JP3250724B2 - Manufacturing method of needle electrode - Google Patents
Manufacturing method of needle electrodeInfo
- Publication number
- JP3250724B2 JP3250724B2 JP15530897A JP15530897A JP3250724B2 JP 3250724 B2 JP3250724 B2 JP 3250724B2 JP 15530897 A JP15530897 A JP 15530897A JP 15530897 A JP15530897 A JP 15530897A JP 3250724 B2 JP3250724 B2 JP 3250724B2
- Authority
- JP
- Japan
- Prior art keywords
- needle
- electrode
- constricted portion
- manufacturing
- producing
- Prior art date
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- Cold Cathode And The Manufacture (AREA)
Description
【０００１】[0001]
【発明の属する技術分野】本発明は、電子顕微鏡、測長
機、電子線露光機、電子線テスター等に用いられる電子
線放射陰極や、マスク・リペアー、イオン注入装置、半
導体デバイス断面分析装置、透過電子顕微鏡用薄膜作成
装置等の集束イオンビーム（ＦＩＢ）源に用いられるイ
オン源等に適用される針状電極の製造方法に関する。BACKGROUND OF THE INVENTION 1. Field of the Invention The present invention relates to an electron beam emitting cathode used for an electron microscope, a length measuring machine, an electron beam exposure machine, an electron beam tester, etc., a mask repair, an ion implanter, a semiconductor device cross-sectional analyzer, The present invention relates to a method of manufacturing a needle-shaped electrode applied to an ion source used for a focused ion beam (FIB) source such as a thin film forming apparatus for a transmission electron microscope.
【０００２】[0002]
【従来の技術】電子顕微鏡をはじめとする電子線利用機
器の高精度化、高効率化のために、より高輝度の電子線
が必要とされ、ポイント・フィラメントをはじめとする
熱電子放射陰極或いはショットキー放射陰極などの様々
な電子放射陰極が検討されている。2. Description of the Related Art In order to increase the accuracy and efficiency of electron beam-based devices such as electron microscopes, higher-luminance electron beams are required. Various electron emission cathodes such as a Schottky emission cathode are being studied.
【０００３】例えば、高輝度電子源としてタングステン
の単結晶の細線を電解研磨により切り放して尖鋭端を電
子放射面とした冷電界陰極が高分解能電子顕微鏡の電子
源として広く用いられているし、また、タングステン単
結晶のチップの表面にＺｒＯ層を被覆して（１００）面
の仕事関数を約４．５ｅＶから約２．８ｅＶまで低下さ
せたＺｒＯ／Ｗ熱電界放射陰極が近年注目されている。[0003] For example, a cold field cathode having a sharp electron emission surface obtained by cutting a thin line of a single crystal of tungsten by electropolishing as a high-brightness electron source is widely used as an electron source for a high-resolution electron microscope. In recent years, a ZrO / W thermal field emission cathode in which the work function of the (100) plane is reduced from about 4.5 eV to about 2.8 eV by coating a surface of a tungsten single crystal chip with a ZrO layer has been attracting attention.
【０００４】何れの電子放射陰極においても放射電流密
度は、Ｆｏｗｌｅｒ−Ｎｏｒｄｈｅｉｍの式やＳｃｈｏ
ｔｔｋｙの式から判るように、陰極の先端部の仕事関数
と電界強度分布により決まる。電界強度分布は陰極と陽
極間に印加された電圧と、特に陰極の先端形状に強く依
存しており、電子放射陰極の特性を支配する重要な因子
の一つである。The emission current density of any of the electron emission cathodes is determined by Fowler-Nordheim equation or Scho
As can be seen from the equation of ttky, it is determined by the work function and the electric field intensity distribution at the tip of the cathode. The electric field intensity distribution strongly depends on the voltage applied between the cathode and the anode, and particularly on the shape of the tip of the cathode, and is one of the important factors governing the characteristics of the electron emission cathode.
【０００５】電子放射陰極の先端形状に関して、例え
ば、前述したＺｒＯ／Ｗ熱電界放射陰極においては、曲
率半径を１μｍ以上に大きくするときに放射電流のエネ
ルギー幅が低減されること、或いは安定性が向上するこ
とが知られている（Ｊ．Ｖａｃ．Ｓｃｉ．Ｔｅｃｈｎｏ
ｌ．，１６（６）１９７９，１７０４−１７０８、Ｊ．
Ａｐｐｌｉｄ Ｐｈｙｓｉｃｓ．，４６，５（１９７
５）２０２９−２０５０参照）。Regarding the tip shape of the electron emission cathode, for example, in the above-mentioned ZrO / W thermal field emission cathode, when the radius of curvature is increased to 1 μm or more, the energy width of the emission current is reduced or the stability is reduced. Is known to be improved (J. Vac. Sci. Techno).
l. , 16 (6) 1979, 1704-1708;
Applied Physics. , 46, 5 (197
5) 2029-2050).
【０００６】又、特開平７−１０５８３４号公報には、
エネルギー幅が低く、エミッションが安定な熱電界放射
陰極を得るために、従来公知の熱電界放射陰極を放電す
る方法を開示している。また、従来からの電界放射陰極
を２８００Ｋ程度に加熱処理する方法を試みたが、円錐
半角が４０度以上と大きくなり実用的でないことをも開
示している。更に、大きな曲率半径を有し、しかも円錐
半角の小さな先端形状を有する熱電界放射陰極は、従来
の電解研磨法のみでは対応できないことをも示唆してい
る。Japanese Patent Application Laid-Open No. 7-105834 discloses that
In order to obtain a thermal field emission cathode having a low energy width and stable emission, a method of discharging a conventionally known thermal field emission cathode is disclosed. Further, although a conventional method of heat-treating the field emission cathode to about 2800 K has been tried, it also discloses that the half angle of the cone becomes as large as 40 degrees or more, which is not practical. Furthermore, it also suggests that a thermal field emission cathode having a large radius of curvature and a small tip shape having a half cone angle cannot be dealt with only by the conventional electropolishing method.
【０００７】実際、従来公知の電解研磨法では、曲率半
径が大きくなるに従い円錐半角も大きくなり、曲率半径
が０．６μｍ以下のときでさえ円錐半角を５度下に制御
すること、或いは曲率半径が０．６〜２．０μｍのとき
に円錐半角を１０度以下に制御することが困難であっ
た。In fact, in the conventional electropolishing method, as the radius of curvature increases, the half angle of the cone also increases. Even when the radius of curvature is 0.6 μm or less, the half angle of the cone is controlled to be 5 degrees lower. Was 0.6 to 2.0 μm, it was difficult to control the half cone angle to 10 degrees or less.
