JP2003313571A - Carbon nanohorn solid lubricant - Google Patents

Carbon nanohorn solid lubricant

Info

Publication number
JP2003313571A
JP2003313571A JP2002118500A JP2002118500A JP2003313571A JP 2003313571 A JP2003313571 A JP 2003313571A JP 2002118500 A JP2002118500 A JP 2002118500A JP 2002118500 A JP2002118500 A JP 2002118500A JP 2003313571 A JP2003313571 A JP 2003313571A
Authority
JP
Japan
Prior art keywords
carbon nanohorn
solid lubricant
friction
test
aggregate
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
Application number
JP2002118500A
Other languages
Japanese (ja)
Inventor
Sumio Iijima
澄男 飯島
Masako Yudasaka
雅子 湯田坂
Kazunori Umeda
一徳 梅田
Akihiro Tanaka
章浩 田中
Current Assignee (The listed assignees may be inaccurate. Google has not performed a legal analysis and makes no representation or warranty as to the accuracy of the list.)
Japan Science and Technology Agency
NEC Corp
National Institute of Advanced Industrial Science and Technology AIST
Original Assignee
NEC Corp
National Institute of Advanced Industrial Science and Technology AIST
Japan Science and Technology Corp
Priority date (The priority date 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 date listed.)
Filing date
Publication date
Application filed by NEC Corp, National Institute of Advanced Industrial Science and Technology AIST, Japan Science and Technology Corp filed Critical NEC Corp
Priority to JP2002118500A priority Critical patent/JP2003313571A/en
Priority to PCT/JP2003/004181 priority patent/WO2003089552A1/en
Publication of JP2003313571A publication Critical patent/JP2003313571A/en
Pending legal-status Critical Current

Links

Classifications

    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B82—NANOTECHNOLOGY
    • B82Y—SPECIFIC USES OR APPLICATIONS OF NANOSTRUCTURES; MEASUREMENT OR ANALYSIS OF NANOSTRUCTURES; MANUFACTURE OR TREATMENT OF NANOSTRUCTURES
    • B82Y30/00—Nanotechnology for materials or surface science, e.g. nanocomposites
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B82—NANOTECHNOLOGY
    • B82Y—SPECIFIC USES OR APPLICATIONS OF NANOSTRUCTURES; MEASUREMENT OR ANALYSIS OF NANOSTRUCTURES; MANUFACTURE OR TREATMENT OF NANOSTRUCTURES
    • B82Y40/00—Manufacture or treatment of nanostructures
    • C—CHEMISTRY; METALLURGY
    • C01—INORGANIC CHEMISTRY
    • C01B—NON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
    • C01B32/00—Carbon; Compounds thereof
    • C01B32/15—Nano-sized carbon materials
    • C01B32/18—Nanoonions; Nanoscrolls; Nanohorns; Nanocones; Nanowalls
    • C—CHEMISTRY; METALLURGY
    • C10—PETROLEUM, GAS OR COKE INDUSTRIES; TECHNICAL GASES CONTAINING CARBON MONOXIDE; FUELS; LUBRICANTS; PEAT
    • C10M—LUBRICATING COMPOSITIONS; USE OF CHEMICAL SUBSTANCES EITHER ALONE OR AS LUBRICATING INGREDIENTS IN A LUBRICATING COMPOSITION
    • C10M103/00—Lubricating compositions characterised by the base-material being an inorganic material
    • C10M103/02—Carbon; Graphite
    • C—CHEMISTRY; METALLURGY
    • C10—PETROLEUM, GAS OR COKE INDUSTRIES; TECHNICAL GASES CONTAINING CARBON MONOXIDE; FUELS; LUBRICANTS; PEAT
    • C10M—LUBRICATING COMPOSITIONS; USE OF CHEMICAL SUBSTANCES EITHER ALONE OR AS LUBRICATING INGREDIENTS IN A LUBRICATING COMPOSITION
    • C10M2201/00—Inorganic compounds or elements as ingredients in lubricant compositions
    • C10M2201/04—Elements
    • C10M2201/041—Carbon; Graphite; Carbon black
    • C—CHEMISTRY; METALLURGY
    • C10—PETROLEUM, GAS OR COKE INDUSTRIES; TECHNICAL GASES CONTAINING CARBON MONOXIDE; FUELS; LUBRICANTS; PEAT
    • C10M—LUBRICATING COMPOSITIONS; USE OF CHEMICAL SUBSTANCES EITHER ALONE OR AS LUBRICATING INGREDIENTS IN A LUBRICATING COMPOSITION
    • C10M2201/00—Inorganic compounds or elements as ingredients in lubricant compositions
    • C10M2201/04—Elements
    • C10M2201/041—Carbon; Graphite; Carbon black
    • C10M2201/0413—Carbon; Graphite; Carbon black used as base material
    • C—CHEMISTRY; METALLURGY
    • C10—PETROLEUM, GAS OR COKE INDUSTRIES; TECHNICAL GASES CONTAINING CARBON MONOXIDE; FUELS; LUBRICANTS; PEAT
    • C10N—INDEXING SCHEME ASSOCIATED WITH SUBCLASS C10M RELATING TO LUBRICATING COMPOSITIONS
    • C10N2020/00—Specified physical or chemical properties or characteristics, i.e. function, of component of lubricating compositions
    • C10N2020/01—Physico-chemical properties
    • C10N2020/055—Particles related characteristics
    • C10N2020/06—Particles of special shape or size
    • C—CHEMISTRY; METALLURGY
    • C10—PETROLEUM, GAS OR COKE INDUSTRIES; TECHNICAL GASES CONTAINING CARBON MONOXIDE; FUELS; LUBRICANTS; PEAT
    • C10N—INDEXING SCHEME ASSOCIATED WITH SUBCLASS C10M RELATING TO LUBRICATING COMPOSITIONS
    • C10N2030/00—Specified physical or chemical properties which is improved by the additive characterising the lubricating composition, e.g. multifunctional additives
    • C10N2030/06—Oiliness; Film-strength; Anti-wear; Resistance to extreme pressure
    • C—CHEMISTRY; METALLURGY
    • C10—PETROLEUM, GAS OR COKE INDUSTRIES; TECHNICAL GASES CONTAINING CARBON MONOXIDE; FUELS; LUBRICANTS; PEAT
    • C10N—INDEXING SCHEME ASSOCIATED WITH SUBCLASS C10M RELATING TO LUBRICATING COMPOSITIONS
    • C10N2050/00—Form in which the lubricant is applied to the material being lubricated
    • C10N2050/015—Dispersions of solid lubricants
    • C10N2050/02—Dispersions of solid lubricants dissolved or suspended in a carrier which subsequently evaporates to leave a lubricant coating
    • C—CHEMISTRY; METALLURGY
    • C10—PETROLEUM, GAS OR COKE INDUSTRIES; TECHNICAL GASES CONTAINING CARBON MONOXIDE; FUELS; LUBRICANTS; PEAT
    • C10N—INDEXING SCHEME ASSOCIATED WITH SUBCLASS C10M RELATING TO LUBRICATING COMPOSITIONS
    • C10N2050/00—Form in which the lubricant is applied to the material being lubricated
    • C10N2050/08—Solids

