JP6096065B2 - Manufacturing method of sliding member - Google Patents
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Description
本発明は、摺動部材の製造方法に関する。 The present invention relates to a method for manufacturing a sliding member .
ダイヤモンドライクカーボン（ＤＬＣ）膜は優れたトライボロジー特性を示す。このため、従来から様々な分野で注目されている。ＤＬＣ膜と鋼材の摺動では摩擦粉に起因する移着膜が低摩擦化に寄与することが示唆されている。また、低摩擦を示す移着膜では，最表面にＤＬＣ由来のグラファイト化されたカーボンが生成されており，低硬度カーボン移着物が低摩擦の要因と考えられている。 Diamond-like carbon (DLC) films exhibit excellent tribological properties. For this reason, it has been attracting attention in various fields. It has been suggested that the transfer film caused by the friction powder contributes to the reduction of friction in sliding between the DLC film and the steel material. Further, in the transfer film showing low friction, graphitized carbon derived from DLC is generated on the outermost surface, and the low hardness carbon transfer product is considered to be a factor of low friction.
シリコンを添加したＳｉ−ＤＬＣ膜に酸素プラズマ処理を施すと、シリコン酸化物がカーボン移着物を固着させるバインダーの役割を果たし、低摩擦化することが報告されている。このように、低摩擦化を実現するためには低硬度カーボンの生成とともに移着膜の固着性が重要となる。 It has been reported that when an oxygen plasma treatment is performed on a Si-DLC film to which silicon is added, silicon oxide serves as a binder for fixing the carbon transfer material and lowers the friction. As described above, in order to realize low friction, the adhesion of the transfer film is important along with the generation of low hardness carbon.
一方、サブミクロンの周期ピッチと溝深さをもつグレーティング状の周期構造をＤＬＣ膜に付与すると、摺動時にＤＬＣ膜と鋼材の微細な摩耗粉が生成され、マイルド摩耗面に似た滑らかで強固に固着した移着膜の形成が期待できる。 On the other hand, when a grating-like periodic structure having a submicron periodic pitch and groove depth is applied to the DLC film, fine wear powder of the DLC film and the steel material is generated during sliding, which is smooth and strong similar to a mild wear surface. The formation of a transfer film adhered to the substrate can be expected.
ＤＬＣの摩擦特性を向上させるために、基材の摺動面に成膜されたＤＬＣ膜に、フェムト秒レーザ等を照射することで、照射領域をガラス状炭素に改質された改質領域を形成するようにした摺動材（摺動部材）が従来においては提案されている（特許文献１及び特許文献２）。 In order to improve the friction characteristics of DLC, a DLC film formed on the sliding surface of the base material is irradiated with a femtosecond laser or the like, so that the irradiation region is modified to glassy carbon. Conventionally proposed sliding materials (sliding members) are formed (Patent Document 1 and Patent Document 2).
また、従来には、基材の表面に、水素を含有した非晶質炭素被膜を成膜する工程と、非晶質炭素被膜の表面に紫外線を照射する工程とで、摺動部材を製造するものもある（特許文献３）。 Conventionally, a sliding member is manufactured by a process of forming an amorphous carbon film containing hydrogen on the surface of a substrate and a process of irradiating the surface of the amorphous carbon film with ultraviolet rays. There is also a thing (patent document 3).
前記特許文献１及び特許文献２に示すものでは、ＤＬＣ層を形成した後、そのＤＬＣ層の表面にレーザ照射するものであり、特許文献３では、ＤＬＣ層を形成した後、そのＤＬＣ層の表面に紫外線を照射するものである。このため、レーザ照射等によって、ＤＬＣをグラファイト化していることになり、ＤＬＣ本来の物性が損なわれることになる。また、長期に渡る使用によって、改質層が消滅すれば、摺動部材としての機能を損なうことになっていた。 In Patent Document 1 and Patent Document 2, after the DLC layer is formed, the surface of the DLC layer is irradiated with laser. In Patent Document 3, after the DLC layer is formed, the surface of the DLC layer is formed. Is irradiated with ultraviolet rays. For this reason, DLC is graphitized by laser irradiation or the like, and the original physical properties of DLC are impaired. Further, if the modified layer disappears after long-term use, the function as the sliding member is impaired.
