JP3559818B2 - Manufacturing method of nano electron source - Google Patents
Manufacturing method of nano electron source Download PDFInfo
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- JP3559818B2 JP3559818B2 JP2000159335A JP2000159335A JP3559818B2 JP 3559818 B2 JP3559818 B2 JP 3559818B2 JP 2000159335 A JP2000159335 A JP 2000159335A JP 2000159335 A JP2000159335 A JP 2000159335A JP 3559818 B2 JP3559818 B2 JP 3559818B2
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Description
【0001】
【発明の属する技術分野】
本発明は、電子源上に吸着した分子と表面原子との結合を利用し、電子源に負の高電圧を印加することで、高温加熱なしに、0.1から数ナノメータの曲率半径をもつナノ突起を製造することを特徴とするナノ電子源の製造法に関する。
【0002】
【従来の技術】
数ナノメータ以下の曲率半径のナノ突起をもつ電界放出電子源は、下記の3つの優れた特徴をもっているため、新しい電子源として、プロジェクション電子顕微鏡等で使用されている。即ち、
(1)放出電流の変動が極端に少ない。原子数個で終端されたナノ突起構造は領域が狭いため、分子が吸着する確率が少なく、また、残留気体のイオン衝撃による形状変化の確率も下がり、放出電流は安定である。
(2)放出方向領域が±2度内に電子が収束するために、電子放出の効率が著しく向上し輝度が増加する。
(3)狭い領域から放出されるため、電子ビームの可干渉性が優れており電子線ホログラフィー等への応用が可能である。
【0003】
従来より、ナノ電子源を製造する方法は、フランス リオン大学のBinh教授らによって開発されている(文献 Vu.Thien Binh,V.Semet,N.Garcia,Ultramicroscopy 58(1995)307−317.)。図3に従来技術としてのナノ電子源の製造法を模式的に示す。図3で1は数十ナノメートルの曲率半径をもつ金属針先端である。2は製造されたナノ突起で、3は高感度イオン検出器(マイクロチャンネル・プレート)である。6はナノ突起より電界蒸発した表面原子である。
【0004】
従来技術では図3に示すように、非常に高い温度(タングステンの場合には1500〜2000℃)に清浄な金属針先端1を加熱し、この金属針に正の高電圧を印加して、表面原子の拡散を誘起し、先端に集める。このため、特別の加熱装置を必要とする。更に、ナノ突起2の完成時の瞬間に、高電圧・高温度を緊急に、除かねば、せっかく製造したナノ突起2を破壊してしまう。このために、ナノ突起2の完成を検出する特別に感度の高い高感度イオン検出器3を必要としていた。
【0005】
図3に示すように、ナノ突起2が完成すると、ナノ突起2の先端に高電界が集中し、先端の原子が電界によってイオン化し蒸発する。つまり、電界蒸発と呼ばれる現象がおこる。この蒸発した1個のイオンを検出してナノ突起2の完成を確認する。このため、高価な検出器(マイクロチャンネルトロン)を使用する。さらに、ナノ突起2の完成瞬間は事前予告なしに、突然、蒸発原子が発生するため、電圧と温度を的確に除く瞬間を捕らえるためには、特殊な技術が要求されていた。
【0006】
【発明が解決しようとする課題】
本発明の目的は、加熱の必要がなく、マイクロチャンネルプレート等の特別な検出器を必要とせず、容易な操作によって、ナノ突起を電子源表面上に再現性よく製造することができるナノ電子源の製造法を提供することにある。
【0007】
【課題を解決するための手段】
上記目的を達成するための本発明の構成は以下に示す通りである。即ち、本発明は、
数十〜数百ナノメータの曲率半径をもつ電界放出電子源先端(1)をタングステンで形成する第1の工程と、
前記電界放出電子源先端(1)に残留分子(5)を吸着させて、吸着させた前記残留分子(5)の作用により前記電界放出電子源先端(1)の表面原子を移動しやすくする第2の工程と、
さらに、前記電界放出電子源先端(1)の表面に負の高電圧を印加して、数ナノメータの曲率半径をもつナノ突起(2)を加熱することなしに形成する第3の工程とからなるナノ電子源の製造法としての構成を有する。
【0008】
【発明の実施の形態】
本発明の特徴は、従来技術と大きく異なり、(1)加熱の必要がない、(2)マイクロチャンネルプレート等の特別な検出器を必要としない、(3)容易な操作によって、ナノ突起を電子源表面上に再現性よく製造する、ナノ電子源の製造法である。このナノ電子源の製造法により、ナノ電子源の適用できる対象が著しく増加する。
【0009】
図1に本発明のナノ電子源の製造法を模式的に示す。図1において、1は数十ナノメートルの曲率半径をもつ金属針先端である。2は製造されたナノ突起で、4は螢光板であり、5は先端付近に吸着した分子である。7はナノ突起2より放出した電子ビームである。
【0010】
