | 1991-10-24 | Internatl Business Mach Corp <Ibm> | Method and device for rearranging adsorptive atom |
| JPH04345047A (en) * | 1991-05-22 | 1992-12-01 | Jeol Ltd | Fine working method of material surface |
| JPH0551300A (en) * | 1991-08-26 | 1993-03-02 | Rikagaku Kenkyusho | Monoatomic deposition method |
-
1995
- 1995-08-24 JP JP21641395A patent/JP3721440B2/en not_active Expired - Lifetime
Patent Citations (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JPS63109A (en) * | 1986-06-19 | 1988-01-05 | Nec Corp | Semiconductor and manufacture thereof |
| JPS6360196A (en) * | 1986-08-29 | 1988-03-16 | Nec Corp | Surface treatment |
| JPH02173278A (en) * | 1988-12-26 | 1990-07-04 | Hitachi Ltd | Method and device for fine processing |
| JPH03238744A (en) * | 1989-11-07 | 1991-10-24 | Internatl Business Mach Corp <Ibm> | Method and device for rearranging adsorptive atom |
| JPH04345047A (en) * | 1991-05-22 | 1992-12-01 | Jeol Ltd | Fine working method of material surface |
| JPH0551300A (en) * | 1991-08-26 | 1993-03-02 | Rikagaku Kenkyusho | Monoatomic deposition method |
Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JP2011198824A (en) * | 2010-03-17 | 2011-10-06 | Yukio Watabe | Method of manufacturing hetero structure including metal oxide, and method of manufacturing the metal oxide |
| JP2013075356A (en) * | 2011-09-14 | 2013-04-25 | Yukio Watabe | Structure having heterojunction including metal oxide |
Also Published As
| Publication number | Publication date |
|---|---|
| JP3721440B2 (en) | 2005-11-30 |
Similar Documents
| Publication | Publication Date | Title |
|---|---|---|
| Iwami et al. | Preparation of silver tips for scanning tunneling microscopy imaging | |
| US5959957A (en) | Probe and a cantilever formed with same material | |
| Hendricks et al. | Imaging of the in situ deposition of lead on highly oriented pyrolytic graphite by scanning tunneling and atomic force microscopies | |
| Hernández-Saz et al. | A methodology for the fabrication by FIB of needle-shape specimens around sub-surface features at the nanometre scale | |
| US7223611B2 (en) | Fabrication of nanowires | |
| Coleman Jr et al. | On the mechanism of GaAs anodization | |
| JP3721440B2 (en) | Processing method for layered material | |
| Thomson et al. | Surface modification of YBa2Cu3O7-delta thin films using the scanning tunneling microscope: five methods | |
| Walls et al. | The preparation of field electron/field-ion emitters by ion etching | |
| DeRose et al. | Electrochemical deposition of nucleic acid polymers for scanning probe microscopy | |
| JP3563271B2 (en) | Method of producing probe for scanning probe microscope and apparatus therefor | |
| Fujita et al. | Nanostructure fabrication on silicon surfaces by atom transfer from a gold tip using an ultrahigh vacuum scanning tunneling microscope | |
| Hung et al. | Scanning probe nanolithography of conducting metal oxides | |
| Won-chul Moon et al. | Fabrication of nanopit arrays on Si (111) | |
| Owen et al. | Observation of the evolution of etch features on polycrystalline ZnO: Al thin-films | |
| Myhra et al. | Tip-induced nano-writing/machining of Si and DLC surfaces–“anodic” versus thermal oxidation? | |
| Roberts et al. | Controlled nanometre-scale line and symbol formation on graphite in air using a scanning tunnelling microscope | |
| Driesel | Micromachining using focused ion beams | |
| RU2197037C1 (en) | Method for producing metal-insulator-high- temperature-superconductor nanostructure | |
| Hyland et al. | Surface modification of thin film gold electrodes for improved in vivo performance | |
| Scott et al. | Scanning tunneling microscopy of platinum films on mica: evolution of topography and crystallinity during film growth | |