本発明は、上記課題に鑑みて、周期構造が消滅した後の長期に渡って摺動特性が損なうことがない摺動部材及びこのような摺動部材を製造することができる製造方法を提供する。 In view of the above problems, the present invention provides a sliding member that does not impair sliding characteristics over a long period after the periodic structure disappears, and a manufacturing method that can manufacture such a sliding member. .
本発明の摺動部材の製造方法は、第１部材の摺動面に、凸部頂点が非平坦面となって連続的に高さが変化するグレーティング状凹凸の周期構造を有する非晶質炭素膜を形成する膜形成工程と、第１部材の摺動面と第２部材の摺動面とを相対的に摺動させて，前記周期構造を犠牲層として摩滅させ、かつ、前記非晶質炭素膜から発生する摩耗粉をグラファイト化させて低硬度カーボンを生成させるとともに第２部材からも摩耗粉を発生させて移着層を形成する摩耗工程とを備えたものである。 The method for manufacturing a sliding member according to the present invention includes an amorphous carbon having a periodic structure of grating-like irregularities in which the height of a convex portion is a non-flat surface and the height continuously changes on the sliding surface of the first member. A film forming step for forming a film, a sliding surface of the first member and a sliding surface of the second member are relatively slid to wear the periodic structure as a sacrificial layer , and the amorphous And a wear process in which the wear powder generated from the carbon film is graphitized to generate low-hardness carbon and the transfer powder is generated from the second member to form a transfer layer .
本発明の摺動部材の製造方法によれば、連続的に高さが変化するグレーティング状凹凸の周期構造を非晶質炭素膜（ＤＬＣ膜）に設けているため、摺動時に小さな曲率半径をもつ周期構造先端が摩耗し、なじみが進行する。この際，第１部材から発生する微細なＤＬＣ膜の摩耗粉はグラファイト化され、低摩擦化の実現に重要な低硬度カーボンの生成が促進される。周期構造を有するＤＬＣ膜は微細な加工ツールとして作用し、第２部材からもマイルド摩耗粉のような微細な摩耗粉が発生する。また，周期構造は第２部材に形成される突出した移着粒子を削り落とし、トラップすることで移着粒子の成長を抑制し、摩耗粉の微細化と移着膜の平滑化に寄与する。この段階では顕著な摩擦低減効果は得られないが、周期構造を犠牲層として摩滅させる工程において、微細な摩耗粉が延しつぶされる。 According to the manufacturing method of the sliding member of the present invention, since the periodic structure of the grating-like irregularities whose height continuously changes is provided in the amorphous carbon film (DLC film), a small radius of curvature is provided when sliding. The tip of the periodic structure that it has wears away, and familiarity progresses. At this time, the wear powder of the fine DLC film generated from the first member is graphitized, and the generation of low-hardness carbon important for realizing low friction is promoted. The DLC film having a periodic structure acts as a fine processing tool, and fine wear powder such as mild wear powder is generated from the second member. Further, the periodic structure scrapes off the protruding transfer particles formed on the second member and traps them to suppress the growth of transfer particles, thereby contributing to the refinement of wear powder and the smoothing of the transfer film. At this stage, a significant friction reducing effect cannot be obtained, but fine wear powder is crushed in the process of wearing the periodic structure as a sacrificial layer.
前記非晶質炭素膜は、前記第１部材の基材表面に予め凸部頂点が非平坦面となって連続的に高さが変化するグレーティング状の凹凸の周期構造形成を行った後、成膜して形成するのが好ましい。 The amorphous carbon film is formed on the surface of the base material of the first member after forming a periodic structure of grating-like irregularities whose convex vertices are non-flat surfaces and the height continuously changes. The film is preferably formed.