本発明のナノ電子源の製造法は、図1に示すように、従来技術とは異なり、残留気体等の吸着によって汚した表面を使用する。この吸着原子や分子を適当に選ぶことによって、表面原子は著しく動きやすくなり、室温でも表面原子が移動する。
【0011】
次に、従来技術とは異なり、高い負の電圧を印加して電界放出電流をとると、表面原子は電子源先端の電界の集中した部分に引きよせられ、ナノ突起が形成され始める。一度突起が形成されると、その先端にはさらに電界が集中し、また原子が集まり、最終的には原子1個、または、数個で終端されたナノ突起ができる。
【0012】
本発明のナノ電子源の製造法では、突起形成過程の始まりは、放出電流の増加によってわかるので、完成時が的確にわかる。また、多くの放出電流を観測しているので、従来技術のような高感度の検出器を必要としない。つまり、ナノ突起形成過程での電界集中が起こり、同じ電圧で観測すると放出流が3桁近く増加し、放射方向が電子源の真下の2度程度内の限られた方向に集中するようになるため、この何れかを検出すれば、ナノ突起の形成は検出可能である。
【0013】
従来技術では1個のイオン化した原子を検出するのに対して、本発明のナノ電子源の製造法では、1億個の電子を検出するため、ナノ突起形成の検出の信頼性も著しく向上し、再現性も大幅に改善する。
【0014】
【実施例】
〈111〉結晶軸に向いたタングステンの単結晶線の一端を電界研磨法で100nmの曲率半径の鋭い針に加工する。この先端を10−8Torrの内で2000℃のフラッシュ加熱や電界蒸発によって、清浄にする。この清浄表面の曲率半径は電界イオン顕微鏡および電界電子放出顕微鏡にて確認した。このようにして準備したタングステン金属針が、多くの電子顕微鏡で使用されている電界放射電子源である。この電子源を10−7Torrの真空中にほぼ半日放置するとチップ表面には、主な残留気体である水素やCO(一酸化炭素)が吸着し汚れた表面となる。
【0015】
単原子層の厚さ分子の吸着した電子源のタングステン針に負のバイアス電圧を印加して、電圧を2−3kVまで増加させると電子が放出される。そして電流が10−8A以上になると、放出パターンの中心方向の放出電流が、急激に増大し始め、放出ビームのパターンは中心のみに集中する。増加が3桁近く増加したときに高電圧を遮断するとナノ突起が形成された。つまりタングステンの〈111〉方向に収束した電子ビームが放出される。このナノ電子源を電界イオン顕微鏡で観測するとタングステンと思われる1〜数個の原子で終端したナノ突起構造が通常の電子源表面に形成されていることがわかる。
【0016】
このナノ突起の形成により、電流変動が極端に少なくなり、輝度が増加した。図2は、本発明のナノ電子源の製造法により製造したナノ突端構造をもつナノ電子源からの放出電流の時間変化を示す。同じ放出電流である清浄なタングステン金属針(ナノ突起のない)からの放出電流は時間とともに減少するのに対して、ナノ突起からの電流は一定であり安定している優れた特性を示していることがわかる。
【0017】
【発明の効果】
本発明のナノ電子源の製造法によれば、清浄な金属針先端を加熱するための特別の加熱装置を必要とすることはなく、またナノ突起の完成を検出する特別に感度の高い高感度イオン検出器も必要とすることはなく、電圧と温度を的確に除く瞬間を捕らえるための特殊な技能も要求されることはない。
【0018】
本発明のナノ電子源の製造法によれば、電子源上に吸着した分子と表面原子との結合を利用し、電子源に負の高電圧を印加することで、高温加熱なしに0.1から数ナノメータの曲率半径をもつナノ突起を電子源表面上に再現性よく製造することができる。
【0019】
従来技術では1個のイオン化した原子を検出するのに対して、本発明のナノ電子源の製造法によれば、1億個の電子を検出するため、信頼性、および再現性も著しく向上する。
【0020】
本発明のナノ電子源の製造法により製造されたナノ突端構造をもつナノ電子源からの放出電流は時間変動が極端に少なくなり、輝度も増加し、安定である。
【図面の簡単な説明】
【図1】本発明のナノ電子源の製造法の模式図
【図2】本発明のナノ電子源の製造法により製造したナノ突端構造をもつナノ電子源からの放出電流の時間変化(ナノ突起のない通常の電子源との比較)
【図3】従来のナノ電子源の製造法の模式図
【符号の説明】
1 金属針先端
2 ナノ突起
3 高感度イオン検出器
4 螢光板
5 吸着分子
6(ナノ突起より電界蒸発した)表面原子
7 電子ビーム[0001]
TECHNICAL FIELD OF THE INVENTION
The present invention utilizes a bond between molecules adsorbed on an electron source and surface atoms, and has a radius of curvature of 0.1 to several nanometers without high-temperature heating by applying a high negative voltage to the electron source. The present invention relates to a method for producing a nano electron source, which comprises producing nano projections.