【０００８】本発明者らは、特開平８−３６９８１号公
報において、１．２〜１０μｍの大きな曲率半径と、円
錐全角が２５度以下の熱電界放射陰極において、エネル
ギー幅が０．５ｅＶ以下で、角電流密度が０．０２ｍＡ
／ｓｒ以上の電子線を変動率５％以下で安定して得られ
ること、更に、ドライエッチングする方法等を従来の電
解研磨法に組み合わせることで、前記熱電界放射陰極を
得ることができることを開示している。The present inventors have disclosed in Japanese Patent Application Laid-Open No. 8-36981 that a large radius of curvature of 1.2 to 10 μm and a thermal field emission cathode having a total cone angle of 25 ° or less have an energy width of 0.5 eV or less. , Angular current density is 0.02 mA
Discloses that an electron beam of at least / sr can be stably obtained with a variation rate of 5% or less, and that the thermal field emission cathode can be obtained by combining a dry etching method and the like with a conventional electrolytic polishing method. are doing.
【０００９】しかし、前記公知資料に開示された方法で
は、放電やドライエッチングという生産性の悪い工程を
採用し、しかも高価な専用の装置を必要とするので、安
価に所望の先端形状を有する、ことに先端曲率半径が
０．６μｍ以上で、円錐半角が１０度以下の先端形状を
有する電子放射陰極を得ることができないという問題を
抱えている。However, the method disclosed in the above-mentioned known document employs a process with low productivity such as electric discharge or dry etching, and requires an expensive dedicated apparatus. In particular, there is a problem that an electron emission cathode having a tip shape having a tip curvature radius of 0.6 μm or more and a conical half angle of 10 degrees or less cannot be obtained.
【００１０】一方、ＦＩＢも種々の半導体検査装置や半
導体プロセス装置に利用され、近年注目を浴びている
が、ことにガリウムをイオン種とした液体金属イオン源
がＦＩＢ用イオン源として広く普及している。On the other hand, FIB is also used in various semiconductor inspection devices and semiconductor processing devices, and has been receiving attention in recent years. In particular, a liquid metal ion source using gallium as an ion species has been widely used as an ion source for FIB. I have.
【００１１】液体金属イオン源は高融点金属の針状電極
を液体金属により濡らし、前記針状電極の尖鋭端に強電
界を印加して液体金属をイオン化する。針状電極の尖鋭
端では強電界によりテイラー・コーンと呼ばれる液体金
属の円錐状の突起が形成され、この先端部よりイオンが
放出される。テイラー・コーンの円錐角は全角で９７度
程度であるといわれ、針状電極の尖鋭端の円錐角を前記
のテーラー・コーンの円錐角に合わせて形成することが
重要であることが知られている。The liquid metal ion source wets a needle electrode of a high melting point metal with a liquid metal, and applies a strong electric field to a sharp end of the needle electrode to ionize the liquid metal. At the sharp end of the needle-like electrode, a conical protrusion of liquid metal called a Taylor cone is formed by a strong electric field, and ions are emitted from this tip. It is said that the cone angle of the Taylor cone is about 97 degrees in full angle, and it is known that it is important to form the cone angle of the sharp end of the needle electrode in accordance with the cone angle of the Taylor cone. I have.
【００１２】このため、尖鋭端の形成には、前述の電子
放射陰極の針状電極と同様に電解研磨法により形成され
るのが一般的であるが、電解研磨法以外に機械研磨によ
る加工法も用いられる。しかし、機械研磨による加工法
は、微細部分の加工であるために、特殊な治具を必要と
し、結果的にコストが高くなる問題があるし、電界研磨
法では容易にテーラー・コーンの円錐角に近い円錐角を
有する針状電極が安定して得られないという問題があ
る。For this reason, the sharp end is generally formed by an electrolytic polishing method as in the case of the above-mentioned needle electrode of the electron emission cathode. Is also used. However, the machining method using mechanical polishing requires a special jig due to the processing of minute parts, and as a result, there is a problem that the cost is high. In the electrolytic polishing method, the cone angle of the tailor cone is easily increased. There is a problem that a needle electrode having a cone angle close to the above cannot be stably obtained.
【００１３】即ち、電界研磨による針状電極の加工方法
としては、例えば「固体物理」第２巻第２号（１９６
６）第３３頁から第３８頁に開示されているが、従来の
方法では円錐半角と先端半径とが強い相関関係があり単
独に制御できない、特に先端半径が大きいときに円錐半
角を小さくすることが困難であるという問題がある。That is, as a method of processing a needle-shaped electrode by electric field polishing, for example, “Solid State Physics” Vol. 2 No. 2 (196)
6) Although disclosed on pages 33 to 38, the conventional method has a strong correlation between the half cone angle and the tip radius and cannot be controlled independently. Particularly, when the tip radius is large, the half cone angle is reduced. There is a problem that is difficult.
【００１４】[0014]
【発明が解決しようとする課題】本発明は上記の事情に
鑑みてなされたものであり、本発明者らが実験的に検討
し、電界研磨法において高融点金属の細線に予めくびれ
部を形成し、該くびれ部から切断する方法を採用すると
きに、所望の先端形状を有する針状電極を安定して、従
って安価に得ることができ、しかも前記針状電極を電子
放射陰極やイオン源に用いるに好適であるという知見を
得て、本発明に至ったものである。SUMMARY OF THE INVENTION The present invention has been made in view of the above circumstances, and has been experimentally studied by the present inventors to form a narrow portion in advance in a fine wire of a high melting point metal by an electropolishing method. When the method of cutting from the constricted portion is adopted, a needle-like electrode having a desired tip shape can be obtained stably and therefore at a low cost, and the needle-like electrode is used as an electron emission cathode or an ion source. The present inventors have found that they are suitable for use, and have arrived at the present invention.
【００１５】本発明の目的は、所望の先端形状を有する
針状電極を安価に安定して提供することにあり、またそ
の結果、電子顕微鏡、測長機、電子線露光機、電子線テ
スター等に用いられる電子線放射陰極や、マスク・リペ
アー、イオン注入装置、半導体デバイス断面分析装置、
透過電子顕微鏡用薄膜作成装置等の集束イオンビーム
（ＦＩＢ）源に用いられるイオン源等を安価に、安定し
て提供することにある。An object of the present invention is to provide a needle-shaped electrode having a desired tip shape stably at a low cost, and as a result, an electron microscope, a length measuring machine, an electron beam exposure machine, an electron beam tester, etc. Electron beam emitting cathodes used for masks, mask repairs, ion implanters, semiconductor device cross-sectional analyzers,
An object of the present invention is to provide an inexpensive and stable ion source used for a focused ion beam (FIB) source such as a thin film forming apparatus for a transmission electron microscope.
