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JP7478335B2 - How diamonds are processed - Google Patents
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JP7478335B2 - How diamonds are processed - Google Patents

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JP7478335B2
JP7478335B2 JP2020093193A JP2020093193A JP7478335B2 JP 7478335 B2 JP7478335 B2 JP 7478335B2 JP 2020093193 A JP2020093193 A JP 2020093193A JP 2020093193 A JP2020093193 A JP 2020093193A JP 7478335 B2 JP7478335 B2 JP 7478335B2
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nickel
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規夫 徳田
孝夫 猪熊
翼 松本
平 莨谷
雅嗣 長井
勇斗 中村
和斗 坂内
俊晴 牧野
宙光 加藤
聡 山崎
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Kanazawa University NUC
National Institute of Advanced Industrial Science and Technology AIST
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National Institute of Advanced Industrial Science and Technology AIST
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特許法第30条第2項適用 1.刊行物 2019年第80回応用物理学会秋季学術講演会 予稿集「20p-E312-1」,発行日 2019年9月4日 2.集会名 2019年第80回応用物理学会秋季学術講演会,開催日 令和1年9月20日,開催場所 北海道大学 札幌キャンパス(北海道札幌市北区北8条西5丁目 3.刊行物 The 2nd International Forum on Quantum Metrology and Sensing PROCEEDINGS,第40ページ 4.集会名 The 2nd International Forum on Quantum Metrology and Sensing,開催日 令和1年12月17日,開催場所 京都ブライトンホテル(京都府京都市上京区仕丁町330新町通中立売下る) 5.刊行物 Hasselt Diamond Workshop 2020-SBDD XXV 予稿集,発行日 令和2年3月10日Article 30, paragraph 2 of the Patent Act applies 1. Publication: 80th Autumn Meeting of the Japan Society of Applied Physics, Abstracts "20p-E312-1", published September 4, 2019 2. Meeting name: The 80th Autumn Meeting of the Japan Society of Applied Physics, held on September 20, 2019, at Hokkaido University Sapporo Campus (5-chome, Kita 8-jo Nishi, Kita-ku, Sapporo, Hokkaido 3. Publication: The 2nd International Forum on Quantum Metrology and Sensing PROCEEDINGS, page 40 4. Meeting name: The 2nd International Forum on Quantum Metrology and Sensing, held on December 17, 2019, at Kyoto Brighton Hotel (330, Shicho-cho, Kamigyo-ku, Kyoto, Kyoto Prefecture) 5. Publication: Hasselt Diamond Workshop 2020-SBDD XXV Proceedings, Publication date: March 10, 2020

本発明は、ダイヤモンドの加工方法に関し、特にインプリント技術を応用した加工方法に係る。 The present invention relates to a method for processing diamonds, and in particular to a processing method that applies imprint technology.

ダイヤモンドは物質の中で最も硬い分類に属し、所望する形状や構造への加工が難しい。
ダイヤモンドは大きなバンドギャップを有するために半導体材料として優れていることから、各種半導体・量子デバイス、センサーへの応用が期待されている。
また、宝飾品としての高い価値も有している。
このようなニーズから、ダイヤモンドの精度が高く、安価な加工方法が期待されている。
従来、ダイヤモンドを半導体デバイスとしてパターニングを行う場合に、ダイヤモンドの表面を所定のパターンにマスキングし、プラズマ等によりドライエッチングする方法が行われている。
しかしながら、特殊な装置が必要で高価であるとともに、マスキングパターンを垂直方向にエッチングすることが難しいために加工精度も高くない。
例えば、特許文献1に誘導結合プラズマエッチング方法を開示するが、同技術もエッチング技術であることから上記と同様の技術的課題を有している。
Diamond is one of the hardest materials and is difficult to machine into desired shapes and structures.
Diamond has a large band gap and is therefore an excellent semiconductor material, and is therefore expected to be used in a variety of semiconductor and quantum devices and sensors.
It also has high value as jewelry.
In response to these needs, there is a demand for a highly accurate and inexpensive method for processing diamonds.
Conventionally, when diamond is patterned as a semiconductor device, the surface of the diamond is masked in a predetermined pattern and then dry etched with plasma or the like.
However, this method requires special equipment, which is expensive, and also does not provide high processing accuracy because it is difficult to etch the masking pattern in the vertical direction.
For example, Patent Document 1 discloses an inductively coupled plasma etching method, but since this technique is also an etching technique, it has the same technical problems as those mentioned above.

