JP2694776B2 - Diamond needle polishing method - Google Patents
Diamond needle polishing methodInfo
- Publication number
- JP2694776B2 JP2694776B2 JP821391A JP821391A JP2694776B2 JP 2694776 B2 JP2694776 B2 JP 2694776B2 JP 821391 A JP821391 A JP 821391A JP 821391 A JP821391 A JP 821391A JP 2694776 B2 JP2694776 B2 JP 2694776B2
- Authority
- JP
- Japan
- Prior art keywords
- diamond
- needle
- tip
- etching
- hardness
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
- Expired - Fee Related
Links
- 229910003460 diamond Inorganic materials 0.000 title claims description 28
- 239000010432 diamond Substances 0.000 title claims description 28
- 238000005498 polishing Methods 0.000 title claims description 16
- 238000000034 method Methods 0.000 title claims description 11
- UFHFLCQGNIYNRP-UHFFFAOYSA-N Hydrogen Chemical compound [H][H] UFHFLCQGNIYNRP-UHFFFAOYSA-N 0.000 claims description 7
- 239000001257 hydrogen Substances 0.000 claims description 7
- 229910052739 hydrogen Inorganic materials 0.000 claims description 7
- 238000001020 plasma etching Methods 0.000 claims description 3
- 239000012300 argon atmosphere Substances 0.000 claims description 2
- 239000010409 thin film Substances 0.000 description 14
- 238000005530 etching Methods 0.000 description 13
- 239000000523 sample Substances 0.000 description 13
- 238000000992 sputter etching Methods 0.000 description 7
- 238000007373 indentation Methods 0.000 description 5
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 description 4
- 239000007789 gas Substances 0.000 description 4
- 150000002500 ions Chemical class 0.000 description 4
- 230000000694 effects Effects 0.000 description 3
- 229910052799 carbon Inorganic materials 0.000 description 2
- 239000010408 film Substances 0.000 description 2
- 229910002804 graphite Inorganic materials 0.000 description 2
- 239000010439 graphite Substances 0.000 description 2
- 150000002430 hydrocarbons Chemical class 0.000 description 2
- 238000004519 manufacturing process Methods 0.000 description 2
- 229910001220 stainless steel Inorganic materials 0.000 description 2
- 239000010935 stainless steel Substances 0.000 description 2
- 239000000758 substrate Substances 0.000 description 2
- 230000005641 tunneling Effects 0.000 description 2
- 239000004215 Carbon black (E152) Substances 0.000 description 1
- 230000001133 acceleration Effects 0.000 description 1
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 description 1
- 238000005516 engineering process Methods 0.000 description 1
- 239000011521 glass Substances 0.000 description 1
- 238000009499 grossing Methods 0.000 description 1
- 238000007542 hardness measurement Methods 0.000 description 1
- 229930195733 hydrocarbon Natural products 0.000 description 1
- 238000005468 ion implantation Methods 0.000 description 1
- 239000000463 material Substances 0.000 description 1
- 230000003287 optical effect Effects 0.000 description 1
- 239000001301 oxygen Substances 0.000 description 1
- 229910052760 oxygen Inorganic materials 0.000 description 1
- 238000007517 polishing process Methods 0.000 description 1
- 238000003825 pressing Methods 0.000 description 1
- 239000007787 solid Substances 0.000 description 1
- 239000000126 substance Substances 0.000 description 1
- 230000003746 surface roughness Effects 0.000 description 1
Landscapes
- Crystals, And After-Treatments Of Crystals (AREA)
Description
【０００１】[0001]
【産業上の利用分野】本発明は、押込み式の硬度計に用
いられるダイヤモンド圧子や、走査型トンネル顕微鏡に
用いられるダイヤモンド製の走査探針等、いわゆる鋭利
な先端を有するダイヤモンド針の研磨方法に関する。BACKGROUND OF THE INVENTION 1. Field of the Invention The present invention relates to a method for polishing a diamond needle having a sharp tip, such as a diamond indenter used in an indentation type hardness tester and a diamond scanning probe used in a scanning tunneling microscope. .