【００１６】加えて、本発明の目的は、大きな曲率半径
好ましくは１．５μｍ以上を有し、しかも円錐半角の小
さい好ましくは１０度以下の先端形状を有し、その結果
エネルギー幅が小さく、高角電流密度を有し、長期に渡
って安定な電子線特性を有する熱電界放射陰極を提供す
ることにある。In addition, an object of the present invention is to provide a tip having a large radius of curvature, preferably 1.5 μm or more, and a small half angle of a cone, preferably 10 degrees or less, so that the energy width is small and the high angle An object of the present invention is to provide a thermal field emission cathode having a current density and stable electron beam characteristics for a long period of time.
【００１７】[0017]
【課題を解決するための手段】本発明は、高融点金属の
細線にくびれ部を形成し、該くびれ部より切断する針状
電極の製造方法であって、前記くびれ部を高融点金属の
細線をその軸方向に往復動させながら電解研磨すること
で形成することを特徴とする針状電極の製造方法であ
る。SUMMARY OF THE INVENTION The present invention relates to a method of manufacturing a needle-like electrode in which a constricted portion is formed in a thin wire of a high melting point metal and cut from the constricted portion, wherein the constricted portion is formed of a thin line of a high melting point metal. Is formed by electropolishing while reciprocating in the axial direction of the electrode.
【００１８】本発明は、前記くびれ部を０．０１μｍ／
ｓｅｃ以上０．１μｍ／ｓｅｃ以下の初期速度で電解研
磨して形成することを特徴とする前記の針状電極の製造
方法である。また、本発明は、高融点金属の細線にくび
れ部を形成し、該くびれ部を加熱溶断することを特徴と
する針状電極の製造方法である。According to the present invention, the constricted portion is formed at 0.01 μm /
forming the needle electrode by electropolishing at an initial speed of not less than sec and not more than 0.1 μm / sec.
Is the way. Further, the present invention provides a method for forming a narrow wire of a high melting point metal.
A method of manufacturing a needle-shaped electrode, comprising forming a constricted portion and heating and fusing the constricted portion.
【００１９】本発明は、前記加熱溶断に際し、細線に通
電しジュール発熱によりくびれ部を加熱溶断すること、
好ましくは、細線の一端を液体金属に浸漬し該液体金属
を介して通電すること、更に好ましくは、液体金属がＧ
ａであることを特徴とする前記の針状電極の製造方法で
ある。The present invention is characterized in that, at the time of the heating and fusing, a narrow wire is heated and blown by Joule heat while energizing a thin wire;
Preferably, one end of the fine wire is immersed in a liquid metal and an electric current is passed through the liquid metal.
a. The method for producing a needle-like electrode described above, wherein
【００２０】本発明は、電解液として０．１規定以上
０．８規定以下の水酸化ナトリウム水溶液及び／又は水
酸化カリウム水溶液を用い、直流電解研磨することを特
徴とする前記の針状電極の製造方法であり、好ましく
は、前記直流電解研磨時の電解電流の低減率を測定し、
該低減率が所定値となった時に電解研磨を停止するこ
と、更に好ましくは、前記所定値が１０％以上であるこ
とを特徴とする前記の針状電極の製造方法である。The present invention is characterized in that a direct current electrolytic polishing is carried out by using an aqueous solution of sodium hydroxide and / or potassium hydroxide of 0.1N or more and 0.8N or less as an electrolytic solution. The manufacturing method, preferably, measuring the reduction rate of the electrolytic current during the DC electrolytic polishing,
The method of manufacturing a needle-shaped electrode according to the above, wherein the electropolishing is stopped when the reduction rate reaches a predetermined value, and more preferably, the predetermined value is 10% or more.
【００２１】本発明は、前記の高融点金属の細線がタン
グステン、モリブデン、タンタル、レニウムからなる群
から選ばれる少なくとも１種以上からなることを特徴と
する前記の針状電極の製造方法であり、好ましくは、高
融点金属の細線がタングステン又はモリブデンの単結晶
からなること、更に好ましくは、高融点金属の細線が＜
１００＞方位の単結晶であることを特徴とする前記の針
状電極の製造方法である。The present invention is the above-mentioned method for producing a needle-like electrode, wherein the fine wire of the refractory metal is at least one selected from the group consisting of tungsten, molybdenum, tantalum, and rhenium. Preferably, the fine wire of the high melting point metal is made of a single crystal of tungsten or molybdenum, and more preferably, the fine wire of the high melting point metal is <
The method for producing a needle-shaped electrode according to the above, wherein the single-crystal has a 100> orientation.
【００２２】更に、本発明は、前記の針状電極の製造方
法を経て得られる針状電極を、更に、真空中で熱処理し
て該針状電極の先端曲率半径を調整すること、或いは、
減圧下で酸素及び／又は水を導入しながら加熱すること
で気相エッチングして該針状電極の先端曲率半径を調整
することを特徴とする電界放射陰極用の針状電極の製造
方法である。Further, the present invention provides a method of manufacturing a needle-shaped electrode obtained by the above-described needle-shaped electrode, wherein the needle-shaped electrode is further heat-treated in a vacuum to adjust a tip radius of curvature of the needle-shaped electrode.
A method for producing a needle electrode for a field emission cathode, comprising adjusting the radius of curvature of the needle electrode by vapor phase etching by heating while introducing oxygen and / or water under reduced pressure. .
【００２３】[0023]
【発明の実施の形態】以下、本発明の針状電極の製造方
法について、電子放射陰極の場合を例に説明する。ま
ず、従来公知の電子放射陰極は、以下に示す（工程１）
〜（工程５）を経て製造される。BEST MODE FOR CARRYING OUT THE INVENTION Hereinafter, a method for producing a needle-shaped electrode according to the present invention will be described with reference to an electron emitting cathode as an example. First, a conventionally known electron emission cathode is shown below (Step 1).
To (Step 5).
【００２４】（工程１）碍子にロウ付けされた２本の金
属支柱の先端にＶ字型のタングステンフィラメントをス
ポット溶接により取り付ける。更に、Ｖ字型タングステ
ンフィラメントの頂点部に長さ３．０ｍｍ、直径約０．
１３ｍｍの＜１００＞方位のタングステン単結晶細線を
スポット溶接により取り付ける。(Step 1) A V-shaped tungsten filament is attached to the tips of two metal posts brazed to the insulator by spot welding. Further, the top of the V-shaped tungsten filament has a length of 3.0 mm and a diameter of about 0.3 mm.
