JPS6132326A - Formation of acicular body by electrolytic polishing - Google Patents
Formation of acicular body by electrolytic polishingInfo
- Publication number
- JPS6132326A JPS6132326A JP15348184A JP15348184A JPS6132326A JP S6132326 A JPS6132326 A JP S6132326A JP 15348184 A JP15348184 A JP 15348184A JP 15348184 A JP15348184 A JP 15348184A JP S6132326 A JPS6132326 A JP S6132326A
- Authority
- JP
- Japan
- Prior art keywords
- emitter
- time
- electrolytic polishing
- pulse voltage
- electrolytic
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
- Pending
Links
Classifications
-
- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01J—ELECTRIC DISCHARGE TUBES OR DISCHARGE LAMPS
- H01J9/00—Apparatus or processes specially adapted for the manufacture, installation, removal, maintenance of electric discharge tubes, discharge lamps, or parts thereof; Recovery of material from discharge tubes or lamps
- H01J9/02—Manufacture of electrodes or electrode systems
- H01J9/022—Manufacture of electrodes or electrode systems of cold cathodes
- H01J9/025—Manufacture of electrodes or electrode systems of cold cathodes of field emission cathodes
-
- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01J—ELECTRIC DISCHARGE TUBES OR DISCHARGE LAMPS
- H01J2237/00—Discharge tubes exposing object to beam, e.g. for analysis treatment, etching, imaging
- H01J2237/06—Sources
- H01J2237/08—Ion sources
- H01J2237/0802—Field ionization sources
- H01J2237/0807—Gas field ion sources [GFIS]
Abstract
Description
【発明の詳細な説明】
産業上の利用分野
本発明は電解研摩による針状体の形成方法に関するもの
であって、電界電離型気体イオン銃や電界イオン顕ｍｋ
Ｅｆｔ用のＷ製針状エミフターを形成するのに用い”
ζ最適なものである。DETAILED DESCRIPTION OF THE INVENTION Field of Industrial Application The present invention relates to a method for forming needle-shaped bodies by electrolytic polishing, and is applicable to field ionization type gas ion guns and field ion microscopes mk.
Used to form W needle-shaped emifter for Eft.
ζIt is the optimal one.
従来の技術
従来、この、ｆｉｉのＷ製針状エミッターは、通常電解
ｆσト摩法により形成されている。この電解研摩法は、
電解研摩すべきエミッターを陽極とすると共に対向電皓
を陰極としてアルカリ水溶液等の電解液中で電解を行う
ことによりエミッターを溶解させるものである。この電
解研摩法によれば、電解中にエミッターの先端に高電界
が作用するため、先端が比較的細い針状エミッターを得
ることが可能である。BACKGROUND OF THE INVENTION Conventionally, fii W needle-shaped emitters are usually formed by an electrolytic fσ polishing method. This electrolytic polishing method is
The emitter to be electrolytically polished is used as an anode and the opposite electrode is used as a cathode to dissolve the emitter by performing electrolysis in an electrolytic solution such as an alkaline aqueous solution. According to this electrolytic polishing method, a high electric field acts on the tip of the emitter during electrolysis, so it is possible to obtain a needle-like emitter with a relatively thin tip.
しかしながら、従来の電解研摩法では電解中の電解液の
濃度、特にエミッターの表面近傍における電解液の濃度
を適切に制御するのが難しく、このため先端形状が良好
でかつ先端が十分に細いエミッターを再現性良く形成す
ることが困難であった。However, with conventional electrolytic polishing methods, it is difficult to appropriately control the concentration of the electrolyte during electrolysis, especially the concentration of the electrolyte near the emitter surface. It was difficult to form with good reproducibility.
すなわち、従来の電解研摩法では、エミッターを電解液
中に浸漬した状態で連続的に直流電解を行うか、あるい
はエミッターを機械的または手動的に電解液中に出し入
れすることにより電解液の濃度を制御するようにしてい
た。しかしながら、前者の方法では、エミッターの表面
近傍において電解により発生するガスやエミッターから
の溶解成分等の濃度が電解の進行と共に高くなるため、
電解液の電気抵抗が増加すると共にエミッター表面への
電解液の供給が妨げられてしまい、また後・”Ｈの方法
では、電解の途中のエミノクー表面は著しく活性な状態
になっているためにエミッターを電解液中から空気中に
取り出すと同時に酸化されてしまうので、いずれの方法
によっても電解の円滑な進行が妨げられるのみならず、
エミッターの先端形状や先端の細さの再現性も著しく悪
いという欠点があった。In other words, in the conventional electrolytic polishing method, direct current electrolysis is performed continuously while the emitter is immersed in the electrolyte, or the concentration of the electrolyte is adjusted by mechanically or manually moving the emitter into and out of the electrolyte. I was trying to control it. However, in the former method, the concentration of gas generated by electrolysis near the surface of the emitter and dissolved components from the emitter increases as the electrolysis progresses.