【０００２】[0002]
【従来の技術】ビッカース硬度計のような押込み式の硬
度計では、従来よりダイヤモンド製の押込み圧子が用い
られている。近年、ＬＳＩ，磁気ディスク，光ディスク
などの各種薄膜デバイスが実用化されるに伴い、それら
デバイスを構成する薄膜の機械的性質に基づいた製品管
理やプロセス管理、特に測定が比較的容易な押込み硬度
に基づいた製品管理やプロセス管理が重要視されてき
た。このような技術的背景から、従来測定が困難であっ
た厚さがサブミクロン以下の薄膜についても硬度の測定
を可能にした硬度計が例えば、ワイ ツカモト（Ｙ．Ｔ
ｓｕｋａｍｏｔｏ）等により、スイン ソリッド フィ
ルムズ（Ｔｈｉｎ ＳｏｌｉｄＦｉｌｍｓ）１５４巻，
１９８７年，１７１頁に報告され、かつ市販されてい
る。2. Description of the Related Art Indentation type hardness meters such as the Vickers hardness meter have conventionally used diamond indenters. With the recent commercialization of various thin film devices such as LSIs, magnetic disks, and optical disks, product management and process management based on the mechanical properties of the thin films that make up these devices, especially indentation hardness that is relatively easy to measure. Product management and process management based on it have been emphasized. From such a technical background, there is a hardness meter that can measure the hardness of a thin film having a thickness of submicron or less, which has been difficult to measure in the past, for example, a Weizkamoto (Y.T.
Sukamoto) and others, Thin Solid Films 154 volumes,
1987, page 171 and commercially available.
【０００３】薄膜用の押込み硬度計では、押込み圧子先
端の曲率半径をいかに小さくするかが１つの技術的な課
題である。ダイヤモンド針は通常研磨砥石を用いて機械
研磨することによって、その先端を鋭利にするが、機械
研磨によって得られる先端の最小曲率半径は１μｍ程度
であり、少なくともサブミクロンの曲率半径を要求する
薄膜硬度計用の圧子に用いることは困難である。In the indentation hardness tester for thin film, one technical problem is how to reduce the radius of curvature of the tip of the indenter. Diamond needles are usually sharpened by mechanically polishing with a grinding wheel, but the minimum radius of curvature of the mechanically polished tip is about 1 μm, and a thin film hardness that requires at least a submicron radius of curvature. It is difficult to use as a measuring indenter.
【０００４】また、近年急速に普及した走査型トンネル
顕微鏡（以下、ＳＴＭと略す。）においても走査探針先
端の鋭利化は、原子オーダーの高い分解能を保証し、表
面形状を忠実に再現するうえで、必須の技術である。ま
た、走査探針には長時間にわたって安定したトンネル電
流が測定できるという意味での化学的安定性と、試料と
探針との衝突時に探針先端が破損し難いという意味で機
械的耐久性も要求されるが、以上の点を克服するものと
して表面にイオン注入を施した伝導性ダイヤモンドが注
目されている。Further, in the scanning tunneling microscope (hereinafter abbreviated as STM) which has rapidly spread in recent years, sharpening of the tip of the scanning probe guarantees a high resolution of atomic order and faithfully reproduces the surface shape. It is an essential technology. The scanning probe also has chemical stability in the sense that a stable tunnel current can be measured for a long time, and mechanical durability in the sense that the probe tip is less likely to be damaged when the sample collides with the probe. Although required, conductive diamond having an ion-implanted surface has attracted attention as a means of overcoming the above points.