A 13 mm <100> oriented tungsten single crystal fine wire is attached by spot welding.
【００２５】（工程２）リング状電極にＮａＯＨ水溶液
を張り前記タングステン単結晶細線の先端部を浸漬し、
電解研磨によりタングステン単結晶細線を研磨して前記
細線の一部を切り離し、先端が鋭利な針状電極を形成す
る。(Step 2) An aqueous solution of NaOH is applied to the ring-shaped electrode, and the tip of the tungsten single crystal fine wire is immersed.
A tungsten single crystal fine wire is polished by electrolytic polishing to cut off a part of the fine wire to form a needle-like electrode having a sharp tip.
【００２６】（工程３）前記タングステン単結晶細線の
タングステンフィラメントの頂点部から約０．２ｍｍの
位置に水素化ジルコニウムを有機溶剤中で粉砕しスラリ
ー状としたものを塗布する。(Step 3) Zirconium hydride is pulverized in an organic solvent to form a slurry at a position of about 0.2 mm from the apex of the tungsten filament of the tungsten single crystal thin wire.
【００２７】（工程４）超高真空装置中で３×１０-9Ｔ
ｏｒｒまで真空引きした後、金属支柱を介しタングステ
ンフィラメントに通電してタングステン単結晶細線を約
１８００Ｋまで加熱し、その後酸素を３×１０-6Ｔｏｒ
ｒまで導入して４８Ｈｒ維持する。この操作により水素
化ジルコニウムは熱分解、酸化されて、酸化ジルコニウ
ムからなるリザーバが形成される。(Step 4) 3 × 10 −9 T in an ultra-high vacuum apparatus
After evacuation to orr, the tungsten filament is heated to about 1800 K by energizing a tungsten filament through a metal support, and then oxygen is supplied to 3 × 10 −6 Torr.
and maintained for 48 hours. By this operation, the hydrogenated zirconium is thermally decomposed and oxidized to form a reservoir made of zirconium oxide.
【００２８】（工程５）碍子にサプレッサー電極を被
せ、サプレッサー電極の孔から針状電極を突き出し、引
き出し電極が対になっている電子銃に搭載し、超高真空
装置に設置する。５×１０-10Ｔｏｒｒまで真空引き
し、タングステンフィラメントに通電して針状電極を１
８００Ｋに加熱する。続いて、針状電極に、引き出し電
極に対して負の高圧（引き出し電圧）を印加し、電子放
射を開始する。引き出し電極を通過した軸上電流をモニ
ターし、電流が安定するまで電子放射を維持する。尚、
高圧印加、計測系に付いては第２図に示した通りであ
る。また、測定した軸上電流Ｉｐと立体角ωから軸上角
電流密度Ｉ’ｐ＝Ｉｐ／ωを算出する。(Step 5) A suppressor electrode is put on the insulator, a needle-like electrode is protruded from a hole of the suppressor electrode, mounted on an electron gun paired with an extraction electrode, and installed in an ultra-high vacuum device. Vacuum down to 5 × 10 −10 Torr, apply electricity to the tungsten filament and set the needle electrode to 1
Heat to 800K. Subsequently, a negative high voltage (extraction voltage) is applied to the needle electrode with respect to the extraction electrode, and electron emission is started. The on-axis current passing through the extraction electrode is monitored, and the electron emission is maintained until the current is stabilized. still,
The high voltage application and measurement system is as shown in FIG. The on-axis angular current density I′p = Ip / ω is calculated from the measured on-axis current Ip and the solid angle ω.
【００２９】これに対して、本発明においては、針状電
極の先端形状を制御するために、（工程２）に変えて、
以下に示す（工程Ａ）及び（工程Ｂ）、又は（工程Ａ）
及び（工程Ｃ）、或いは（工程２）を略し（工程４）と
（工程５）の間に（工程Ａ）及び（工程Ｃ）を経由する
ことを特徴としている。更に、本発明では、付加的な工
程として（工程Ｄ）を経由することを特徴とする。On the other hand, in the present invention, in order to control the shape of the tip of the needle electrode, instead of (step 2),
(Step A) and (Step B) shown below , or (Step A)
(Step C) or (Step 2) is omitted, and (Step A) and (Step C) are interposed between (Step 4) and (Step 5). Further, the present invention is characterized in that an additional step is performed via (step D).
【００３０】（工程Ａ）リング状電極にＮａＯＨ水溶液
を張り、タングステン単結晶細線を浸漬し、タングステ
ン細線を上下に移動させながら電解研磨することにより
タングステン細線を研磨してタングステン単結晶細線の
一部にくびれ部を形成する（図１参照）。ここで、本発
明でいうくびれ部とは、直径がＤ1 である細線の一部に
形成された直径がＤ2 の部分がＤ2 ＜Ｄ1 の関係を満足
する部分をいうが、Ｄ2 ≦０．８Ｄ1 の関係を満足する
ことが円錐半角の小さな針状電極が得易いので好まし
い。(Step A) A part of a tungsten single crystal thin wire is polished by applying an NaOH aqueous solution to the ring-shaped electrode, immersing the tungsten single crystal thin wire, and electropolishing while moving the tungsten thin wire up and down. A constriction is formed (see FIG. 1). Here, the constricted portion referred to in the present invention means a portion formed on a part of a fine wire having a diameter of D1 and having a diameter of D2 which satisfies the relationship of D2 <D1. Satisfying the relationship is preferable because it is easy to obtain a small needle-like electrode having a half cone angle.
【００３１】そして、前記（工程Ａ）を経た後、次に示
す本発明者らが見いだした特定の条件下で電解研磨する
（工程Ｂ）或いは（工程Ｃ）を経ることで、タングステ
ン単結晶細線の一部を切り離し、針状電極とする。After the above (Step A), electrolytic polishing (Step B) or (Step C) under the following specific conditions found by the present inventors provides a tungsten single crystal thin wire. Is cut off to form a needle electrode.