Abstract

<P>PROBLEM TO BE SOLVED: To provide a new carbon nanohorn solid lubricant that can reduce friction and abrasion on the sliding faces at the sliding part in a variety of equipments, micro-machines, biodevice, space device and the like. <P>SOLUTION: The carbon nanohorn solid lubricant contains an aggregate of monolayer carbon nanohorns. <P>COPYRIGHT: (C)2004,JPO

Description

【発明の詳細な説明】Detailed Description of the Invention

【０００１】[0001]

【発明の属する技術分野】この出願の発明は、カーボン
ナノホーン固体潤滑剤に関するものである。さらに詳し
くは、この出願の発明は、各種機器の摺動部や、マイク
ロマシン、生体機器、宇宙機器等における摺動面の摩擦
および摩耗を低減することのできる新しいカーボンナノ
ホーン固体潤滑剤に関するものである。TECHNICAL FIELD The present invention relates to a carbon nanohorn solid lubricant. More specifically, the invention of this application relates to a new carbon nanohorn solid lubricant capable of reducing friction and wear of sliding parts of various devices and sliding surfaces of micromachines, biomedical devices, space devices and the like. .

【０００２】[0002]

【従来の技術とその課題】新しいナノ構造黒鉛（グラフ
ァイト）材料として、フラーレン、単層もしくは多層カ
ーボンナノチューブ、単層カーボンナノホーン集合体等
が様々な分野で注目され、その物性が調べられるととも
に、それらの応用についての研究が数多く成されてい
る。2. Description of the Related Art Fullerene, single-walled or multi-walled carbon nanotubes, single-walled carbon nanohorn aggregates, and the like have attracted attention in various fields as new nanostructured graphite (graphite) materials, and their physical properties have been investigated and Much research has been done on the application of.

【０００３】ところが、これらの炭素材料のトライボロ
ジー性能については、Ｃ60や単層もしくは多層カーボン
ナノチューブについて調べられているのみであって、単
層カーボンナノホーン集合体については未だかつて報告
されていなかった。However, regarding the tribological performance of these carbon materials, only C 60 and single-walled or multi-walled carbon nanotubes have been investigated, and single-walled carbon nanohorn aggregates have never been reported.

【０００４】一方で、近年の加工技術の精密化および集
積化により、いわゆるナノテクノロジーが著しく発展し
てきている。そしてこのナノテクノロジーの環境で使用
されるマイクロマシン、生体機器等においては、ナノメ
ートルオーダーで物体の摩擦および摩耗を低減するため
の潤滑剤が必要とされている。また一方で、最近では宇
宙開発にも用いることのできる真空中で使用可能な固体
潤滑剤の開発が盛んに行われてもいる。On the other hand, so-called nanotechnology has been remarkably developed due to recent refinement and integration of processing techniques. In addition, in the micromachines, biomedical devices and the like used in this nanotechnology environment, a lubricant is required to reduce friction and wear of objects on the order of nanometers. On the other hand, recently, solid lubricants which can be used in space development and can be used in a vacuum have also been actively developed.