【０００５】[0005]
【発明が解決しようとする課題】以上のようにダイヤモ
ンド製の圧子や走査探針に少なくともサブミクロン以下
の先端半径を与える技術に対して強い要求があるが、従
来の機械研磨法ではこれらに適した鋭利な先端半径を有
するダイヤモンド針を製造することは困難であった。As described above, there is a strong demand for a technique of giving a tip radius of at least a submicron or less to a diamond indenter or a scanning probe, but the conventional mechanical polishing method is suitable for these. It has been difficult to manufacture diamond needles with sharp tip radii.
【０００６】[0006]
【課題を解決するための手段】本発明のダイヤモンド針
の研磨方法は、先端の曲率半径を１μｍ程度に機械研磨
を施したダイヤモンド針に水素を含むアルゴン雰囲気で
の反応性イオンエッチングを施すものである。According to the method of polishing a diamond needle of the present invention, a diamond needle mechanically polished to have a radius of curvature of about 1 μm is subjected to reactive ion etching in an argon atmosphere containing hydrogen. is there.
【０００７】[0007]
【作用】従来、イオンエッチングはＬＳＩなど多くの薄
膜デバイスに微細パターンを形成する手段として用いら
れている技術である。Ａｒなどの元素をプラズマなどに
よってイオン化し、陽極／試料（陰極）間に印加した電
圧によって加速したイオンを試料に衝突させることによ
って試料表面の一部もしくは全部をエッチングする（は
ぎとる）ものである。しかし、通常のＡｒイオンを用い
たイオンエッチングではダイヤモンド表面に機械研磨時
の傷が残留し、十分な平滑化が達せられないこと、ダイ
ヤモンド（炭素）のような酸素と反応して気体を形成す
るものは機械研磨に比較すれば鋭利になるものの、先の
薄膜硬度計やＳＴＭに要求される十分な先端半径を得る
ことは難しいことなどの欠点がある。そこで、Ａｒに水
素を混入すると、ダイヤモンド（炭素）表面と水素とが
反応することによって炭化水素化合物が形成され、炭化
水素がエッチングされることによって機械研磨時の傷が
平滑化し、かつ先端がより鋭利化かつ平滑化することの
作用に基づいてダイヤモンド針先端を精密に研磨するこ
とができる。In the past, ion etching is a technique used as a means for forming fine patterns in many thin film devices such as LSI. An element such as Ar is ionized by plasma or the like, and ions accelerated by a voltage applied between the anode and the sample (cathode) are made to collide with the sample, thereby etching (peeling off) part or all of the sample surface. However, ordinary ion etching using Ar ions leaves scratches on the diamond surface during mechanical polishing, and cannot be sufficiently smoothed. It reacts with oxygen such as diamond (carbon) to form a gas. Although the material is sharper than mechanical polishing, it has a drawback that it is difficult to obtain a sufficient tip radius required for the thin film hardness meter and STM. Therefore, when hydrogen is mixed into Ar, a diamond (carbon) surface reacts with hydrogen to form a hydrocarbon compound, and the hydrocarbon is etched to smooth the scratches during mechanical polishing and to further improve the tip. The tip of the diamond needle can be precisely polished based on the effect of sharpening and smoothing.
【０００８】[0008]
【実施例】イオンエッチング処理を行うダイヤモンド針
は、直径３ｍｍ，長さ６ｍｍのステンレス製棒の先端に
ろう付けし、対面角８０°の三角錐に機械研磨を施した
ものであり、その先端の曲率半径は１．５μｍである。
また、三角錐平面部の最大表面粗さＲmax は０．１５μ
ｍである。なお、機械研磨では研磨時にダイヤモンド針
先端に作用する力によって先端にチッピングが生じ、曲
率半径を１．５μｍ以下にすることは不可能であった。
機械研磨を施したこのダイヤモンド針をイオンエッチン
グ装置の陰極に取り付ける。ダイヤモンド針の取り付け
は、ステンレス製棒の中心軸がイオンエッチング装置の
陽極に対して垂直になるように行う。したがって、研磨
すべきダイヤモンド三角錐針の表面は、入射イオンに対
して先の対面角８０°に相当する角度分傾斜している。EXAMPLE A diamond needle for ion etching is a stainless steel rod having a diameter of 3 mm and a length of 6 mm which is brazed to a triangular pyramid having a facing angle of 80 ° and mechanically polished. The radius of curvature is 1.5 μm.
