JP7152561B2 - A Method for Realizing Super Lubrication on a Macroscopic Scale by Forming a Pair System with a Hydrogen-Containing Carbon Film and Molybdenum Disulfide - Google Patents

A Method for Realizing Super Lubrication on a Macroscopic Scale by Forming a Pair System with a Hydrogen-Containing Carbon Film and Molybdenum Disulfide Download PDF

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JP7152561B2
JP7152561B2 JP2021100443A JP2021100443A JP7152561B2 JP 7152561 B2 JP7152561 B2 JP 7152561B2 JP 2021100443 A JP2021100443 A JP 2021100443A JP 2021100443 A JP2021100443 A JP 2021100443A JP 7152561 B2 JP7152561 B2 JP 7152561B2
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俊彦 ▲張▼
倩 ▲賈▼
斌 ▲張▼
元烈 于
▲凱▼雄 高
振国 ▲頼▼
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中国科学院蘭州化学物理研究所
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    • C23—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; CHEMICAL SURFACE TREATMENT; DIFFUSION TREATMENT OF METALLIC MATERIAL; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL; INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL
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    • C23C16/00—Chemical coating by decomposition of gaseous compounds, without leaving reaction products of surface material in the coating, i.e. chemical vapour deposition [CVD] processes
    • C23C16/22—Chemical coating by decomposition of gaseous compounds, without leaving reaction products of surface material in the coating, i.e. chemical vapour deposition [CVD] processes characterised by the deposition of inorganic material, other than metallic material
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Description

本発明は水素含有炭素膜と二硫化モリブデンでペアシステムを形成することにより巨視的スケールにおける超潤滑を実現する方法を提供し、膜堆積と表面保護の分野に属する。 The present invention provides a method for achieving superlubrication on a macroscopic scale by forming a pair system with a hydrogen-containing carbon film and molybdenum disulfide, and belongs to the field of film deposition and surface protection.

機械的摩耗による経済的損失はＧＤＰの５％～７％と高く、それによる損失は数兆元にのぼる。高性能潤滑材技術を使用すれば、自動車の摩擦損失を１８％削減することが期待される。現代の航空宇宙機は、１５年ひいては３０年の動作寿命が要求されており、可動部品の耐摩耗性に対する要求は高まりつつある。ただし、航空宇宙部品の可動部品の性能は依然として改善する必要があり、これは航空宇宙機全体の長期的かつ安定的な作動にとって非常に重要である。 The economic loss due to mechanical wear is as high as 5% to 7% of GDP, and the resulting loss amounts to several trillion yuan. The use of high performance lubricant technology is expected to reduce automotive friction losses by 18%. Modern aerospace vehicles are required to operate for 15 or even 30 years, and the demands on the wear resistance of moving parts are increasing. However, the performance of moving parts in aerospace components still needs to be improved, which is very important for the long-term and stable operation of the entire aerospace vehicle.

アモルファスカーボンフィルムは、摩耗減少と耐摩耗の特性があり、航空宇宙への用途の可能性があり、ベアリングやその他の航空宇宙機のトランスミッションコンポーネントでの使用が期待されている。しかし、従来のアモルファスカーボンフィルムは、単一の環境（Ｎ２と真空）のみで、超潤滑と低摩耗を実現し、高い耐摩耗性を備えているが、空気中では０．０４に達し、寿命は短くなる。 Amorphous carbon films, with wear-reducing and wear-resistant properties, have potential aerospace applications and are expected to be used in bearings and other aerospace transmission components. However, the conventional amorphous carbon film achieves super lubrication and low wear only in a single environment (N2 and vacuum), and has high wear resistance, but in air it reaches 0.04 and the life becomes shorter.

本発明の目的は、アモルファスカーボンフィルムの空気中における耐摩耗性が低いという問題を解決することであり、大気中の炭素膜の適用問題を解決するために、水素含有炭素膜と二硫化モリブデンでペアシステムを形成することにより巨視的スケールにおける超潤滑を実現する方法を提供する。 The purpose of the present invention is to solve the problem that the wear resistance of amorphous carbon films in air is low. We provide a method to achieve superlubrication on a macroscopic scale by forming a pair system.

本発明は、水素含有炭素膜と二硫化モリブデン膜の特性により、水素含有炭素膜と二硫化モリブデンでペアシステムを形成し、摩擦界面の調整及び制御により、大気中の炭素膜の巨視的スケールにおける超潤滑を実現する。 According to the characteristics of the hydrogen-containing carbon film and molybdenum disulfide film, the present invention forms a pair system with the hydrogen-containing carbon film and molybdenum disulfide film, and adjusts and controls the friction interface to achieve the macroscopic scale of the carbon film in the atmosphere. Achieve super lubrication.