【０００５】そこでこの出願の発明は、以上の通りの事
情に鑑みてなされたものであり、単層カーボンナノホー
ン集合体の新たな応用として、一般的な各種機器の摺動
部にはもちろんのこと、マイクロマシン、生体機器、宇
宙機器等における摺動面の摩擦および摩耗を低減するこ
とのできる新しいカーボンナノホーン固体潤滑剤を提供
することを課題としている。Therefore, the invention of this application has been made in view of the circumstances as described above, and as a new application of the single-layer carbon nanohorn aggregate, it is needless to say that it is applied to sliding parts of various general equipment. It is an object of the present invention to provide a new carbon nanohorn solid lubricant capable of reducing friction and wear of sliding surfaces in micromachines, biomedical equipment, space equipment and the like.

【０００６】[0006]

【課題を解決するための手段】そこで、この出願の発明
は、以下の通りの発明を提供する。Therefore, the invention of this application provides the following inventions.

【０００７】すなわち、まず第１には、この出願の発明
は、単層カーボンナノホーン集合体が含有されているこ
とを特徴とするカーボンナノホーン固体潤滑剤を提供す
る。That is, first of all, the invention of this application provides a carbon nanohorn solid lubricant containing a single-layer carbon nanohorn aggregate.

【０００８】そして、この出願の発明は、上記の発明に
ついて、第２には、単層カーボンナノホーン集合体が分
散媒に含有されていることを特徴とするカーボンナノホ
ーン固体潤滑剤を、第３には、単層カーボンナノホーン
集合体が１２００℃以上の温度での熱処理を施されてい
ることを特徴とするカーボンナノホーン固体潤滑剤を、
第４には、膜状体であることを特徴とするカーボンナノ
ホーン固体潤滑剤を提供する。The invention of this application relates to the above invention, secondly, a carbon nanohorn solid lubricant comprising a single-layer carbon nanohorn aggregate in a dispersion medium. Is a carbon nanohorn solid lubricant, wherein the single-layer carbon nanohorn aggregate is subjected to heat treatment at a temperature of 1200 ° C. or higher,
Fourthly, there is provided a carbon nanohorn solid lubricant which is a film-shaped body.

【０００９】[0009]

【発明の実施の形態】この出願の発明は、上記の通りの
特徴を持つものであるが、以下にその実施の形態につい
て説明する。BEST MODE FOR CARRYING OUT THE INVENTION The invention of this application has the characteristics as described above, and the embodiments thereof will be described below.

【００１０】この出願の発明者らは、単層カーボンナノ
ホーン集合体の更なる応用について検討し、トライボロ
ジー性能に着目して研究を重ねた結果、単層カーボンナ
ノホーン集合体の固体潤滑剤としての有用性を見出すに
至った。すなわち、この出願の発明が提供するカーボン
ナノホーン固体潤滑剤は、単層カーボンナノホーン集合
体が含有されていることを特徴とするものである。The inventors of the present application studied further applications of the single-layer carbon nanohorn aggregates, and conducted repeated research focusing on tribological performance. As a result, the single-layer carbon nanohorn aggregates were useful as solid lubricants. I came to find a sex. That is, the carbon nanohorn solid lubricant provided by the invention of this application is characterized by containing a single-layer carbon nanohorn aggregate.

【００１１】単層カーボンナノホーン集合体は、この出
願の発明者らが発見した新しい炭素同素体であって、た
とえば図１（ａ）〜（ｃ）に例示したように、単層カー
ボンナノチューブの一端が角状に閉じた形態の単層カー
ボンナノホーンが、その角状端を外側にして複数が集合
し、全体としては球状の粒子として存在しているもので
ある。この単層カーボンナノホーン集合体には、単層カ
ーボンナノホーンの角状端が外側に突き出ているダリア
型単層カーボンナノホーン集合体や、その表面に角状の
突起が見られずに滑らかな表面を有しているつぼみ型単
層カーボンナノホーン集合体が存在し、この出願の発明
においてはそのいずれをも用いることができる。The single-walled carbon nanohorn aggregate is a new carbon allotrope discovered by the inventors of the present application. For example, as shown in FIGS. 1 (a) to 1 (c), one end of the single-walled carbon nanotube is The single-walled carbon nanohorns in the form of closed horns are present in the form of spherical particles as a whole, with a plurality of the horned ends facing outward. This single-walled carbon nanohorn aggregate has a dahlia type single-walled carbon nanohorn aggregate in which the angular end of the single-walled carbon nanohorn protrudes outward, and a smooth surface without any angular protrusions on the surface. There is a bud type single-walled carbon nanohorn aggregate that has, and any of them can be used in the invention of this application.