As the electrical resistance of the electrolyte increases, the supply of the electrolyte to the emitter surface is obstructed, and in the second method, the emitter surface becomes extremely active during electrolysis, so the emitter Since it is oxidized as soon as it is taken out from the electrolyte into the air, both methods not only hinder the smooth progress of electrolysis, but
The problem was that the reproducibility of the shape and thinness of the emitter tip was extremely poor.
発明が解決しようとする問題点
本発明は、上述の問題にかんがみ、従来の電解研摩によ
る針状体の形成方法が有する上述のような欠点を是正し
た電解研摩による針状体の形成方法を提供することを目
的とする。Problems to be Solved by the Invention In view of the above-mentioned problems, the present invention provides a method for forming needle-like bodies by electrolytic polishing, which corrects the above-mentioned drawbacks of the conventional method for forming needle-like bodies by electrolytic polishing. The purpose is to
問題点を解決するための手段
本発明に係る電解研摩による針状体の形成方法は、直流
パルス電圧を用いしかもこの直流パルス電圧のオン時間
に対するオフ時間の比を１以上としている。Means for Solving the Problems The method of forming needle-shaped bodies by electrolytic polishing according to the present invention uses a DC pulse voltage and sets the ratio of the OFF time to the ON time of the DC pulse voltage to 1 or more.
作用
このようにすることによって、先端の曲率半径が極めて
小さくかつ先端形状が良好な針状体を再現性良く形成す
ることができる。By doing this, it is possible to form a needle-shaped body with an extremely small radius of curvature at the tip and a good tip shape with good reproducibility.
実施例
以下本発明に係る電解研摩による針状体の形成方法をＷ
製の針状エミッターの形成に適用した一実施例を図面を
参照しながら説明する。Examples Below, the method for forming needle-shaped bodies by electrolytic polishing according to the present invention will be described.
An example in which the present invention is applied to the formation of a needle-like emitter will be described with reference to the drawings.
第１図は本発明に係る電解研摩による針状体の形成方法
を実施するための電解研摩装置である。FIG. 1 shows an electrolytic polishing apparatus for carrying out the method of forming needle-shaped bodies by electrolytic polishing according to the present invention.
この第１図に示す電解研摩装置においては、石英製の電
解槽１内に電解液２ （例えば水酸化ナトリウムとアン
モニアとの混合溶液）が入れられている。この電解液２
中には、その一端がＷ製のリード線３を介して直流パル
ス電源４の子端子に接続されている、例えば径が２００
μｍのＷ ｋｇから成るエミッター５の他端が例えば５
＋ｓ＊程度浸漬され、さらにリード線３を介して直流
パルス電源４の一端子に接続されているＷ製の対向、電
極６が浸漬されている。なおリード線３とエミッター５
とは例えばスポット溶接により接続されている。In the electrolytic polishing apparatus shown in FIG. 1, an electrolytic solution 2 (for example, a mixed solution of sodium hydroxide and ammonia) is placed in an electrolytic bath 1 made of quartz. This electrolyte 2
Inside, one end is connected to the child terminal of the DC pulse power source 4 via the lead wire 3 made of W, for example, the diameter is 200 mm.
The other end of the emitter 5 consisting of W kg of μm is e.g.
The counter electrode 6 made of W and connected to one terminal of the DC pulse power source 4 via the lead wire 3 is further immersed. In addition, lead wire 3 and emitter 5
For example, they are connected by spot welding.