このように構成することで、形態が異なるだけで通常のＤＬＣ膜と組成的には同一な周期構造を有するＤＬＣ膜を形成できる。 With this configuration, it is possible to form a DLC film having a periodic structure that is compositionally identical to that of a normal DLC film only in the form.
前記第２部材の少なくとも摺動面が、前記摩耗工程において酸化物の摩耗粉を生じる材質としているのが好ましい。 It is preferable that at least the sliding surface of the second member is made of a material that generates oxide wear powder in the wear process.
前記第１部材の基材表面にあらかじめ形成する周期構造は、加工闘値近傍の照射強度で直線偏光のレーザを照射し、その照射部分をオーバーラップさせながら走査して、自己組織的に形成されているのが好ましい。 The periodic structure formed in advance on the substrate surface of the first member is formed in a self-organized manner by irradiating a linearly polarized laser beam with an irradiation intensity in the vicinity of the processing threshold value and scanning while overlapping the irradiated portions. It is preferable.
凸部頂点が非平坦面となって連続的に高さが変化するグレーティング状凹凸の周期構造を有する非晶質炭素膜の凹凸が２０ｎｍ以上１００ｎｍ以下かつ非晶質炭素膜の膜厚以下であるのが好ましい。 The unevenness of the amorphous carbon film having a periodic structure of grating-like unevenness in which the height of the convex part is a non-flat surface and continuously changes in height is 20 nm or more and 100 nm or less and the film thickness of the amorphous carbon film or less. Is preferred.
凸部頂点が非平坦面となって連続的に高さが変化するグレーティング状凹凸の周期構造を有する非晶質炭素膜の周期ピッチが１０μｍ以下であるのが好ましい。 It is preferable that the periodic pitch of the amorphous carbon film having a periodic structure of grating-like irregularities in which the height of the convex portion is a non-flat surface and the height continuously changes is 10 μm or less.
本発明の摺動部材の製造方法では、周期構造を犠牲層として摩滅させる工程において、微細な摩耗粉が延しつぶされ、強固に固着された低硬度カーボン移着層が形成されるとともにＤＬＣ膜が平滑化する。このため、周期構造が消滅した後も長期に渡って摺動特性が向上する摺動部材が得られる。 In the manufacturing method of the sliding member of the present invention, in the step of wearing the periodic structure as a sacrificial layer, fine wear powder is crushed to form a firmly fixed low-hardness carbon transfer layer and a DLC film. Becomes smooth. For this reason, even after the periodic structure disappears, a sliding member having improved sliding characteristics over a long period of time can be obtained.
グレーティング状の凹凸の周期構造形成を行った後、非晶質炭素膜を成膜するものでは、形態が異なるだけで通常のＤＬＣ膜と組成的には同一な周期構造を有するＤＬＣ膜を形成できる。したがって、硬度低下などの物性変化を生じることなく、ＤＬＣ膜本来の特性を維持したものとなる。なお、ＤＬＣ膜の硬度が低下すると、ＤＬＣ膜の微細な加工ツールとしての作用が低下し、移着粒子の成長抑制や摩耗粉の微細化に支障が生じるため、周期構造が消滅した後も長期に渡って摺動特性が向上する摺動部材が得られない。 In the case of forming an amorphous carbon film after forming a grating-like irregular periodic structure, a DLC film having a periodic structure that is compositionally identical to that of a normal DLC film can be formed only in the form. . Therefore, the original characteristics of the DLC film are maintained without causing changes in physical properties such as a decrease in hardness. When the hardness of the DLC film is reduced, the function of the DLC film as a fine processing tool is reduced, which hinders the growth of transfer particles and the miniaturization of wear powder. Thus, a sliding member with improved sliding characteristics cannot be obtained.