【００１２】これらの単層カーボンナノホーン集合体の
大きさについては、代表的には直径が８０〜１００ｎｍ
の範囲内であって、単独の球状粒子もしくは複数の球状
粒子が集合したスス状物質として得ることができる。こ
のような単層カーボンナノホーン集合体は、球状粒子で
あるために転がり特性が期待でき、しかも本来のものと
してナノメートルオーダーの大きさを有している。ま
た、上記のような特徴的な形状によるものかは不確かで
はあるが、基板の材質等に大きな影響を受けることな
く、良好なトライボロジー性能を示すことができる。つ
まり、各種機器等における摺動面の摩擦および摩耗をも
低減することのできる固体潤滑物質として有用なカーボ
ンナノホーン固体潤滑剤が実現されることになる。また
このカーボンナノホーン固体潤滑剤は、ナノメートルオ
ーダーの機器や、宇宙環境に使用される機器等において
も使用することができる。The size of these single-wall carbon nanohorn aggregates is typically 80-100 nm in diameter.
Within the range, a single spherical particle or a soot-like substance in which a plurality of spherical particles are aggregated can be obtained. Since such a single-layer carbon nanohorn aggregate is a spherical particle, rolling characteristics can be expected, and in addition, it has a size of the order of nanometers as it is. Further, although it is uncertain whether it is due to the characteristic shape as described above, good tribological performance can be exhibited without being greatly affected by the material of the substrate and the like. In other words, a carbon nanohorn solid lubricant useful as a solid lubricant that can reduce friction and wear of sliding surfaces in various devices is realized. The carbon nanohorn solid lubricant can also be used in equipment on the order of nanometers, equipment used in the space environment, and the like.

【００１３】この出願の発明のカーボンナノホーン固体
潤滑剤は、本質的には、単層カーボンナノホーン集合体
のみでその潤滑材としての機能を果たすことができる
が、利用の簡便性等を考慮して、たとえば分散媒等に添
加することも可能とされる。この分散媒としては、ベン
ゼン、トルエン、キシレン、ヘキサン、酢酸エチル等の
炭化水素や、メタノール、エタノール、エチレングリコ
ール、グリセリン等のアルコール、エチルエーテル、ジ
エチルエーテル等のエーテル、およびエステル等のその
誘導体等の各種の有機溶媒や、ポリイミド、ポロテトラ
フルオロエチレン（ＰＴＦＥ）、ポリエーテルエーテル
ケトン（ＰＥＥＫ）等の樹脂、水、水ガラス、油や、こ
れらを適宜に混合した混合物等を用いることができる。
これらの分散媒は、潤滑材としてのこのカーボンナノホ
ーン固体潤滑剤の使用においては、基材（摺動面）上に
存在して個々の単層カーボンナノホーン集合体を保持す
るようにしていてもよいし、もしくは予め揮発するなど
して除去されていてもよい。また、分散媒への単層カー
ボンナノホーンの含有量は、用途や目的に応じて適宜調
整することができる。The carbon nanohorn solid lubricant according to the invention of this application can essentially function as a lubricant only by a single-layer carbon nanohorn aggregate, but in consideration of ease of use and the like. It is also possible to add it to, for example, a dispersion medium. Examples of the dispersion medium include hydrocarbons such as benzene, toluene, xylene, hexane and ethyl acetate, alcohols such as methanol, ethanol, ethylene glycol and glycerin, ethers such as ethyl ether and diethyl ether, and derivatives such as esters. Various organic solvents, resins such as polyimide, porotetrafluoroethylene (PTFE) and polyether ether ketone (PEEK), water, water glass, oil, and a mixture of these appropriately mixed can be used.
These dispersion media may be present on the base material (sliding surface) to hold individual single-layer carbon nanohorn aggregates when the carbon nanohorn solid lubricant is used as a lubricant. Alternatively, it may be removed by volatilizing in advance. In addition, the content of the single-layer carbon nanohorn in the dispersion medium can be appropriately adjusted according to the application or purpose.

【００１４】さらにこの出願の発明が提供するカーボン
ナノホーン固体潤滑剤は、単層カーボンナノホーン集合
体が１２００℃以上の温度での熱処理を施されているこ
とを特徴としている。この１２００℃以上の温度での熱
処理は、単層カーボンナノホーン集合体のグラファイト
化を促進するものであって、複数の単層カーボンナノホ
ーン集合体の相互の絡み合いを強固なものにすることが
できる。したがって、たとえば、摺動面の材質、摺動条
件等に応じて、熱処理した単層カーボンナノホーン集合
体と熱処理していない単層カーボンナノホーン集合体と
を使い分けすること等ができ、目的により応じた固体潤
滑剤が提供されることになる。たとえば熱処理された単
層カーボンナノホーン集合体を用いる場合についての具
体的な例をあげると、熱処理された単層カーボンナノホ
ーン集合体を潤滑油等に含有してカーボンナノホーン固
体潤滑剤を調整し、これをブレーキ、クラッチ、無段変
速機等の摺動面などに適用することで、摩擦調整剤とし
て利用することができる。Further, the carbon nanohorn solid lubricant provided by the invention of this application is characterized in that the single-layer carbon nanohorn aggregate is subjected to a heat treatment at a temperature of 1200 ° C. or higher. This heat treatment at a temperature of 1200 ° C. or higher promotes graphitization of the single-layer carbon nanohorn aggregate, and can strengthen the mutual entanglement of the single-layer carbon nanohorn aggregates. Therefore, for example, the heat-treated single-wall carbon nanohorn aggregates and the non-heat-treated single-wall carbon nanohorn aggregates can be selectively used according to the material of the sliding surface, sliding conditions, etc. A solid lubricant will be provided. For example, a specific example of using a heat-treated single-layer carbon nanohorn aggregate includes a heat-treated single-layer carbon nanohorn aggregate in a lubricating oil or the like to prepare a carbon nanohorn solid lubricant. Can be used as a friction modifier by applying to a sliding surface of a brake, a clutch, a continuously variable transmission, or the like.