Further, the maximum surface roughness R max of the triangular pyramid flat portion is 0.15 μm.
m. In mechanical polishing, chipping occurs at the tip due to the force acting on the tip of the diamond needle during polishing, and it has been impossible to reduce the radius of curvature to 1.5 μm or less.
This mechanically polished diamond needle is attached to the cathode of the ion etching device. The diamond needle is attached so that the central axis of the stainless steel rod is perpendicular to the anode of the ion etching apparatus. Therefore, the surface of the diamond triangular pyramid needle to be polished is inclined with respect to the incident ions by the angle corresponding to the above-mentioned facing angle of 80 °.
【０００９】針を取り付けた後、イオンエッチング装置
の真空排気を行う。到達真空度は５×１０-7Ｔｏｒｒで
ある。イオンエッチング条件は以下のとうりである。Ａ
ｒに体積比で１０％の水素を添加し、その圧力を１×１
０-4Ｔｏｒｒとした。イオンの加速電圧は５００Ｖ，エ
ッチング時間は４時間で行った。エッチング後のダイヤ
モンド先端の曲率半径は０．０６μｍ、三角錐平面部の
Ｒmax は０．０５μｍであった。After attaching the needle, the ion etching apparatus is evacuated. The ultimate vacuum is 5 × 10 −7 Torr. Ion etching conditions are as follows. A
Add 10% hydrogen by volume to r and adjust the pressure to 1 × 1.
0 -4 Torr. The ion acceleration voltage was 500 V, and the etching time was 4 hours. The radius of curvature of the diamond tip after etching was 0.06 μm, and the R max of the triangular pyramid flat portion was 0.05 μm.
【００１０】比較のために、エッチングガスをＡｒのみ
とし、他の条件は先と同様の条件でエッチングを行っ
た。エッチング後のダイヤモンド先端の曲率半径は０．
５μｍ、三角錐平面部のＲmax は０．１０μｍであっ
た。機械研磨に比較すれば、先端が鋭利になり、機械研
磨による傷も平滑化しているが、Ａｒに水素を添加した
場合に比較するとその効果は小さいことがわかる。For comparison, etching was carried out under the same conditions as above except that Ar was used as the etching gas. The radius of curvature of the diamond tip after etching is 0.
5 μm, R max of the triangular pyramid plane portion was 0.10 μm. Compared with mechanical polishing, the tip is sharper and the scratches due to mechanical polishing are smoothed, but it is clear that the effect is smaller than when hydrogen is added to Ar.
【００１１】従来の機械研磨したダイヤモンド針（機械
研磨針）と、Ａｒガスのみでエッチングした針（Ａｒエ
ッチング針）及び実施例による針（ＡｒＨエッチング
針）の３本の針を先に引用した薄膜用押込み硬度計の圧
子として用い、膜厚０．１μｍの各種薄膜について硬度
測定を行った。機械研磨針は先端半径が大きいため、測
定硬度値に基板（ガラス基板）の硬度が影響し、薄膜の
硬度を正確に測定することが困難であった。Ａｒエッチ
ング針とＡｒＨエッチング針では薄膜の硬度の測定は可
能であったが、特にＡｒエッチング針はＲmax が大きい
ために測定値のバラツキが大であった。A thin film of the above-mentioned three needles, a conventional mechanically polished diamond needle (mechanical polished needle), a needle etched only with Ar gas (Ar etching needle) and a needle according to the embodiment (ArH etching needle). The hardness was measured for various thin films having a film thickness of 0.1 μm, which were used as an indenter for an indentation hardness tester. Since the mechanical polishing needle has a large tip radius, the hardness of the substrate (glass substrate) affects the measured hardness value, making it difficult to accurately measure the hardness of the thin film. It was possible to measure the hardness of the thin film with the Ar etching needle and the ArH etching needle. However, the Ar etching needle had a large R max , and therefore the measured values varied greatly.