第２部材の摺動面が摩耗工程において酸化物の摩耗粉を生じるものでは、酸素に富んだ微細な摩耗粉が延しつぶされて、摩耗率がシビア摩耗の１／２０〜１／１０００となるマイルド摩耗面のような移着層を形成することができる。マイルド摩耗面のような移着層は強固にカーボン移着物を第２部材の摺動面に固着させるバインダーの働きをして、摺動特性向上に寄与する。 When the sliding surface of the second member generates oxide wear powder in the wear process, the fine wear powder rich in oxygen is crushed and the wear rate is 1/20 to 1/1000 of severe wear. A transfer layer such as a mild wear surface can be formed. The transfer layer such as the mild wear surface acts as a binder that firmly fixes the carbon transfer material to the sliding surface of the second member, and contributes to the improvement of the sliding characteristics.
加工闘値近傍の照射強度で 直線偏光のレーザを照射し、その照射部分をオーバーラップさせながら走査して、自己組織的に形成するものでは、機械加工では困難なサブミクロンの周期ピッチと凹凸深さをもつ周期構造を容易に得ることができる。 With a linearly polarized laser beam irradiated at an irradiation intensity in the vicinity of the processing threshold, and scanning with overlapping irradiation parts, it is difficult to machine with submicron periodic pitch and uneven depth, which is difficult to machine. A periodic structure having a thickness can be obtained easily.
非晶質炭素膜（ＤＬＣ膜）の凹凸が２０ｎｍ以上１００ｎｍ以下かつ非晶質炭素膜の膜厚以下とすることで、微細な摩耗粉の発生と周期構造の摩滅を基材が露出することなく効率的に実現できる。 By making the unevenness of the amorphous carbon film (DLC film) 20 nm or more and 100 nm or less and less than the film thickness of the amorphous carbon film, generation of fine wear powder and abrasion of the periodic structure are not exposed. Can be realized efficiently.
非晶質炭素膜（ＤＬＣ膜）の周期ピッチを１０μｍ以下とすることで，低硬度カーボンの生成促進と移着粒子の成長抑制により，マイルド摩耗面に似た移着層を形成することができる。 By setting the periodic pitch of the amorphous carbon film (DLC film) to 10 μm or less, a transfer layer resembling a mild wear surface can be formed by promoting the generation of low hardness carbon and suppressing the growth of transfer particles. .
以下本発明の実施の形態を図１〜図２１に基づいて説明する。 Hereinafter, embodiments of the present invention will be described with reference to FIGS.
図１は本発明に係る摺動部材の製造方法を示すブロック図を示し、この製造方法は、膜形成工程Ｐ１と摩耗工程Ｐ２とを備える。膜形成工程Ｐ１は、図３と図４に示すように、第１部材１の摺動面１ａにグレーティング状凹凸の周期構造３を有する非晶質炭素膜４（図３参照）を形成するものであり、摩耗工程Ｐ２は、第１部材１の摺動面１ａと第２部材２の摺動面２ａとを相対的に摺動させて、周期構造３を犠牲層として摩滅させるものである。図例における第１部材１は平板体で構成し、第２部材２としては円柱状のピン部材で構成した。また、第１部材１及び第２部材２は、炭素鋼、銅、アルミニウム、白金、超硬合金等であっても、炭化ケイ素や窒化ケイ素等のシリコン系セラミックスであっても、エンジニアプラスチック等であってもよい。第２部材２１の摺動面２ａとして、球面状であっても、平坦面であってもよい。また、第２部材２としては、後述するように、摩耗工程において酸化物の摩耗粉を生じる材質が好ましい。 FIG. 1 is a block diagram showing a manufacturing method of a sliding member according to the present invention, and this manufacturing method includes a film forming process P1 and a wear process P2. In the film formation step P1, as shown in FIGS. 3 and 4, an amorphous carbon film 4 (see FIG. 3) having a periodic structure 3 with grating-like irregularities on the sliding surface 1a of the first member 1 is formed. In the wear process P2, the sliding surface 1a of the first member 1 and the sliding surface 2a of the second member 2 are relatively slid to wear the periodic structure 3 as a sacrificial layer. The 1st member 1 in the example was comprised with the flat body, and the 2nd member 2 was comprised with the column-shaped pin member. The first member 1 and the second member 2 may be carbon steel, copper, aluminum, platinum, cemented carbide, silicon ceramics such as silicon carbide or silicon nitride, engineer plastic, etc. There may be. The sliding surface 2a of the second member 21 may be spherical or flat. Moreover, as the 2nd member 2, the material which produces the abrasion powder of an oxide in an abrasion process so that it may mention later is preferable.