【００１５】また、ダリア型とつぼみ型の単層カーボン
ナノホーン集合体とにおいても、つぼみ型の単層カーボ
ンナノホーン集合体のほうが摩擦低減効果が高いと考え
られ、このような特徴を活かして固体潤滑剤とすること
も考慮される提供される。Further, among the dahlia-type and bud-type single-wall carbon nanohorn aggregates, the bud-type single-wall carbon nanohorn aggregates are considered to have a higher friction reducing effect. It is also provided that the agent is considered.

【００１６】加えてこの出願の発明が提供するカーボン
ナノホーン固体潤滑剤は、たとえば膜状体等としても実
現することができる。この膜状体の膜厚および面積等に
ついては、任意のものとすることができる。また、前記
の分散媒が存在していても、存在していなくてもよい。
膜状体としてのこの出願の発明のカーボンナノホーン固
体潤滑剤は、その膜厚、大きさ等により各種の方法によ
り実現することができる。たとえば一つの例として、以
下のような方法により簡便に提供されることになる。In addition, the carbon nanohorn solid lubricant provided by the invention of this application can also be realized, for example, as a film. The film thickness, the area, and the like of this film-like body may be arbitrary. Further, the dispersion medium may or may not be present.
The carbon nanohorn solid lubricant of the invention of this application as a film can be realized by various methods depending on its film thickness, size and the like. For example, as one example, it is simply provided by the following method.

【００１７】＜１＞ 単層カーボンナノホーン集合体を
たとえば前記のいずれかの分散媒に分散させ、平滑面上
に塗布し、分散媒を固化あるいは蒸発させた後、平滑面
から単層カーボンナノホーン集合体を剥離し、膜状体と
してのカーボンナノホーン固体潤滑剤を得る。<1> A single-layer carbon nanohorn aggregate is dispersed, for example, in any one of the above dispersion media, coated on a smooth surface, and the dispersion medium is solidified or evaporated, and then the single-wall carbon nanohorn aggregate is formed from the smooth surface. The body is peeled off to obtain a carbon nanohorn solid lubricant as a film.

【００１８】＜２＞ 単層カーボンナノホーン集合体を
たとえば前記のいずれかの分散媒に分散させ、目的とす
る基板（摺動面）上に塗布した後、分散媒を固化あるい
は蒸発させて、基板（摺動面）上に膜状体としてのカー
ボンナノホーン固体潤滑剤を得る。<2> A single-layer carbon nanohorn aggregate is dispersed in, for example, any one of the above-mentioned dispersion media, coated on a target substrate (sliding surface), and then the dispersion medium is solidified or evaporated to form a substrate. On the (sliding surface), a carbon nanohorn solid lubricant as a film is obtained.

【００１９】以上のようなカーボンナノホーン固体潤滑
剤を基板（摺動面）上に作用させることで、摩擦および
摩耗を低減することができる新しい固体潤滑剤が実現さ
れることになる。By applying the above carbon nanohorn solid lubricant on the substrate (sliding surface), a new solid lubricant capable of reducing friction and wear can be realized.

【００２０】以下に実施例を示し、この発明の実施の形
態についてさらに詳しく説明する。Examples will be shown below to describe the embodiments of the present invention in more detail.

【００２１】[0021]

【実施例】この出願の発明のカーボンナノホーン固体潤
滑剤のトライボロジー性能を調べるために摩擦試験を行
なった。試料としては、（ａ）単層カーボンナノホーン
集合体と、（ｂ）加熱処理した単層カーボンナノホーン
集合体を用いた。この（ａ）単層カーボンナノホーン集
合体は、ＣＯ2レーザー蒸発法により作製した、チュー
ブ部の平均直径が２〜３ｎｍ、平均長さ３０〜５０ｎｍ
で、全体としては直径約８０〜１００ｎｍの球状の、ダ
リヤ型単層カーボンナノホーン集合体を用いた。また、
この（ｂ）加熱処理した単層カーボンナノホーン集合体
は、得られた（ａ）単層カーボンナノホーン集合体を１
９６０℃で熱処理してグラファイト化を進行させたもの
を用いた。EXAMPLE A friction test was conducted to investigate the tribological performance of the carbon nanohorn solid lubricant of the invention of this application. As samples, (a) single-layer carbon nanohorn aggregates and (b) heat-treated single-layer carbon nanohorn aggregates were used. This (a) single-layer carbon nanohorn aggregate was produced by the CO 2 laser evaporation method, and the tube portion had an average diameter of 2 to 3 nm and an average length of 30 to 50 nm.
Then, a spherical, single-layer carbon nanohorn aggregate having a diameter of about 80 to 100 nm was used as a whole. Also,
This (b) heat-treated single-walled carbon nanohorn aggregate is obtained by
A material that had been graphitized by heat treatment at 960 ° C. was used.