| Wu et al. | Surface electromigration of Au ultrathin film on MoS2 | |
| Gamo et al. | Amorphous-silicon-on-glass field emitter arrays | |
| Mühl et al. | Electro-oxidative lithography by STM as a proximity electrode of electrically conducting DLC | |
| Robinson | Scanning tunneling microscopy of lead dioxide |
Legal Events
| Date | Code | Title | Description |
|---|---|---|---|
| A977 | Report on retrieval |
Free format text: JAPANESE INTERMEDIATE CODE: A971007 Effective date: 20050217 |
|
| A131 | Notification of reasons for refusal |
Free format text: JAPANESE INTERMEDIATE CODE: A131 Effective date: 20050408 |
|
| A521 | Request for written amendment filed |
Free format text: JAPANESE INTERMEDIATE CODE: A523 Effective date: 20050606 |
|
| TRDD | Decision of grant or rejection written | ||
| A01 | Written decision to grant a patent or to grant a registration (utility model) |
Free format text: JAPANESE INTERMEDIATE CODE: A01 Effective date: 20050811 |
|
| A61 | First payment of annual fees (during grant procedure) |
Free format text: JAPANESE INTERMEDIATE CODE: A61 Effective date: 20050829 |
|
| R150 | Certificate of patent or registration of utility model |
Free format text: JAPANESE INTERMEDIATE CODE: R150 |
|
| S111 | Request for change of ownership or part of ownership |
Free format text: JAPANESE INTERMEDIATE CODE: R313118 |
|
| R350 | Written notification of registration of transfer |
Free format text: JAPANESE INTERMEDIATE CODE: R350 |
|
| FPAY | Renewal fee payment (event date is renewal date of database) |
Free format text: PAYMENT UNTIL: 20090922 Year of fee payment: 4 |
|
| FPAY | Renewal fee payment (event date is renewal date of database) |
Free format text: PAYMENT UNTIL: 20090922 Year of fee payment: 4 |
|
| FPAY | Renewal fee payment (event date is renewal date of database) |
Free format text: PAYMENT UNTIL: 20100922 Year of fee payment: 5 |
|
| FPAY | Renewal fee payment (event date is renewal date of database) |
Free format text: PAYMENT UNTIL: 20110922 Year of fee payment: 6 |
|
| FPAY | Renewal fee payment (event date is renewal date of database) |
Free format text: PAYMENT UNTIL: 20110922 Year of fee payment: 6 |
|
| FPAY | Renewal fee payment (event date is renewal date of database) |
Free format text: PAYMENT UNTIL: 20120922 Year of fee payment: 7 |
|
| FPAY | Renewal fee payment (event date is renewal date of database) |
Free format text: PAYMENT UNTIL: 20120922 Year of fee payment: 7 |
|
| FPAY | Renewal fee payment (event date is renewal date of database) |
Free format text: PAYMENT UNTIL: 20130922 Year of fee payment: 8 |
|
| FPAY | Renewal fee payment (event date is renewal date of database) |
Free format text: PAYMENT UNTIL: 20130922 Year of fee payment: 8 |
|
| S111 | Request for change of ownership or part of ownership |
Free format text: JAPANESE INTERMEDIATE CODE: R313117 |
|
| FPAY | Renewal fee payment (event date is renewal date of database) |
Free format text: PAYMENT UNTIL: 20130922 Year of fee payment: 8 |
|
| R350 | Written notification of registration of transfer |
Free format text: JAPANESE INTERMEDIATE CODE: R350 |
|
| R250 | Receipt of annual fees |
Free format text: JAPANESE INTERMEDIATE CODE: R250 |
|
| S111 | Request for change of ownership or part of ownership |
Free format text: JAPANESE INTERMEDIATE CODE: R313117 |
|
| R350 | Written notification of registration of transfer |
Free format text: JAPANESE INTERMEDIATE CODE: R350 |
|
| S533 | Written request for registration of change of name |
Free format text: JAPANESE INTERMEDIATE CODE: R313533 |
|
| R350 | Written notification of registration of transfer |
Free format text: JAPANESE INTERMEDIATE CODE: R350 |
|
| EXPY | Cancellation because of completion of term |