【００３２】（工程Ｂ）工程Ａと同様に、リング状電極
にＮａＯＨ水溶液を張り、タングステン単結晶細線を浸
漬し、タングステン単結晶細線を上下に移動させながら
電解研磨し、最終的に切断するが、このときの電解研磨
の初期速度を０．０１μｍ／ｓｅｃ以上０．１μｍ／ｓ
ｅｃ以下とすることが好ましい。０．０１μｍ／ｓｅｃ
未満では研磨して得られる針状電極の表面に結晶欠陥が
露われ電子放射特性が不良となることがあるし、０．１
μｍ／ｓｅｃを越えるときは研磨の制御性が良好でなく
なる。尚、電解研磨の速度（研磨速度ともいう）は、細
線を所定時間研磨し、研磨前後の細線の直径変化を研磨
に要した時間で除して求める。細線の直径は、例えば５
０倍の倍率の投影機上で測定する。(Step B) As in step A, an aqueous NaOH solution is applied to the ring-shaped electrode, a tungsten single crystal thin wire is immersed, and the tungsten single crystal thin wire is vertically polished while being electropolished, and finally cut. In this case, the initial rate of the electrolytic polishing is set to 0.01 μm / sec or more and 0.1 μm / s.
ec or less. 0.01 μm / sec
If it is less than 0.1, crystal defects may be exposed on the surface of the needle-shaped electrode obtained by polishing, resulting in poor electron emission characteristics.
If it exceeds μm / sec, the controllability of polishing becomes poor. The rate of electrolytic polishing (also referred to as a polishing rate) is determined by polishing a fine wire for a predetermined time and dividing the change in diameter of the fine wire before and after polishing by the time required for polishing. The diameter of the thin wire is, for example, 5
Measure on a 0x magnification projector.
【００３３】前記の（工程Ａ）及び（工程Ｂ）において
は、電解液に０．１〜０．８規定の水酸化ナトリウム水
溶液及び又は水酸化カリウム水溶液を用いて直流で電解
研磨することが好ましい。０．１規定未満では研磨して
得られる針状電極の表面に結晶欠陥が露われ電子放射特
性が不良となることがあるし、０．８規定を越えるとき
には研磨の制御性が悪くなる。更に、電解研磨時の電解
電流の変化率に着目すると、電解電流は次第に低下して
ゆくので、変化率（即ち、低減率）が所定値以上となっ
た時に電解研磨を停止することが（所望の先端形状をし
た針状電極を再現性良く得ることができるので）望まし
く、ことに低減率が１０％以上となった時に電解研磨を
停止するとき、好ましい。尚、電解研磨を強制的に停止
しない場合、電解研磨が進み所望の先端曲率と円錐半角
を有する針状電極が得られない。また、（工程Ａ）と
（工程Ｂ）とは、別工程として行うのは勿論、一連の操
作を行い一工程とすることも出来る。電解電流の変化率
は、例えば、電解電流測定にデジタル電流計を用い、積
分時間２．５ｍｓ、サンプリングインターバル２０ｍ
ｓ、１００ｓａｍｐｌｉｎｇした平均値で、概ね２秒間
の電流の移動平均を測定することができ、本発明におい
ても同様である。In the above-mentioned (Step A) and (Step B), it is preferable to perform electropolishing with a direct current using a 0.1 to 0.8 N aqueous solution of sodium hydroxide or potassium hydroxide as an electrolytic solution. . If it is less than 0.1 normal, crystal defects may be exposed on the surface of the needle-shaped electrode obtained by polishing, resulting in poor electron emission characteristics. If it exceeds 0.8 normal, the controllability of polishing is deteriorated. Further, focusing on the rate of change of the electrolytic current during electrolytic polishing, since the electrolytic current gradually decreases, it is necessary to stop the electrolytic polishing when the rate of change (that is, the reduction rate) exceeds a predetermined value (desired). This is preferable because it is possible to obtain a needle-like electrode having the above-mentioned tip shape with good reproducibility), particularly when stopping the electropolishing when the reduction rate becomes 10% or more. If the electropolishing is not forcibly stopped, the electropolishing proceeds and a needle electrode having a desired tip curvature and a half cone angle cannot be obtained. In addition, (Step A) and (Step B) can be performed as a single step by performing a series of operations as well as being performed as separate steps. The rate of change of the electrolytic current is determined by, for example, using a digital ammeter for electrolytic current measurement, integrating time of 2.5 ms, and sampling interval of 20 m.
The moving average of the current for approximately 2 seconds can be measured from the average value obtained by sampling s and 100 samples, which is the same in the present invention.
【００３４】また、本発明に於いては、前記（工程Ｂ）
に変えて以下説明する（工程Ｃ）を採用することができ
る。In the present invention, the (step B)
(Step C) described below can be adopted instead of the above.
【００３５】（工程Ｃ）本工程では、（工程Ａ）で形成
されたくびれ部を加熱し、溶断することで、（工程Ａ）
で形成されるくびれ部の半径とほぼ同じ大きさの先端曲
率半径を有する針状電極を形成する。例えば、真空装置
内で、タングステン単結晶細線の先端を金属ボート中の
液体金属に浸漬する。続いて５×１０-7Ｔｏｒｒまで真
空に減圧し、金属支柱を介してタングステンフィラメン
トを通電してタングステン単結晶細線のくびれ部近傍が
１８００Ｋになるまで昇温し、保持する。更に細線通電
用電源により液体金属を介してタングステン単結晶細線
に通電し、くびれ部のみを局所的に加熱して溶断するこ
とができる。また、前記液体金属としては、低温も液体
であり、真空条件下で蒸気圧の低いものが望ましく、例
えばＧａ、Ｈｇ、半田等を用いることができ、とりわけ
Ｇａは室温下で液体であり、しかも各種材料との反応性
が乏しいので取扱いが容易であるという理由で好まし
い。(Step C) In this step, the constricted portion formed in (Step A) is heated and melted to obtain (Step A)
To form a needle-shaped electrode having a tip radius of curvature substantially equal to the radius of the constricted portion formed by the above. For example, the tip of a tungsten single crystal thin wire is immersed in a liquid metal in a metal boat in a vacuum device. Subsequently, the pressure is reduced to a vacuum of 5 × 10 −7 Torr, the tungsten filament is energized through a metal support, and the temperature is raised and maintained until the vicinity of the constricted portion of the tungsten single crystal thin wire reaches 1800 K. Further, a thin single-crystal tungsten wire can be energized via a liquid metal by a thin-wire power supply, and only the narrow portion can be locally heated and melted. The liquid metal is also liquid at low temperatures and preferably has a low vapor pressure under vacuum conditions. For example, Ga, Hg, solder, or the like can be used. In particular, Ga is liquid at room temperature, and It is preferable because it has low reactivity with various materials and is easy to handle.