特開2013-211562号公報JP 2013-211562 A

本発明は、加工精度が高く、低コスト化が可能なインプリントによるダイヤモンドの加工方法の提供を目的とする。 The present invention aims to provide a method for processing diamonds by imprinting, which has high processing accuracy and enables low cost.

本発明に係るインプリントによるダイヤモンドの加工方法は、表面が所定の構造に形成された炭素固溶性基材をダイヤモンドの表面に接触させた状態で加熱することで、前記ダイヤモンドの表面に前記炭素固溶性基材の表面構造が転写成形されることを特徴とする。 The method for processing diamonds by imprinting according to the present invention is characterized in that a carbon-soluble substrate, the surface of which has been formed into a predetermined structure, is heated while in contact with the surface of the diamond, so that the surface structure of the carbon-soluble substrate is transferred to the surface of the diamond.

ここで、炭素固溶性基材とは、ダイヤモンドの表面に接触させた状態で加熱すると接触部でダイヤモンドを構成する炭素を固溶化し、固溶エッチングが進行する基材をいう。
このような炭素固溶性基材としては、ニッケル、鉄、コバルト、チタン、クロム、銅及びそれらの酸化物又は合金等が例として挙げられる。
その中でもニッケルは、炭素の最大固溶濃度が2.7at%と高く、高温でも炭化物を形成しにくい優れた性質を有している。
ダイヤモンドの表面に接触した基材への炭素固溶を促進するには、800℃以上の加熱が好ましい。
加熱温度が高い方が固溶化反応は速くなるが、高温になり過ぎると基材の表面に炭化物が形成され易く、逆に固溶化の阻害要因となるため1200℃以下が好ましい。
Here, the carbon-soluble substrate refers to a substrate that, when heated in contact with the surface of a diamond, turns the carbon that constitutes the diamond into a solid solution at the contact area, and solid solution etching proceeds.
Examples of such carbon-solid-soluble substrates include nickel, iron, cobalt, titanium, chromium, copper, and oxides or alloys thereof.
Among these, nickel has a high maximum solid solution concentration of carbon of 2.7 at %, and has the excellent property of being resistant to the formation of carbides even at high temperatures.
In order to promote the formation of a solid solution of carbon in the substrate in contact with the surface of the diamond, heating to 800° C. or higher is preferred.
The higher the heating temperature, the faster the solution reaction will be. However, if the temperature is too high, carbides are likely to be formed on the surface of the base material, which in turn becomes an obstacle to solution formation, so the temperature is preferably 1200° C. or lower.