【００２２】また、比較のために、（ｃ）平均粒径２２
μｍ、０．６μｍの２種類のグラファイト粉末と、
（ｄ）Ｃ60、（ｅ）多層カーボンナノチューブを用い
た。（ｄ）Ｃ60はアーク放電法で作製し、液体クロマト
グラフィーで精製した純度３Ｎのものをめのう乳鉢で粉
砕して使用した。（ｅ）多層カーボンナノチューブは、
炭化水素触媒分解法で作製した、直径１０〜５０ｎｍ、
長さ数μｍの多層カーボンナノチューブの集合体を用い
た。For comparison, (c) average particle size 22
Two kinds of graphite powder of μm and 0.6 μm,
(D) C 60 and (e) multi-walled carbon nanotubes were used. (D) C 60 was produced by an arc discharge method and purified by liquid chromatography and having a purity of 3N was crushed and used in an agate mortar. (E) The multi-walled carbon nanotube is
10 to 50 nm in diameter prepared by a hydrocarbon catalytic decomposition method,
An aggregate of multi-walled carbon nanotubes having a length of several μm was used.

【００２３】摩擦試験片は、上記の試料をそれぞれスラ
イドクラス上でアルコールと混合してペースト状にし、
精製水が入ったシャーレに浸して膜状のペーストを水面
上に浮遊させ、次いでこの浮遊膜を、平均表面粗さ２μ
ｍのＳＵＳ３０４基板上にすくい上げて大気中で仮乾燥
させた後、真空乾燥させて調整した。この試験片の膜厚
は約１０μｍであった。A friction test piece was prepared by mixing each of the above samples with alcohol on a slide class to form a paste,
The membranous paste is suspended on the water surface by immersing it in a petri dish containing purified water, and the floating membrane is then subjected to an average surface roughness of 2 μm.
m SUS304 substrate was scooped up and temporarily dried in the air, and then vacuum dried for adjustment. The film thickness of this test piece was about 10 μm.

【００２４】摩擦試験には、直径３／１６インチのＳＵ
Ｓ３０４ボールを相手に、荷重０．１１Ｎ、速度２５ｃ
ｍ／ｍｉｎの条件の回転摩擦を行なった。摩擦時間は５
０分間（摩擦回数１０００回）とし、雰囲気は相対湿度
２５〜４０％の空気とした。なお、摩擦試験は、同一試
料について３、４回繰り返して行なった。For the friction test, SU with a diameter of 3/16 inch was used.
Against S304 ball, load 0.11N, speed 25c
Rotational friction was performed under the condition of m / min. Friction time is 5
The time was 0 minutes (rubbing frequency 1000 times), and the atmosphere was air with relative humidity of 25 to 40%. The friction test was repeated 3 or 4 times for the same sample.

【００２５】先ず最初に、試験片を載せていないＳＵＳ
３０４基板とＳＵＳ３０４ボールとの間の摩擦係数を調
べた結果、試験初期は０．３程度であったのが、試験終
了時には０．８程度にまで上昇した。試験後の基板とボ
ールの表面を観察したところ、表面が激しく荒れている
のが確認された。First of all, SUS without a test piece
As a result of examining the friction coefficient between the 304 substrate and the SUS304 ball, the friction coefficient was about 0.3 at the beginning of the test, but increased to about 0.8 at the end of the test. When the surfaces of the substrate and the balls after the test were observed, it was confirmed that the surfaces were extremely rough.

【００２６】次に、（ｃ）平均粒径２２μｍ、０．６μ
ｍの２種類のグラファイト粉末の摩擦係数は、試験初期
から０．１程度と低く、試験終了時までほぼ同程度の値
を保っていた。グラファイト粉末（平均粒径０．６μ
ｍ）の摩擦係数を調べた結果の一例を図２に示した。こ
の結果は、従来のグラファイト潤滑材についてのデータ
と一致するものである。またグラファイト粉末の粒径の
違いの影響は摩擦係数の変動に見られ、平均粒径２２μ
ｍの粗いグラファイト粉末のほうが０．６μｍの細かい
のもに比べて変動が小さく安定していた。試験後の基板
とボールの表面を光学顕微鏡で観察した結果を図３に例
示した。基板とボールの摩擦痕にはグラファイトとみら
れる移着物が観察されたが、その移着物を拭き取ったと
ころ、摩耗はほとんど認められなかった。Next, (c) average particle size 22 μm and 0.6 μm
The friction coefficients of the two kinds of graphite powders of m were as low as about 0.1 from the initial stage of the test, and remained almost the same value until the end of the test. Graphite powder (average particle size 0.6μ
An example of the result of examining the friction coefficient of m) is shown in FIG. This result is consistent with the data for conventional graphite lubricants. The effect of the difference in the particle size of graphite powder is seen in the fluctuation of the friction coefficient, and the average particle size is 22μ.
The coarser graphite powder of m had a smaller fluctuation and was more stable than the finer graphite powder of 0.6 μm. The results of observing the surface of the substrate and the ball after the test with an optical microscope are illustrated in FIG. A transfer material that was considered to be graphite was observed in the friction mark between the substrate and the ball, but when the transfer material was wiped off, almost no wear was observed.