【００３６】（工程Ｃ）においては、くびれ部の存在す
る単結晶細線に通電することで該くびれ部を局所加熱
し、溶融切断することを上記に例示しているが、該くび
れ部をレーザー光、電子線、赤外線等を用いて局所加熱
し、溶融切断することもできるし、該くびれ部を有する
単結晶細線を高融点フィラメントに固定し、該フィラメ
ントを通電加熱することで前記単結晶細線のくびれ部を
含む全部又は一部を加熱し、くびれ部で溶融切断するこ
ともできる。更に、本発明の（工程Ｃ）を採用する場
合、本発明者らの検討によれば、（工程４）を（工程
Ａ）、（工程Ｃ）より前とすることが好ましい。（工程
４）を（工程Ｃ）よりも後回しにすると、（工程４）で
気相エッチング現象を呈することがあり、先端部がピラ
ミッド状になることがあるからである。In the step (C), the local heating of the constricted portion by applying a current to the single-crystal thin wire having the constricted portion and the melting and cutting of the constricted portion are exemplified above. Local heating using electron beams, infrared rays, etc., can also be melted and cut, or the single crystal thin wire having the constricted portion is fixed to a high melting point filament, and the filament is heated by energization to form the single crystal thin wire. It is also possible to heat all or a part including the constricted portion and melt-cut at the constricted portion. Furthermore, when the (step C) of the present invention is employed, it is preferable that (step 4) be before (step A) and (step C) according to the study of the present inventors. If (Step 4) is performed after (Step C), a gas phase etching phenomenon may be exhibited in (Step 4), and the tip may become a pyramid.
【００３７】本発明は、（工程Ａ）で所望寸法のくびれ
部を形成し、更に（工程Ｂ）又は（工程Ｃ）の操作によ
り前記くびれ部で切断することで、（工程Ａ）で形成さ
れるくびれ部の半径とほぼ同じ大きさの先端曲率半径を
有する針状電極を容易に、再現性良く形成できるという
特徴を有する。また、本発明の方法は、（工程Ａ）によ
って得られる針状電極の先端形状が殆ど定めることがで
きるという特徴を有しているが、（工程Ａ）と（工程
Ｂ）は電解研磨法であり、（工程Ｃ）は加熱溶融する方
法なので、細線が単結晶、多結晶に拘らず適用すること
ができるという特徴を有する。According to the present invention, a constricted portion having a desired size is formed in (Step A), and further cut in the constricted portion by the operation of (Step B) or (Step C) to form the constricted portion in (Step A). It is characterized in that a needle-shaped electrode having a tip radius of curvature substantially equal to the radius of the constricted portion can be easily formed with good reproducibility. Further, the method of the present invention has a feature that the tip shape of the needle-shaped electrode obtained by (Step A) can be almost determined, but (Step A) and (Step B) are formed by the electrolytic polishing method. In addition, since (Step C) is a method of melting by heating, it has a feature that the thin wire can be applied regardless of whether it is a single crystal or a polycrystal.
【００３８】本発明に適用される高融点金属の細線とし
ては、その用途上の制限から、高真空下で耐熱性のある
タングステン、モリブデン、タンタル、レニウム等の高
融点金属が好ましく、このうちタングステン、モリブデ
ン、タンタル、レニウムの１群から選ばれる少なくとも
１種以上からなるもので、直径０．１〜０．５ｍｍ程度
の細線が好ましい。As the fine wire of the refractory metal applied to the present invention, tungsten, molybdenum, tantalum, rhenium and other refractory metals which are heat-resistant under a high vacuum are preferable due to the limitation in use. , Molybdenum, tantalum, rhenium and at least one selected from the group consisting of fine wires having a diameter of about 0.1 to 0.5 mm are preferred.
【００３９】本発明においては、（工程Ａ）と（工程
Ｂ）、或いは（工程Ａ）と（工程Ｃ）を経由する方法を
基本とするが、更に（工程Ｄ）を経由することも可能で
あり、ことに得られる針状電極の先端形状を微細な程度
にまで制御しようとするときに有効である。[0039] In the present invention, (step A) and (step B), or (step A) and is the basic methods via (step C), it is also possible to through further (Step D) In particular, it is effective when trying to control the tip shape of the obtained needle-shaped electrode to a minute degree.
【００４０】（工程Ｄ）本工程は、上述した方法で得ら
れた針状電極の先端形状を更に詳細に制御する工程であ
る。本発明者らの検討によれば、前述の操作で得られた
針状電極を、真空中で熱処理することにより、該針状電
極の先端曲率半径を増大することができる。また、減圧
下で酸素及び／又は水を導入しながら加熱することで、
該針状電極の先端曲率半径を小さくする事ができる。上
述の二つの方法を適宜選択することで、上述した方法で
得られた針状電極の先端形状を更に詳細に制御すること
ができる。(Step D) This step is a step of controlling the tip shape of the needle-shaped electrode obtained by the above method in more detail. According to the study by the present inventors, the needle-shaped electrode obtained by the above-described operation can be heat-treated in a vacuum to increase the radius of curvature of the tip of the needle-shaped electrode. In addition, by heating while introducing oxygen and / or water under reduced pressure,
The radius of curvature of the tip of the needle electrode can be reduced. By appropriately selecting the above two methods, the tip shape of the needle electrode obtained by the above method can be controlled in more detail.
【００４１】以下、実施例に基づいて、本発明を更に詳
細に説明する。Hereinafter, the present invention will be described in more detail with reference to examples.
【００４２】[0042]
〔実施例１〜３、比較例１〜３〕実施例１〜３は、上述
した（工程１）、（工程３）、（工程４）、（工程
Ａ）、（工程Ｃ）、（工程５）を経由し、（工程Ａ）の
電解研磨条件を調整していろいろな曲率半径の針状電極
を有する熱電界放射陰極を作成したものである。一方、
比較例１〜３は、従来公知の（工程１）、（工程２）、
（工程３）、（工程４）、（工程５）を順次経て作成し
たものであり、工程２の電解研磨条件を調整していろい
ろな曲率半径の針状電極を有する熱電界放射陰極を作成
した。これらの熱電界放射陰極について、その先端形状
と電子放射特性を表１に纏めて示す。[Examples 1 to 3, Comparative Examples 1 to 3] Examples 1 to 3 correspond to (Step 1), (Step 3), (Step 4), (Step A), (Step C), and (Step 5) described above. ), The electropolishing conditions in (Step A) were adjusted to produce a thermal field emission cathode having needle electrodes having various radii of curvature. on the other hand,
Comparative Examples 1 to 3 are conventionally known (Step 1), (Step 2),
(Step 3), (Step 4), and (Step 5), which were sequentially formed. The electropolishing conditions in Step 2 were adjusted to prepare a thermal field emission cathode having needle electrodes having various radii of curvature. . Table 1 summarizes the tip shape and electron emission characteristics of these thermal field emission cathodes.