加熱は、基材の炭化を抑えるために不活性ガス又は真空下において行うのが好ましい。
不活性ガスとしては、アルゴン、窒素、ヘリウム等が例として挙げられ、真空下とは、ダイヤモンドの表面の固溶化に影響を与えない範囲に減圧されていることをいう。
ダイヤモンドの表面の固溶化に伴い、この表面にグラファイト層が形成されるため、ダイヤモンドの加工後に熱混酸でこのグラファイト層を除去洗浄してもよい。
また、不活性ガス又は真空下で加熱する際に加熱雰囲気中に2~10vol%の水素ガスを含有させると、グラファイトをメタンガスとして除去させることもできる。
また、この加熱雰囲気中に水蒸気を2~10vol%含有させると、ニッケル基材の表面に酸化膜を形成し、これがニッケル中の固溶炭素と反応することで一酸化炭素又は/及び二酸化炭素として除去することができる。
なお、不活性ガス中の場合は、大気圧又はそれ以上の圧力でもよく、固溶エッチングが促進される。
Heating is preferably carried out under an inert gas or vacuum to prevent carbonization of the substrate.
Examples of inert gases include argon, nitrogen, and helium. "Under vacuum" means that the pressure is reduced to a level that does not affect the formation of a solid solution on the surface of diamond.
As the surface of the diamond is solidified, a graphite layer is formed on this surface. After processing of the diamond, this graphite layer may be removed by washing with hot mixed acid.
Furthermore, when heating is performed in an inert gas or vacuum, if 2 to 10 vol % of hydrogen gas is contained in the heating atmosphere, graphite can be removed as methane gas.
Furthermore, if the heating atmosphere contains 2 to 10 vol % water vapor, an oxide film is formed on the surface of the nickel base material, which reacts with the dissolved carbon in the nickel and can be removed as carbon monoxide and/or carbon dioxide.
In the case of an inert gas, the pressure may be atmospheric pressure or higher, and solid solution etching is promoted.

本発明において、炭素固溶性基材は、ニッケル、鉄、コバルト及びチタン、クロム、銅及びそれらの酸化物又は合金のうちいずれかであることが好ましい。
これらの炭素固溶性基材は、ダイヤモンドよりもはるかに加工しやすく、インプリント成形のいわば転写鋳型としてデバイスパターンや複雑な微細構造に加工ができる。
また、宝飾ダイヤモンドとしての転写鋳型形状に加工することもできる。
In the present invention, the carbon-solid-soluble substrate is preferably any one of nickel, iron, cobalt, titanium, chromium, copper, and oxides or alloys thereof.
These carbon-soluble substrates are much easier to process than diamond, and can be used as a kind of transfer mold for imprint molding to process device patterns and complex microstructures.
It can also be processed into a transfer mold shape for jewelry diamonds.

本発明は、ニッケル等の基材による炭素固溶反応を利用して、基材の表面に形成した構造にならってダイヤモンドの表面が固溶化及びエッチングされるため、基材の表面構造が精度高く転写成形される。
本発明は、不活性ガス下又は真空下で加熱できる加熱装置があればよく、従来のプラズマ装置よりも構造が簡単で大型化も容易である。
The present invention utilizes a carbon solid solution reaction with a base material such as nickel, and the surface of the diamond is solid-solutioned and etched in accordance with the structure formed on the surface of the base material, thereby allowing the surface structure of the base material to be transferred and molded with high precision.
The present invention requires only a heating device capable of heating under an inert gas or under a vacuum, and has a simpler structure than conventional plasma devices and can be easily made large.

本発明に用いる基材の表面構造例を示す。2 shows examples of the surface structure of the substrate used in the present invention. 図1の基材の構造を転写したダイヤモンド表面構造例を示す。2 shows an example of a diamond surface structure to which the structure of the substrate in FIG. 1 has been transferred.