【００２７】（ｄ）Ｃ60の摩擦係数は、試験初期には
０．２〜０．３であったが、その値はだいたい時間とと
もに上昇し、試験終了時には０．５５〜０．６５の高い
値となった。ただし、途中、摩擦変動が観察された。Ｃ
60はこの試験においては、最も潤滑性に劣っていた。試
験後の基板とボールの表面を観察したところ、基板とボ
ールの摩擦痕には移着物が観察されたがグラファイトで
はない硬質の物質であった。(D) The coefficient of friction of C 60 was 0.2 to 0.3 at the beginning of the test, but the value increased with time, and was as high as 0.55 to 0.65 at the end of the test. It became a value. However, during the process, friction fluctuation was observed. C
60 was the least lubricious in this test. When the surfaces of the substrate and the balls were observed after the test, transferred substances were observed in the friction marks between the substrate and the balls, but they were hard substances other than graphite.

【００２８】（ｅ）多層カーボンナノチューブについて
は、試験初期の摩擦係数が０．２５〜０．３５であっ
て、試験終了時には０．３５〜０．４５程度となり、こ
の試験においては（ｄ）Ｃ60に次ぐ高い摩擦係数であっ
た。また、（ｄ）Ｃ60と同様に途中に摩擦の変動が多く
みられた。試験後の基板とボールの表面には移着物が観
察され、僅かなボールの摩耗が認められる場合があっ
た。(E) Regarding the multi-walled carbon nanotube, the friction coefficient at the initial stage of the test was 0.25 to 0.35, and at the end of the test it was about 0.35 to 0.45. In this test, (d) C It had the highest friction coefficient after 60 . Also, as in the case of (d) C 60 , there were many fluctuations in friction during the process. Transferred substances were observed on the surface of the substrate and the ball after the test, and slight abrasion of the ball was sometimes observed.

【００２９】一方のこの出願の発明のカーボンナノホー
ン固体潤滑剤に関しては、（ａ）単層カーボンナノホー
ン集合体は、摩擦係数が、試験初期では０．２〜０．１
程度で（ｃ）グラファイト粉末より若干大きめであった
が、すぐにその値は低下し、試験終了時には０．０５〜
０．１程度の範囲で安定して、平均的には（ｃ）グラフ
ァイトより低い値を示した。図４に摩擦係数の変化の一
例を示した。また、試験後の基板とボールの表面を観察
したところ、基板とボールの摩擦痕には移着物が観察さ
れたが、ボールへの移着物は容易に拭きとることがで
き、摩擦痕は全く観察されなかった。図５に光学顕微鏡
による摩擦痕の観察結果を例示した。On the other hand, regarding the carbon nanohorn solid lubricant of the invention of this application, (a) the single-layer carbon nanohorn aggregate has a friction coefficient of 0.2 to 0.1 at the initial stage of the test.
Although it was slightly larger than that of the graphite powder (c), the value immediately decreased, and when the test was completed,
It was stable in the range of about 0.1, and showed an average value lower than that of (c) graphite. FIG. 4 shows an example of changes in the friction coefficient. Also, when the surface of the substrate and the ball after the test was observed, the transferred substance was observed in the friction mark between the substrate and the ball, but the transferred substance to the ball could be easily wiped off, and the friction mark was not observed at all. Was not done. FIG. 5 exemplifies the results of observation of friction marks by an optical microscope.

【００３０】（ｂ）加熱処理した単層カーボンナノホー
ン集合体の摩擦係数は、（ｄ）Ｃ60および（ｅ）多層カ
ーボンナノチューブよりは低いものであったが、（ａ）
単層カーボンナノホーン集合体に比べると全体的にやや
高い値を示した。(B) The friction coefficient of the heat-treated single-walled carbon nanohorn aggregate was lower than that of (d) C 60 and (e) multi-walled carbon nanotube, but (a)
The overall value was slightly higher than that of the single-layer carbon nanohorn aggregate.

【００３１】上記（ａ）〜（ｅ）の平均的摩擦係数を図
６にまとめて示した。この出願の発明のカーボンナノホ
ーン固体潤滑剤である（ａ）は、（ｃ）グラファイト粉
末よりは変動が大きいものの、（ｃ）グラファイト粉末
と同等かそれに勝る低摩擦を示すことが確認された。The average friction coefficients of the above (a) to (e) are summarized in FIG. It has been confirmed that the carbon nanohorn solid lubricant (a) of the invention of the present application exhibits a friction lower than or equal to (c) graphite powder, although it has a larger fluctuation than (c) graphite powder.