前記水素含有炭素膜は、マイクロ波表面波プラズマの化学気相成長法によって調製されることができ、水素含有炭素膜の水素含有量が２０～２６％、厚さが７００～９００ｎｍである。 The hydrogen-containing carbon film can be prepared by microwave surface wave plasma chemical vapor deposition, and the hydrogen content of the hydrogen-containing carbon film is 20-26% and the thickness is 700-900 nm.

前記二硫化モリブデンは高出力バイポーラマイクロインパルス反応マグネトロンスパッタリングによって調製される。二硫化モリブデン膜の厚さが５００～７００ｎｍである。 Said molybdenum disulfide is prepared by high power bipolar micro-impulse reactive magnetron sputtering. The thickness of the molybdenum disulfide film is 500-700 nm.

二硫化モリブデン膜は、大気中の摩擦係数が比較的に大きく（０．０５）、耐摩耗性に劣るほか、従来の二硫化モリブデン膜は、鋼表面への結合力が低く、摩擦時に脱落しやすい。水素含有炭素膜と二硫化モリブデン膜を相互にマッチングペアさせて、摩擦時に、摩擦剪断力の作用下で無秩序な二硫化モリブデンは摩擦方向に沿って秩序的に配置されるようになって、炭素膜基板の表面に、少ない数の層を持つ二硫化モリブデンの秩序的な構造がその場で形成されて、炭素膜の巨視的スケールにおける超潤滑を実現する。図１は、ＭｏＳ２摩擦ペアがスライドした後の膜摩耗痕の断面の高解像度写真である。摩擦中に、摩擦剪断力の作用下で無秩序な二硫化モリブデンは摩擦方向に沿って秩序的に配置されるようになって、少ない数の層を持つ秩序的な構造を形成し、摩擦界面の調整及び制御により、大気中の炭素膜の巨視的スケールにおける超潤滑を実現した。実験では、酸素が豊富な環境での当該システムの摩擦係数と耐摩耗性がより優れていることが示された。 The molybdenum disulfide film has a relatively large coefficient of friction in the atmosphere (0.05) and is inferior in wear resistance. Cheap. By matching the hydrogen-containing carbon film and the molybdenum disulfide film to each other, during friction, under the action of frictional shear force, the disordered molybdenum disulfide film is arranged in an orderly manner along the friction direction, and the carbon An ordered structure of molybdenum disulfide with a small number of layers is formed in situ on the surface of the film substrate to achieve macroscopic-scale superlubrication of the carbon film. FIG. 1 is a high-resolution photograph of a cross-section of a film wear scar after sliding MoS2 friction pairs . During friction, the disordered molybdenum disulfide becomes arranged in an ordered manner along the friction direction under the action of frictional shear force, forming an ordered structure with a small number of layers, and the friction interface. Through tuning and control, we have achieved superlubrication on a macroscopic scale in atmospheric carbon films. Experiments have shown that the system has better coefficient of friction and wear resistance in an oxygen-rich environment.

摩擦マッチングペアとして、水素含有炭素膜を堆積した鋼ブロックと二硫化モリブデン膜を堆積した金属球を使用し、サンプルをＣＳＭ摩擦摩耗試験機に固定した後、実験パラメータを負荷９Ｎ、周波数５Ｈｚ、振幅５ｍｍ、摩擦時間３０分間に設定し、室温で摩擦を行う。乾燥された空気を導入して、空気の湿度を徐々に５％以下に下げてから、実験を開始する。得られた摩擦係数は、急速に０．００５程度まで減少した。摩擦と摩耗が大幅に減少し、乾燥された大気中の炭素膜の耐用時間が向上された。即ち、酸素が豊富な環境で当該システムの摩擦係数と耐摩耗性は、より優れている。 A steel block deposited with a hydrogen-containing carbon film and a metal ball deposited with a molybdenum disulfide film were used as friction matching pairs. 5 mm, friction time 30 minutes, friction at room temperature. Dry air is introduced to gradually reduce the humidity of the air to 5% or less before starting the experiment. The resulting coefficient of friction decreased rapidly to around 0.005. Friction and wear are greatly reduced, and the service life of carbon films in dry air is improved. That is, the friction coefficient and wear resistance of the system are better in an oxygen-rich environment.