以下、本発明に係るインプリントによるダイヤモンドの加工方法の実施例を具体的に説明するが、本発明は本実施例に限定されるものではない。
図1に、ニッケル基材を用いて表面に微小の凹部形状を形成した転写鋳型の例を示す。
本実施例では、ニッケル基材の表面を水素含有アルゴンガス下で約1100℃、約10分の還元処理を行った。
次に、図1に示したニッケル基材の上にダイヤモンドの表面が重なるように積み重ね、その上に所定の重さの重しを乗せ、適度にニッケル基材の表面とダイヤモンドの接触状態が維持されるようにした。
この状態で赤外線加熱方式のアニール炉に投入し、不活性ガスとしてアルゴンガスを用いて水素ガスを約4vol%混合させた。
図2に、約800℃以上1200℃以下の範囲に加熱し、所定時間経過後に炉から取り出し、ニッケル基材を取り外したダイヤモンドの表面写真を示す。
図1に示したニッケル基材の表面構造が精密に転写されているのが分かる。
Hereinafter, examples of the method for processing diamond by imprinting according to the present invention will be specifically described, but the present invention is not limited to these examples.
FIG. 1 shows an example of a transfer mold in which a nickel base material is used and minute recesses are formed on the surface.
In this embodiment, the surface of the nickel base material was subjected to a reduction treatment in hydrogen-containing argon gas at about 1100° C. for about 10 minutes.
Next, the diamond was stacked on top of the nickel substrate shown in FIG. 1 so that the surface of the diamond overlapped, and a weight of a predetermined weight was placed on top of the stack to maintain an appropriate contact state between the surface of the nickel substrate and the diamond.
In this state, the product was placed in an infrared heating annealing furnace, and argon gas was used as the inert gas, and about 4 vol % of hydrogen gas was mixed therein.
FIG. 2 shows a photograph of the surface of a diamond that has been heated to a temperature range of about 800° C. to 1200° C., taken out of the furnace after a predetermined time has elapsed, and then the nickel substrate has been removed.
It can be seen that the surface structure of the nickel base material shown in FIG. 1 has been precisely transferred.

Claims (2)

表面が所定の構造に形成された炭素固溶性基材をダイヤモンドの表面に接触させた状態で加熱することで、
前記ダイヤモンドの表面に前記炭素固溶性基材の表面構造が転写成形されるものであり、
前記加熱は不活性ガス又は真空下、所定の濃度の水素ガス又は/及び水蒸気が含有された状態で行われ、
前記炭素固溶性基材は水素含有不活性ガス中にて表面を還元処理したニッケル基材であることを特徴とするインプリントによるダイヤモンドの加工方法。
A carbon-dissolved substrate with a surface formed into a specific structure is heated in contact with the diamond surface,
a surface structure of the carbon-soluble substrate is transferred onto a surface of the diamond ;
The heating is carried out under an inert gas or vacuum, in a state containing a predetermined concentration of hydrogen gas and/or water vapor,
2. A method for processing diamond by imprinting, wherein the carbon-soluble substrate is a nickel substrate the surface of which has been subjected to reduction treatment in a hydrogen-containing inert gas .
前記加熱は800~1200℃の範囲であることを特徴とする請求項1記載のインプリントによるダイヤモンドの加工方法。 2. The method for processing diamond by imprinting according to claim 1, wherein the heating is in the range of 800 to 1200°C .
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Citations (4)

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Publication number Priority date Publication date Assignee Title
JP2000281489A (en) 1999-03-31 2000-10-10 Hamamatsu Photonics Kk Method for forming pattern on diamond substrate surface
JP2000281488A (en) 1999-03-31 2000-10-10 Hamamatsu Photonics Kk Surface processing of diamond substrate
JP2017092356A (en) 2015-11-16 2017-05-25 国立大学法人金沢大学 Diamond processing method
JP2018140354A (en) 2017-02-28 2018-09-13 学校法人慶應義塾 Method for manufacturing carbon-based super-hard structure and method for manufacturing mold

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GB2061904B (en) * 1979-04-13 1983-03-30 Inst Geol Yakut Filiala Sibir Method of processing diamonds

Patent Citations (4)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
JP2000281489A (en) 1999-03-31 2000-10-10 Hamamatsu Photonics Kk Method for forming pattern on diamond substrate surface
JP2000281488A (en) 1999-03-31 2000-10-10 Hamamatsu Photonics Kk Surface processing of diamond substrate
JP2017092356A (en) 2015-11-16 2017-05-25 国立大学法人金沢大学 Diamond processing method
JP2018140354A (en) 2017-02-28 2018-09-13 学校法人慶應義塾 Method for manufacturing carbon-based super-hard structure and method for manufacturing mold

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