【００３２】もちろん、この発明は以上の例に限定され
るものではなく、細部については様々な態様が可能であ
ることは言うまでもない。Of course, the present invention is not limited to the above examples, and it goes without saying that various aspects are possible in details.

【００３３】[0033]

【発明の効果】以上詳しく説明した通り、この発明によ
って、この出願の発明は、各種機器の摺動部や、マイク
ロマシン、生体機器、宇宙機器等における摺動面の摩擦
および摩耗を低減することのできる新しいカーボンナノ
ホーン固体潤滑剤が提供される。As described above in detail, according to the present invention, the invention of the present application can reduce the friction and wear of the sliding parts of various devices and sliding surfaces of micromachines, biomedical devices, space devices and the like. A new carbon nanohorn solid lubricant is provided.

【図面の簡単な説明】[Brief description of drawings]

【図１】（ａ）単層カーボンナノホーン集合体と（ｂ）
単層カーボンナノホーンの先端部の構造を例示した模式
図であり、（ｃ）単層カーボンナノホーン集合体スス状
体の透過型電子顕微鏡像を例示した図である。FIG. 1A is a single-layer carbon nanohorn aggregate and FIG.
It is a schematic diagram which illustrated the structure of the front-end | tip part of single-walled carbon nanohorn, and is the figure which illustrated the transmission electron microscope image of (c) single-walled carbon nanohorn aggregate soot-like body.

【図２】グラファイト粉末（平均粒径０．６μｍ）の摩
擦試験の結果を例示した図である。FIG. 2 is a diagram illustrating an example of a result of a friction test of graphite powder (average particle size: 0.6 μm).

【図３】グラファイト粉末（平均粒径０．６μｍ）によ
る摩擦試験後の基板とボールの表面を光学顕微鏡で観察
した結果を例示した図である。FIG. 3 is a diagram illustrating the results of observing the surfaces of a substrate and balls after a friction test with graphite powder (average particle size 0.6 μm) with an optical microscope.

【図４】単層カーボンナノホーン集合体の摩擦試験の結
果を例示した図である。FIG. 4 is a diagram illustrating the results of a friction test of a single-layer carbon nanohorn aggregate.

【図５】単層カーボンナノホーン集合体による摩擦試験
後の基板とボールの表面を光学顕微鏡で観察した結果を
例示した図である。FIG. 5 is a diagram illustrating the results of observing the surfaces of a substrate and balls after a friction test with a single-layer carbon nanohorn aggregate with an optical microscope.

【図６】各材料の平均的摩擦係数を例示した図である。FIG. 6 is a diagram illustrating an average friction coefficient of each material.

フロントページの続き (72)発明者 飯島 澄男 愛知県名古屋市天白区平針 １−1110− 402 (72)発明者 湯田坂 雅子 茨城県つくば市東光台２−８−３ (72)発明者 梅田 一徳 茨城県つくば市小野川８−21 (72)発明者 田中 章浩 茨城県土浦市湖北１−９−19 Ｆターム(参考） 4H104 AA04C QA11 QA12 QA16Continued front page    (72) Inventor Sumio Iijima             1-111 Hiranari, Tenpaku-ku, Nagoya-shi, Aichi             402 (72) Inventor Masako Yudasaka             2-8-3 Tokodai, Tsukuba City, Ibaraki Prefecture (72) Inventor Kazunori Umeda             8-21 Onogawa, Tsukuba City, Ibaraki Prefecture (72) Inventor Akihiro Tanaka             1-9-19 Hubei, Tsuchiura City, Ibaraki Prefecture F-term (reference) 4H104 AA04C QA11 QA12 QA16

Claims (4)

【特許請求の範囲】[Claims] 【請求項１】 単層カーボンナノホーン集合体が含有さ
れていることを特徴とするカーボンナノホーン固体潤滑
剤。1. A carbon nanohorn solid lubricant containing a monolayer carbon nanohorn aggregate. 【請求項２】 単層カーボンナノホーン集合体が分散媒
に含有されていることを特徴とする請求項１記載のカー
ボンナノホーン固体潤滑剤。2. The carbon nanohorn solid lubricant according to claim 1, wherein the single-layer carbon nanohorn aggregate is contained in the dispersion medium. 【請求項３】 単層カーボンナノホーン集合体が１２０
０℃以上の温度での熱処理を施されていることを特徴と
する請求項１または２記載のカーボンナノホーン固体潤
滑剤。3. A single-layer carbon nanohorn aggregate is 120
The carbon nanohorn solid lubricant according to claim 1 or 2, which has been heat-treated at a temperature of 0 ° C or higher. 【請求項４】 膜状体であることを特徴とする請求項１
ないし３いずれかに記載のカーボンナノホーン固体潤滑
剤。4. The film-shaped body according to claim 1,
4. The carbon nanohorn solid lubricant according to any one of 1 to 3.
JP2002118500A 2002-04-19 2002-04-19 Carbon nanohorn solid lubricant Pending JP2003313571A (en)

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PCT/JP2003/004181 WO2003089552A1 (en) 2002-04-19 2003-04-01 Carbon nano-horn solid lubricant

Applications Claiming Priority (1)

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