[0002]
[Prior art]
A field emission electron source having a nanoprojection having a radius of curvature of several nanometers or less has the following three excellent features, and is therefore used as a new electron source in a projection electron microscope and the like. That is,
(1) Fluctuation in emission current is extremely small. Since the nanoprojection structure terminated by several atoms has a small area, the probability of molecules being adsorbed is small, the probability of shape change due to ion bombardment of residual gas is also reduced, and emission current is stable.
(2) Since the electrons converge in the emission direction region within ± 2 degrees, the efficiency of electron emission is significantly improved, and the luminance is increased.
(3) Since the electron beam is emitted from a narrow region, the coherence of the electron beam is excellent, so that it can be applied to electron beam holography and the like.
[0003]
Conventionally, a method for producing a nanoelectron source has been developed by Professor Binh of the University of Lion in France (Documents: Vu. Thien Binh, V. Semet, N. Garcia, Ultramicroscopy 58 (1995) 307-317.). FIG. 3 schematically shows a conventional method for manufacturing a nano electron source. In FIG. 3,
[0004]
In the prior art, as shown in FIG. 3, a clean
[0005]
As shown in FIG. 3, when the
[0006]
[Problems to be solved by the invention]
An object of the present invention is to provide a nano-electron source capable of producing nano-projections on the surface of an electron source with a simple operation without the need for heating, a special detector such as a micro-channel plate, etc. It is to provide a manufacturing method of.
[0007]
[Means for Solving the Problems]
The configuration of the present invention for achieving the above object is as follows. That is, the present invention
A first step of forming a field emission electron source tip (1) having a radius of curvature of tens to hundreds of nanometers from tungsten ;
The remaining molecules (5) are adsorbed to the field emission electron source tip (1), and the surface atoms of the field emission electron source tip (1) are easily moved by the action of the adsorbed residual molecules (5). Two steps,
And a third step of applying a high negative voltage to the surface of the field emission electron source tip (1) to form without heating the nano projections (2) having a radius of curvature of several nanometers. It has a configuration as a method of manufacturing a nano electron source.
[0008]
BEST MODE FOR CARRYING OUT THE INVENTION
The features of the present invention are significantly different from those of the prior art, (1) no heating is required, (2) no special detector such as a microchannel plate is required, and (3) the nano-projections can be formed by an easy operation. This is a method for producing a nano electron source, which is produced on the source surface with good reproducibility. This method of manufacturing a nanoelectron source significantly increases the applications of the nanoelectron source.
[0009]
FIG. 1 schematically shows a method for producing a nanoelectron source according to the present invention. In FIG. 1,
[0010]
As shown in FIG. 1, the method for manufacturing a nano electron source of the present invention uses a surface contaminated by adsorption of a residual gas or the like, unlike the prior art. By appropriately selecting the adsorbed atoms and molecules, the surface atoms become remarkably mobile, and the surface atoms move even at room temperature.
[0011]
Next, unlike the prior art, when a high negative voltage is applied to obtain a field emission current, the surface atoms are attracted to the concentrated portion of the electric field at the tip of the electron source, and nanoprojections begin to form. Once the protrusions are formed, the electric field is further concentrated on the tips, and atoms are gathered, and finally, nanoprotrusions terminated with one or several atoms are formed.
[0012]
In the method for producing a nanoelectron source according to the present invention, the start of the projection formation process can be determined by an increase in the emission current, so that the completion time can be accurately determined. Further, since a large amount of emission current is observed, a highly sensitive detector unlike the related art is not required. In other words, electric field concentration occurs during the nanoprojection formation process, and when observed at the same voltage, the emission current increases by almost three orders of magnitude, and the emission direction is concentrated in a limited direction within about 2 degrees just below the electron source. Therefore, if any of these is detected, the formation of the nano-projections can be detected.
[0013]
While the conventional technology detects one ionized atom, the nanoelectron source manufacturing method of the present invention detects 100 million electrons, so that the reliability of the detection of nanoprojection formation is significantly improved. , And reproducibility is greatly improved.