利点は、高出力マイクロパルス技術を使用して、二硫化モリブデン膜の構造を秩序的になるように制御することにより、摩擦係数が０．０５レベルである２つの摩擦膜材料は、相互カプリングした後に、摩擦係数が０．００５に減少することである。 The advantage is that by using high-power micropulse technology to control the structure of the molybdenum disulfide film to be ordered, the two friction film materials with friction coefficients at the level of 0.05 are mutually coupled. Later, the coefficient of friction is reduced to 0.005.

ＭｏＳ２摩擦ペアがスライドした後の膜摩耗痕の断面の高解像度写真。A high-resolution photograph of the cross-section of the film wear scar after sliding MoS2 friction pairs .

本発明の巨視的スケールにおける超潤滑を実現するための方法は、特定の実施形態を通じて以下にさらに説明される。 The method for achieving superlubrication at the macroscopic scale of the present invention is further described below through specific embodiments.

（１）水素含有炭素膜の調製
ａ．基板材料（高研磨軸受鋼、金型鋼、歯車鋼など）をアルコールで予め２０分間超音波処理し、洗浄し、窒素で乾燥させ、コーティング真空チャンバーに入れてコーティングの準備をした；
ｂ．真空チャンバーを１０－４Ｐａに排気した後、プラズマ化学気相成長装置で８００Ｖの電圧と２．５Ｐａの圧力で、アルゴンガスを通過させてシリコンウェーハの表面に２０分間衝撃を与え、シリコンウェーハ表面の不純物を除去した；
ｃ．水素含有炭素膜の調製：双極対称パルスを使用してプラズマを励起し、パルス電圧が８００Ｖ、デューティ比が５５％、周波数が２０－４０ＫＨｚ、メタン、水素、アルゴンの流量比が１：１：１、圧力が５Ｐａに維持され、プレート間の距離が２５ｍｍであり、堆積時間が９０分間であり、１．１ミクロンの厚さの水素含有炭素膜が得られた。水素含有炭素膜の摩擦係数は０．０１８である；
（２）二硫化モリブデン膜の調製
ａ．直径６ｍｍのＧＣｒ１５、またはステンレス鋼球を使用して、アルコール中で１０分間超音波洗浄した。
ｂ．プラズマ化学気相成長／マグネトロンスパッタリング装置で、プラズマ気相成長法を使用して、事前に処理されたステンレス鋼表面に遷移層を形成し、次に遷移層に高出力マイクロパルスマグネトロンスパッタリングを使用して、二硫化モリブデン層を調製した。具体的には、マイクロパルスは非対称モードを使用し、負のパルス電圧が６５０Ｖ、パルス幅が６００マイクロ秒、マイクロパルス列波のデューティ比が３０％、パルス列波内周波数が１５ＫＨｚ、デューティ比が４％調整可能である。負のパルス電圧は３００Ｖで、他のパラメータは同じで変化しない。まず、アルゴンとメタンの比率を１：２で３０分間堆積し；メタンをオフにして、１時間堆積し、鋼球の表面に厚さ８００ミクロンの二硫化モリブデン膜が得られた。二硫化モリブデン膜の摩擦係数は０．０５である；
（３）炭素膜を堆積した鋼ブロックと二硫化モリブデン膜を堆積した金属球を摩擦マッチングペアとして使用した。ＣＳＭ摩擦摩耗試験機に、サンプルを固定した後、実験パラメータが負荷９Ｎ、周波数５Ｈｚ、振幅５ｍｍ、摩擦時間３０分間、および室温での摩擦を設定した。乾燥された空気を導入して、空気の湿度を徐々に５％以下に下げてから、実験を開始した。得られた摩擦係数は、急速に約０．００５まで減少した。 (1) Preparation of hydrogen-containing carbon film a. Substrate materials (highly polished bearing steel, mold steel, gear steel, etc.) were pre-sonicated with alcohol for 20 minutes, cleaned, dried with nitrogen and placed in a coating vacuum chamber ready for coating;
b. After the vacuum chamber was evacuated to 10 −4 Pa, the surface of the silicon wafer was impacted for 20 minutes by passing argon gas at a voltage of 800 V and a pressure of 2.5 Pa in a plasma chemical vapor deposition apparatus to give a shock to the surface of the silicon wafer. of impurities;
c. Preparation of hydrogen-containing carbon films: Bipolar symmetrical pulses are used to excite plasma, pulse voltage is 800V, duty ratio is 55%, frequency is 20-40KHz, flow ratio of methane, hydrogen and argon is 1:1:1. , the pressure was maintained at 5 Pa, the distance between the plates was 25 mm, the deposition time was 90 minutes, and a hydrogen-containing carbon film with a thickness of 1.1 microns was obtained. The coefficient of friction of the hydrogen-containing carbon film is 0.018;
(2) Preparation of molybdenum disulfide film a. A 6 mm diameter GCr15, or stainless steel ball was used and ultrasonically cleaned in alcohol for 10 minutes.
b. A plasma-enhanced chemical vapor deposition/magnetron sputtering apparatus uses plasma vapor deposition to form a transition layer on a pretreated stainless steel surface, and then uses high-power micropulse magnetron sputtering on the transition layer. to prepare a molybdenum disulfide layer. Specifically, the micropulse uses an asymmetric mode, the negative pulse voltage is 650 V, the pulse width is 600 microseconds, the duty ratio of the micropulse train wave is 30%, the frequency in the pulse train wave is 15 KHz, and the duty ratio is 4%. Adjustable. The negative pulse voltage is 300V and the other parameters remain the same. First, a 1:2 ratio of argon to methane was deposited for 30 minutes; the methane was turned off and deposition was performed for 1 hour, resulting in an 800 micron thick molybdenum disulfide film on the surface of the steel ball. The friction coefficient of molybdenum disulfide film is 0.05;
(3) A steel block deposited with a carbon film and a metal ball deposited with a molybdenum disulfide film were used as friction matching pairs. After fixing the sample in the CSM friction wear tester, the experimental parameters were set to load 9 N, frequency 5 Hz, amplitude 5 mm, friction time 30 minutes, and friction at room temperature. Dry air was introduced to gradually reduce the humidity of the air to below 5% before the experiment was started. The resulting coefficient of friction decreased rapidly to about 0.005.