【００４３】[0043]
【表１】 [Table 1]
【００４４】本発明によれば、円錐半角を１０度以下に
抑えながら、曲率半径を２．０〜１００μｍ、とりわけ
２．０〜２０μｍの範囲で容易に制御できることが、表
１から明かである。It is clear from Table 1 that according to the present invention, the radius of curvature can be easily controlled in the range of 2.0 to 100 μm, particularly 2.0 to 20 μm, while keeping the conical half angle at 10 degrees or less.
【００４５】〔実施例４〜７、比較例４〕実施例４〜７
として、（工程１）、（工程Ａ）、（工程Ｂ）、（工程
３）、（工程４）、（工程５）を経由して熱電界放射陰
極を作成した。いずれの場合も（工程Ａ）と（工程Ｂ）
とを一連の操作とした。実施例４〜７については、（工
程Ａ）、従って（工程Ｂ）の電解液にそれぞれ０．２
５、０．５、０．７、１．０規定の水酸化ナトリウム水
溶液を用い、タングステン単結晶細線を正極として直流
で電解研磨した。また、タングステン単結晶細線は約１
５０μｍのストロークで上下し、印加電圧を６Ｖとし
た。更に、電解電流を測定し、電解電流の変化率が１０
％以上になったのを確認して研磨を終了した。[Examples 4 to 7, Comparative Example 4] Examples 4 to 7
As a result, a thermal field emission cathode was prepared through (Step 1), (Step A), (Step B), (Step 3), (Step 4) and (Step 5). In each case, (Step A) and (Step B)
And were a series of operations. For Examples 4 to 7, the electrolyte of (Step A), and thus (Step B),
Using 0.5, 0.7, 1.0 normal sodium hydroxide aqueous solution, direct current electrolytic polishing was performed using a tungsten single crystal thin wire as a positive electrode. The tungsten single crystal fine wire is about 1
It was moved up and down with a stroke of 50 μm, and the applied voltage was 6 V. Further, the electrolytic current was measured, and the rate of change of the electrolytic current was 10%.
%, The polishing was completed.
【００４６】前記熱電界放射陰極について、先端形状と
電子放射特性を調べ、更に、５０００時間電子放射を行
った後の先端曲率半径の変化率を調べた。また、比較の
例として、比較例１〜３と同一操作で得た熱電界放射陰
極について調べた。それらの結果を表２に記載する。With respect to the thermal field emission cathode, the tip shape and electron emission characteristics were examined, and further, the rate of change of the tip radius of curvature after 5000 hours of electron emission was examined. As a comparative example, a thermal field emission cathode obtained by the same operation as Comparative Examples 1 to 3 was examined. Table 2 shows the results.
【００４７】[0047]
【表２】 [Table 2]
【００４８】表２に示すように、本発明の方法で得られ
た電子放射陰極は５０００時間もの長期間にわたり動作
させても、曲率半径の変化が従来の製造方法による電子
放射陰極よりも小さく、良好である。As shown in Table 2, even when the electron emitting cathode obtained by the method of the present invention is operated for as long as 5000 hours, the change in the radius of curvature is smaller than that of the electron emitting cathode obtained by the conventional manufacturing method. Good.
【００４９】更に、上記実施例４〜７と、上記には記載
していない本発明に係る実験結果とから、電解液濃度と
初期研磨速度との関係を調べたところ、図３に示す関係
を得た。同様に、図４に、本発明の方法で得られる針状
電極の曲率半径と円錐半角の関係を示した。本発明の方
法により、円錐半角の小さいままに曲率半径の大きな針
状電極が得られること、ことに電解液が０．１〜０．８
規定の濃度とする時に、初期研磨速度が０．０１〜０．
１μｍ／ｓｅｃに制御され、円錐半角を１０度以下に維
持しながら曲率半径が２．０μｍ以下の針状電極を得る
ことができることが明かである。Further, the relationship between the electrolyte concentration and the initial polishing rate was examined from the above Examples 4 to 7 and the experimental results according to the present invention not described above. Obtained. Similarly, FIG. 4 shows the relationship between the radius of curvature of the needle electrode obtained by the method of the present invention and the half angle of a cone. According to the method of the present invention, it is possible to obtain a needle-like electrode having a large radius of curvature while keeping the half cone angle small.
When the concentration is specified, the initial polishing rate is from 0.01 to 0.1.
It is clear that a needle-shaped electrode controlled at 1 μm / sec and having a radius of curvature of 2.0 μm or less can be obtained while maintaining the half cone angle at 10 degrees or less.
【００５０】[0050]
【発明の効果】本発明によれば、従来得難かった、先端
曲率半径が０．６μｍ以上で、円錐半角が１０度以下の
先端形状の針状電極が、格別の装置を使うことなく得る
ことができるので、低エネルギー幅で長期に電子放射特
性が安定している熱電界放射陰極を安価に提供が出来、
産業上非常に有用である。According to the present invention, it is possible to obtain a needle-shaped electrode having a tip curvature radius of 0.6 μm or more and a conical half angle of 10 ° or less without using a special device, which was difficult to obtain conventionally. It is possible to provide inexpensively a thermal field emission cathode with low energy width and stable electron emission characteristics for a long time,
Very useful in industry.
【００５１】本発明の方法は、電解研磨や溶断という結
晶異方性の少ない操作に基づいて針状電極の先端形状を
制御しているので、多結晶体の細線から作られるイオン
源用の針状電極にも適用できる。In the method of the present invention, the shape of the tip of the needle electrode is controlled based on operations such as electropolishing and fusing, which have a small crystal anisotropy. The present invention can also be applied to a shape electrode.
【図１】 本発明のくびれ部を形成する電解研磨法の説
明図。FIG. 1 is an explanatory view of an electropolishing method for forming a constricted portion according to the present invention.
【図２】 本発明の実施例、比較例に係る熱電界放射陰
極の電子放射特性を測定する回路図。FIG. 2 is a circuit diagram for measuring electron emission characteristics of the thermal field emission cathodes according to the example of the present invention and the comparative example.
【図３】 本発明における電解液濃度と初期研磨速度と
の関係を示す図。FIG. 3 is a diagram showing a relationship between an electrolyte concentration and an initial polishing rate in the present invention.
【図４】 本発明になる針状電極の曲率半径と円錐半角
との関係を示す図。FIG. 4 is a diagram showing a relationship between a radius of curvature of a needle-shaped electrode according to the present invention and a half cone angle.