【００１２】また、膜厚０．０５μｍの薄膜についての
硬度測定ではＡｒＨエッチング針のみが薄膜の硬度を分
離・測定することができた。また、ＳＴＭの探針に上記
３本の針を用い、グラファイトについて観察を行ったと
ころ、機械研磨針では原子分解能が得られなかったが、
ノイズが少ない最も明瞭なグラファイト原子像が得られ
た。なお、ＳＴＭの探針として上記３本のダイヤモンド
針を用いる場合には、電気伝導性を確保するためにＣｕ
のイオン注入処理を施こした。In the hardness measurement of a thin film having a thickness of 0.05 μm, only the ArH etching needle could separate and measure the hardness of the thin film. Further, when the above-mentioned three needles were used for the STM probe and the graphite was observed, it was impossible to obtain atomic resolution with the mechanical polishing needle.
The clearest graphite atomic image with little noise was obtained. When the above-mentioned three diamond needles are used as the STM probe, Cu is used to ensure electrical conductivity.
Ion implantation process was performed.
【００１３】[0013]
【発明の効果】以上のように本発明は、従来の機械研磨
法によって作製したダイヤモンド針に、Ａｒに水素を添
加したエッチングガスを用いた反応性イオンエッチング
を施すことにより、機械研磨法では困難であった０．１
μｍ以下の先端の曲率半径と極めて良好な表面性が得ら
れるという効果がある。この鋭利化と良好な表面性によ
り、薄膜硬度計用の押込み圧子或いはＳＴＭ用の探針と
して優れた特性を有するダイヤモンド針を作製すること
ができる。As described above, the present invention is difficult to perform by the mechanical polishing method by subjecting a diamond needle manufactured by the conventional mechanical polishing method to reactive ion etching using an etching gas obtained by adding hydrogen to Ar. Was 0.1
There is an effect that a radius of curvature of the tip of μm or less and an extremely good surface property can be obtained. Due to this sharpening and good surface properties, it is possible to manufacture a diamond needle having excellent properties as a pressing indenter for a thin film hardness meter or a probe for STM.
Claims (1)
を施したダイヤモンド針に水素を含むアルゴン雰囲気で
の反応性イオンエッチングを施すことを特徴とするダイ
ヤモンド針の研磨方法1. A method for polishing a diamond needle, characterized in that a diamond needle mechanically polished to have a radius of curvature of about 1 μm is subjected to reactive ion etching in an argon atmosphere containing hydrogen.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| JP821391A JP2694776B2 (en) | 1991-01-28 | 1991-01-28 | Diamond needle polishing method |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| JP821391A JP2694776B2 (en) | 1991-01-28 | 1991-01-28 | Diamond needle polishing method |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| JPH04244000A JPH04244000A (en) | 1992-09-01 |
| JP2694776B2 true JP2694776B2 (en) | 1997-12-24 |
Family
ID=11686956
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| JP821391A Expired - Fee Related JP2694776B2 (en) | 1991-01-28 | 1991-01-28 | Diamond needle polishing method |
Country Status (1)
| Country | Link |
|---|---|
| JP (1) | JP2694776B2 (en) |
Families Citing this family (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JP3971090B2 (en) * | 2000-04-05 | 2007-09-05 | 株式会社神戸製鋼所 | Method for producing diamond having needle-like surface and method for producing carbon-based material having cilia-like surface |
| JP4697514B2 (en) * | 2004-01-16 | 2011-06-08 | 住友電気工業株式会社 | Diamond single crystal substrate manufacturing method and diamond single crystal substrate |
-
1991
- 1991-01-28 JP JP821391A patent/JP2694776B2/en not_active Expired - Fee Related
Also Published As
| Publication number | Publication date |
|---|---|
| JPH04244000A (en) | 1992-09-01 |
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