Claims (5)

水素含有炭素膜と二硫化モリブデン堆積薄膜でペアシステムが形成され、摩擦時に摩擦剪断力および摩擦熱の作用下で無秩序な二硫化モリブデンは秩序な二次元構造を形成し、界面の調整及び制御により、大気中の炭素膜の巨視的スケールにおける超潤滑を実現するとこを特徴とする水素含有炭素膜と二硫化モリブデンでペアシステムを形成することにより巨視的スケールにおける超潤滑を実現する方法。 A pair system is formed by the hydrogen-containing carbon film and the molybdenum disulfide deposited thin film , and the disordered molybdenum disulfide forms an ordered two-dimensional structure under the action of frictional shear force and frictional heat during friction. A method for realizing super lubrication on a macroscopic scale by forming a pair system with a hydrogen-containing carbon film and molybdenum disulfide, characterized by realizing super lubrication on a macroscopic scale of a carbon film in the atmosphere. 前記水素含有炭素膜は、マイクロ波表面波プラズマの化学気相成長法によって調製されることを特徴とする請求項１に記載の水素含有炭素膜と二硫化モリブデンでペアシステムを形成することにより巨視的スケールにおける超潤滑を実現する方法。 The hydrogen-containing carbon film and molybdenum disulfide according to claim 1, wherein the hydrogen-containing carbon film is prepared by microwave surface wave plasma chemical vapor deposition. How to achieve super lubrication on a large scale. 前記水素含有炭素膜は、水素含有量が２０～２６％、厚さが７００～９００ｎｍであることを特徴とする請求項１又は２に記載の水素含有炭素膜と二硫化モリブデンでペアシステムを形成することにより巨視的スケールにおける超潤滑を実現する方法。 The hydrogen-containing carbon film and molybdenum disulfide form a pair system according to claim 1 or 2, wherein the hydrogen-containing carbon film has a hydrogen content of 20 to 26% and a thickness of 700 to 900 nm. A method to achieve superlubrication on a macroscopic scale by 前記二硫化モリブデン堆積薄膜が高出力バイポーラマイクロインパルス反応マグネトロンスパッタリングによって調製されることを特徴とする請求項１に記載の水素含有炭素膜と二硫化モリブデンでペアシステムを形成することにより巨視的スケールにおける超潤滑を実現する方法。 2. The molybdenum disulfide deposited thin film is prepared by high power bipolar micro-impulse reactive magnetron sputtering. How to achieve super lubrication. 前記二硫化モリブデン堆積薄膜は厚さが５００～７００ｎｍであることを特徴とする請求項１～４のいずれか１項に記載の水素含有炭素膜と二硫化モリブデンでペアシステムを形成することにより巨視的スケールにおける超潤滑を実現する方法。 By forming a pair system with a hydrogen-containing carbon film and molybdenum disulfide according to any one of claims 1 to 4, wherein the molybdenum disulfide deposited thin film has a thickness of 500 to 700 nm. A method for achieving superlubrication on a macroscopic scale.
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