１１ タングステン単結晶細線 １２ リング状電極 １３ 電解液 ２１ 熱電界放射陰極 ２２ サプレッサー電極 ２３ 引き出し電極 ２４ フィラメント加熱用電源 ２５ 高圧発生電源 ２６ アパーチャー ２７ プローブ電流測定電極 ２８ プローブ電流測定用微少電流計 ２９ バイアス電源 DESCRIPTION OF SYMBOLS 11 Tungsten single crystal thin wire 12 Ring electrode 13 Electrolyte 21 Thermoelectric field emission cathode 22 Suppressor electrode 23 Leader electrode 24 Filament heating power supply 25 High voltage generation power supply 26 Aperture 27 Probe current measurement electrode 28 Microcurrent meter for probe current measurement 29 Bias power supply
Claims (14)
くびれ部より切断する針状電極の製造方法であって、前
記くびれ部を高融点金属の細線をその軸方向に往復動さ
せながら電解研磨することで形成することを特徴とする
針状電極の製造方法。1. A method of manufacturing a needle-shaped electrode in which a constricted portion is formed in a fine wire of a high melting point metal and cut from the constricted portion, wherein the constricted portion is reciprocated by moving a thin line of a high melting point metal in an axial direction thereof.
A method for producing a needle-like electrode, characterized in that the electrode is formed by electropolishing while performing polishing.
１μｍ／ｓｅｃ以下の初期速度で電解研磨して形成する
ことを特徴とする請求項１記載の針状電極の製造方法。2. The constricted portion has a thickness of 0.01 μm / sec or more.
2. The method according to claim 1, wherein the electrode is formed by electropolishing at an initial speed of 1 [mu] m / sec or less.
くびれ部を加熱溶断することを特徴とする針状電極の製
造方法。3. A method for producing a needle-shaped electrode, comprising forming a constricted portion in a fine wire of a high melting point metal and fusing the constricted portion by heating.
を加熱溶断することを特徴とする請求項３記載の針状電
極の製造方法。4. The method for producing a needle-shaped electrode according to claim 3, wherein a current is applied to the thin wire to heat and melt the constricted portion by Joule heat.
を介して通電することを特徴とする請求項４記載の針状
電極の製造方法。5. The method according to claim 4, wherein one end of the thin wire is immersed in a liquid metal, and a current is supplied through the liquid metal.
求項５記載の針状電極の製造方法。6. The method according to claim 5, wherein the liquid metal is Ga.
下の水酸化ナトリウム水溶液及び／又は水酸化カリウム
水溶液を用い、直流電解研磨することでくびれ部より切
断することを特徴とする請求項１又は請求項２記載の針
状電極の製造方法。7. A method according to claim 1, wherein an aqueous solution of sodium hydroxide and / or potassium hydroxide having a concentration of 0.1 N or more and 0.8 N or less is used as an electrolytic solution, and the constriction is cut off by DC electropolishing. The method for producing a needle-shaped electrode according to claim 1 or 2.
し、該低減率が所定値となった時に電解研磨を停止する
ことを特徴とする請求項７記載の針状電極の製造方法。8. A method for manufacturing a needle-shaped electrode according to claim 7, wherein a reduction rate of the electrolytic current during DC electrolytic polishing is measured, and when the reduction rate reaches a predetermined value, the electrolytic polishing is stopped. .
とする請求項８記載の針状電極の製造方法。9. The method according to claim 8, wherein the predetermined value is 10% or more.
ブデン、タンタル、レニウムからなる群から選ばれる少
なくとも１種以上からなることを特徴とする請求項１乃
至請求項９記載の針状電極の製造方法。10. The method for manufacturing a needle-shaped electrode according to claim 1, wherein the fine wire of the refractory metal is at least one selected from the group consisting of tungsten, molybdenum, tantalum and rhenium. .
リブデンの単結晶からなることを特徴とする請求項１０
記載の針状電極の製造方法。11. The fine wire of a high melting point metal is made of a single crystal of tungsten or molybdenum.
A method for producing the needle-like electrode according to the above.
結晶であることを特徴とする請求項１１記載の針状電極
の製造方法。12. The method for producing a needle-shaped electrode according to claim 11, wherein the fine wire of the refractory metal is a single crystal having a <100> orientation.
記載の針状電極の製造方法を経て得られる針状電極を、
更に、真空中で熱処理して該針状電極の先端曲率半径を
調整することを特徴とする電界放射陰極用の針状電極の
製造方法。13. The method according to claim 10, 11 or 12.
Needle-like electrode obtained through the method for manufacturing a needle-like electrode described,
Further, a method for producing a needle electrode for a field emission cathode, comprising adjusting the radius of curvature of the needle electrode by heat treatment in a vacuum.
記載の針状電極の製造方法を経て得られる針状電極を、
更に、減圧下で酸素及び／又は水を導入しながら加熱す
ることで気相エッチングして該針状電極の先端曲率半径
を調整することを特徴とする電界放射陰極用の針状電極
の製造方法。14. A method according to claim 10, wherein the method comprises the steps of:
Needle-like electrode obtained through the method for manufacturing a needle-like electrode described,
Further, a method of manufacturing a needle electrode for a field emission cathode, comprising adjusting the radius of curvature of the needle electrode by vapor phase etching by heating while introducing oxygen and / or water under reduced pressure. .
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| JP15530897A JP3250724B2 (en) | 1996-06-12 | 1997-06-12 | Manufacturing method of needle electrode |
Applications Claiming Priority (5)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| JP08151137 | 1996-06-12 | ||
| JP12059497 | 1997-05-12 | ||
| JP8-151137 | 1997-05-12 | ||
| JP9-120594 | 1997-05-12 | ||
| JP15530897A JP3250724B2 (en) | 1996-06-12 | 1997-06-12 | Manufacturing method of needle electrode |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| JPH1131453A JPH1131453A (en) | 1999-02-02 |
| JP3250724B2 true JP3250724B2 (en) | 2002-01-28 |
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ID=27314078
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|---|---|---|---|
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| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JP2003007195A (en) * | 2001-06-20 | 2003-01-10 | Denki Kagaku Kogyo Kk | Electron emission cathode and its manufacturing method |
| WO2010070837A1 (en) | 2008-12-16 | 2010-06-24 | 株式会社日立ハイテクノロジーズ | Electron beam device and electron beam application device using the same |
| JP2010238670A (en) * | 2010-06-11 | 2010-10-21 | Denki Kagaku Kogyo Kk | Manufacturing method of electron emission cathode |
| JP6014156B2 (en) | 2012-10-12 | 2016-10-25 | 株式会社日立ハイテクノロジーズ | Manufacturing method of electron source |
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- 1997-06-12 JP JP15530897A patent/JP3250724B2/en not_active Expired - Lifetime
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