上述のように構成された電解研摩装置によりエミッター
５を電解研摩するには、まず直流パルス電源４によって
第２図に示すような直流パルス電圧を発生し、これをエ
ミッター５と対向電極６との間に印加する。なおパルス
条件としては、例えば印加電圧４■、周期５ｍ５ｅｃｓ
デユーテイ１０％（オン時間は９．５ ｍ５ｅｃ−、オ
フ時間は４．５ ｍ５ｅｃ）を用い、印加時間は２０ｓ
ｅｃとする。In order to electrolytically polish the emitter 5 using the electrolytic polishing apparatus configured as described above, first, a DC pulse voltage as shown in FIG. Apply in between. The pulse conditions include, for example, an applied voltage of 4 cm and a period of 5 m5 ecs.
The duty was 10% (on time: 9.5 m5ec-, off time: 4.5 m5ec), and the application time was 20 s.
Let it be ec.
上述の直流パルス電圧の印加によりエミッター５の電解
研摩が進行し、電解研摩終了後には第３図に示すような
先端がとがった針状のエミッター５が得られた。この得
られたエミッター５の先端を走査型電子顕微鏡により観
察した所、第４図に示すように先端の曲率半径は約５０
０Å以下と極めて小さく、また形状も極めて良好であっ
た。Electrolytic polishing of the emitter 5 progressed by applying the above-mentioned DC pulse voltage, and after the electrolytic polishing was completed, a needle-shaped emitter 5 with a pointed tip as shown in FIG. 3 was obtained. When the tip of the obtained emitter 5 was observed using a scanning electron microscope, the radius of curvature of the tip was approximately 50 as shown in FIG.
It was extremely small, less than 0 Å, and the shape was also extremely good.
また上述と同様な電解研摩を反復して行って再現性を調
べた所、エミッター５の先端の形状及び曲率半径は実質
的に一定であり、再現性が極めて良好であることが確認
された。Further, when the same electrolytic polishing as described above was repeated and the reproducibility was examined, it was confirmed that the shape and radius of curvature of the tip of the emitter 5 were substantially constant, and the reproducibility was extremely good.
なお上述のように再現性が極めて良好であるのは次のよ
うな理由による。すなわち、上述の実施例においては、
第２図に示す直流パルス電圧のオフ時間をオン時間に比
べて９倍長くしているため、このオフ時間中に電解研摩
により発生するガスやエミッター５からの溶解成分等が
電解液２中に拡散すると共に新たな電解液２がエミッタ
ー５の表面に供給される。このためエミッター５の表面
の近傍における電解液２の濃度が電解研摩中実質的に一
定となる。また従来のように電解研摩中にエミッター５
を空気中に取り出す必要がないので、エミッター５の表
面が酸化されることがない。The reason why the reproducibility is extremely good as described above is as follows. That is, in the above embodiment,
Since the off time of the DC pulse voltage shown in Fig. 2 is nine times longer than the on time, gas generated by electrolytic polishing and dissolved components from the emitter 5 enter the electrolyte 2 during this off time. As it diffuses, new electrolyte 2 is supplied to the surface of emitter 5. Therefore, the concentration of the electrolytic solution 2 near the surface of the emitter 5 remains substantially constant during electrolytic polishing. Also, unlike conventional methods, the emitter 5 during electrolytic polishing
Since there is no need to take out the emitter 5 into the air, the surface of the emitter 5 will not be oxidized.
本発明は上述の実施例に限定されるものではなく、本発
明の技術的思想に基づく種々の変形が可能である。例え
ば、第２図に示す直流パルス電圧は、オン時間に対する
オフ時間の比が１以上であれば必要に応じて上述の実施
例とは異なる電圧値、周期、オン時間、オフ時間及び印
加時間を用いることも可能であるが、オン時間及びオフ
時間はそれぞれ１ｍ５ｅｃ以下及びｌ ｍ５ｅｃ以上で
あるのが好ましく、またオン時間に対するオフ時間の比
は４以上であるのが好ましい。なお本発明で用いる直流
パルス電圧は必ずしも第２図に示すような完会な方形波
である必要はない。また電解液やエミッター５の材質も
上述の実施例で用いたものに限定されるものではなく、
さらに電解研摩前のエミッター５の径も上述の実施例で
用いた数値に限定されるものではない。The present invention is not limited to the above-described embodiments, and various modifications can be made based on the technical idea of the present invention. For example, if the ratio of the off time to the on time is 1 or more, the DC pulse voltage shown in FIG. However, it is preferable that the on time and off time are less than 1 m5 ec and more than 1 m5 ec, respectively, and the ratio of off time to on time is preferably 4 or more. Note that the DC pulse voltage used in the present invention does not necessarily have to be a perfect square wave as shown in FIG. Furthermore, the materials of the electrolyte and the emitter 5 are not limited to those used in the above embodiments.