[0014]
【Example】
<111> One end of a tungsten single crystal line oriented to the crystal axis is formed into a sharp needle having a radius of curvature of 100 nm by an electric field polishing method. This tip is cleaned by flash heating at 2000 ° C. or electric field evaporation within 10 −8 Torr. The radius of curvature of this clean surface was confirmed with a field ion microscope and a field electron emission microscope. The tungsten metal needle prepared in this manner is a field emission electron source used in many electron microscopes. If this electron source is left for about half a day in a vacuum of 10 −7 Torr, the surface of the chip becomes dirty due to adsorption of hydrogen and CO (carbon monoxide), which are main residual gases.
[0015]
When a negative bias voltage is applied to the tungsten needle of the electron source to which the molecules of the thickness of the monoatomic layer are adsorbed and the voltage is increased to 2-3 kV, electrons are emitted. When the current becomes 10 −8 A or more, the emission current in the center direction of the emission pattern starts to increase sharply, and the emission beam pattern is concentrated only at the center. Cutting off the high voltage when the increase increased by nearly three orders of magnitude formed nanoprojections. That is, an electron beam converged in the <111> direction of tungsten is emitted. Observation of this nano-electron source with a field ion microscope reveals that a nano-projection structure terminated by one or several atoms, which is considered to be tungsten, is formed on the surface of a normal electron source.
[0016]
Due to the formation of the nano projections, the current fluctuation was extremely reduced, and the luminance was increased. FIG. 2 shows a time change of an emission current from a nanoelectron source having a nanotip structure manufactured by the method for manufacturing a nanoelectron source of the present invention. The emission current from a clean tungsten metal needle (without nanoprotrusions) of the same emission current decreases with time, whereas the current from nanoprotrusions shows a constant and stable superior property. You can see that.
[0017]
【The invention's effect】
According to the method for manufacturing a nano electron source of the present invention, a special heating device for heating the tip of a clean metal needle is not required, and a special high sensitivity and high sensitivity for detecting the completion of the nano protrusion is provided. There is no need for an ion detector, and no special skills are required to capture the moment when voltage and temperature are properly removed.
[0018]
According to the method for producing a nanoelectron source of the present invention, by utilizing a bond between a molecule adsorbed on the electron source and a surface atom and applying a high negative voltage to the electron source, 0.1 mm without high-temperature heating. Can produce nanoprotrusions having a radius of curvature of several nanometers on the surface of the electron source with good reproducibility.
[0019]
According to the method of manufacturing a nano-electron source of the present invention, 100 million electrons are detected, whereas reliability and reproducibility are significantly improved. .
[0020]
The emission current from the nano-electron source having the nano-tip structure manufactured by the method for manufacturing a nano-electron source of the present invention has extremely small time fluctuation, increases the luminance, and is stable.
[Brief description of the drawings]
FIG. 1 is a schematic view of a method for manufacturing a nano electron source according to the present invention. FIG. 2 is a time change of an emission current from a nano electron source having a nano-tip structure manufactured by the method for manufacturing a nano electron source according to the present invention. Comparison with a normal electron source without
FIG. 3 is a schematic view of a conventional method for manufacturing a nano electron source.
DESCRIPTION OF
Claims (1)
前記電界放出電子源先端に残留分子を吸着させて、吸着させた前記残留分子の作用により前記電界放出電子源先端の表面原子を移動しやすくする第2の工程と、
さらに、前記電界放出電子源先端の表面に負の高電圧を印加して、数ナノメータの曲率半径をもつナノ突起を加熱することなしに形成する第3の工程とからなるナノ電子源の製造法。A first step of forming the tip of a field emission electron source having a radius of curvature of tens to hundreds of nanometers with tungsten ;
A second step of adsorbing residual molecules at the tip of the field emission electron source and easily moving surface atoms of the tip of the field emission electron source by the action of the adsorbed residual molecules;
A third step of applying a high negative voltage to the surface of the tip of the field emission electron source to form without heating a nano projection having a radius of curvature of several nanometers. .
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| JP2000159335A JP3559818B2 (en) | 2000-05-30 | 2000-05-30 | Manufacturing method of nano electron source |
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|---|---|---|---|
| JP2000159335A JP3559818B2 (en) | 2000-05-30 | 2000-05-30 | Manufacturing method of nano electron source |
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| JP3559818B2 true JP3559818B2 (en) | 2004-09-02 |
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| JP5063715B2 (en) * | 2010-02-04 | 2012-10-31 | 株式会社日立ハイテクノロジーズ | Electron source, electron gun, electron microscope apparatus and electron beam drawing apparatus using the same |
| JP6028277B2 (en) * | 2012-07-30 | 2016-11-16 | 国立研究開発法人物質・材料研究機構 | Metal boride field emitter fabrication method |
| CN113777122A (en) * | 2021-08-31 | 2021-12-10 | 中国科学院西安光学精密机械研究所 | A Parallel Electron Beam Detection System Based on Nano Electron Source |
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