Further, the diameter of the emitter 5 before electrolytic polishing is not limited to the values used in the above embodiments.
発明の効果
本発明に係る電解研摩による針状体の形成方法によれば
、直流パルス電圧を用いしかもこの直流パルス電圧のオ
ン時間に対するオフ時間の比を１以」二としているので
、先端の曲率半径が極めて小さ−くかつ先端形状が良好
な針状体を再現性良く形成することができる。Effects of the Invention According to the method of forming a needle-shaped body by electrolytic polishing according to the present invention, a DC pulse voltage is used and the ratio of the DC pulse voltage's on time to off time is set to 1 or more, so that the curvature of the tip is reduced. A needle-shaped body with an extremely small radius and a good tip shape can be formed with good reproducibility.
４０図面のｒＩｒＩ車な説明
第１図は本発明に係る電解研摩による針状体の形成方法
を実施するための電解研摩装置の概略的な措成図、第２
図は第１図の直流パルス電源により発生される直流パル
ス電圧を示す電圧波形図、第３図は本発明に係る電解研
摩による針状体の形成方法により得られる針状エミッタ
ーの先端部を示す側面図、第４図は第３図に示すエミッ
ターの先端の拡大側面図である。40 Explanation of rIrI vehicle in drawings FIG. 1 is a schematic diagram of an electrolytic polishing apparatus for carrying out the method of forming needle-like bodies by electrolytic polishing according to the present invention, and FIG.
The figure is a voltage waveform diagram showing the DC pulse voltage generated by the DC pulse power supply in Figure 1, and Figure 3 shows the tip of a needle-shaped emitter obtained by the method for forming needle-shaped bodies by electrolytic polishing according to the present invention. Side View, FIG. 4 is an enlarged side view of the tip of the emitter shown in FIG. 3.
なお図面に用いられた符号において、
２−−−−−−−−−−−−−−−一電解液４−・−・
・−・−・・・−・−・・・直流パルス電源５−・・・
・−・・−一−−−−−−−−エミソター（針状体）６
−・−・・・・−・−・・対向電極
である。In addition, in the symbols used in the drawings, 2--
・−・−・−・−・DC pulse power supply 5−・・・・
・−・・−1−−−−−−−Emisotar (acicular body) 6
−・−・・−・−・・Counter electrode.
Claims (1)
時間に対するオフ時間の比を１以上としたことを特徴と
する電解研摩による針状体の形成方法。1. A method for forming a needle-like body by electrolytic polishing, characterized in that a DC pulse voltage is used and the ratio of the DC pulse voltage's off time to on time is 1 or more.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| JP15348184A JPS6132326A (en) | 1984-07-24 | 1984-07-24 | Formation of acicular body by electrolytic polishing |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| JP15348184A JPS6132326A (en) | 1984-07-24 | 1984-07-24 | Formation of acicular body by electrolytic polishing |
Publications (1)
| Publication Number | Publication Date |
|---|---|
| JPS6132326A true JPS6132326A (en) | 1986-02-15 |
Family
ID=15563514
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| JP15348184A Pending JPS6132326A (en) | 1984-07-24 | 1984-07-24 | Formation of acicular body by electrolytic polishing |
Country Status (1)
| Country | Link |
|---|---|
| JP (1) | JPS6132326A (en) |
Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JPH0272535A (en) * | 1988-09-06 | 1990-03-12 | Ube Ind Ltd | Tip sharpening method for electron cathode material |
Citations (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JPS5918541A (en) * | 1982-07-23 | 1984-01-30 | Hitachi Ltd | Manufacturing method for electron emission cathode |
-
1984
- 1984-07-24 JP JP15348184A patent/JPS6132326A/en active Pending
Patent Citations (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JPS5918541A (en) * | 1982-07-23 | 1984-01-30 | Hitachi Ltd | Manufacturing method for electron emission cathode |
Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JPH0272535A (en) * | 1988-09-06 | 1990-03-12 | Ube Ind Ltd | Tip sharpening method for electron cathode material |
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