膜形成工程Ｐ１は図２に示すように、周期構造形成工程Ｐ１ａと成膜工程Ｐ１ｂとを備える。周期構造形成工程Ｐ１ａは、図５（ａ）（ｂ）に示すように、微小の凹部５と微小の凸部６とが交互に所定ピッチで配設されてなる周期構造を形成する工程であり、図７に示すように、レーザ発生器１１と光学系１０とを備えたレーザ表面加工装置を使用して形成する。 As shown in FIG. 2, the film forming process P1 includes a periodic structure forming process P1a and a film forming process P1b. The periodic structure forming step P1a is a step of forming a periodic structure in which minute concave portions 5 and minute convex portions 6 are alternately arranged at a predetermined pitch as shown in FIGS. 5 (a) and 5 (b). As shown in FIG. 7, a laser surface processing apparatus provided with a laser generator 11 and an optical system 10 is used.
このレーザ表面加工装置では、レーザ発生器１１は、ミラー１２により加工材料Ｗに向けて折り返され、メカニカルシャッタ１３に導かれる。レーザ照射時はメカニカルシャッタ１３を開放し、レーザ照射強度は１／２波長板１４と偏光ビームスプリッタ１６によって調整可能とし、１／２波長板１５によって偏光方向を調整し、集光レンズ１７によって、ＸＹθステージ１９上の加工材料Ｗ表面に集光照射することになる。 In this laser surface processing apparatus, the laser generator 11 is folded back toward the processing material W by the mirror 12 and guided to the mechanical shutter 13. At the time of laser irradiation, the mechanical shutter 13 is opened, the laser irradiation intensity can be adjusted by the half-wave plate 14 and the polarization beam splitter 16, the polarization direction is adjusted by the half-wave plate 15, and the condenser lens 17 The surface of the work material W on the XYθ stage 19 is focused and irradiated.
第１工程２１では、加工閾値近傍の照射強度で直線偏光のレーザを照射し、その照射部分をオーバラップさせながら走査して、自己組織的に形成している。すなわち、アブレーション閾値近傍のフルエンスで直線偏光のレーザをワーク（加工材料）Ｗに照射した場合、入射光と加工材料Ｗの表面に沿った散乱光またはプラズマ波の干渉により、レーザ波長と同程度の周期間隔で、エネルギ一分布にわずかな粗密が生じる。一般的な加工方法ではレーザ照射面全体が加工されるが、加工閾値近傍のエネルギー密度でレーザ照射することで、高エネルギ一部分を選択的に加工することができる。その結果、１光軸のレーザ照射でありながら、グレーティング状の周期構造が形成される。このとき、加工に用いるレーザのパルス幅が長くなるほど熱影響や加工蒸散物との相互作用によるレーザの散乱によって周期構造に乱れが生じることになる。 In the first step 21, a linearly polarized laser beam is irradiated with an irradiation intensity in the vicinity of the processing threshold, and the irradiated portion is scanned while overlapping to form a self-organized structure. That is, when a workpiece (working material) W is irradiated with a linearly polarized laser beam at a fluence near the ablation threshold, interference between the incident light and the scattered light or plasma wave along the surface of the processing material W is approximately the same as the laser wavelength. At periodic intervals, there is a slight roughness in the energy distribution. In a general processing method, the entire laser irradiation surface is processed, but a portion of high energy can be selectively processed by laser irradiation at an energy density near the processing threshold. As a result, a grating-like periodic structure is formed while performing laser irradiation with one optical axis. At this time, the longer the pulse width of the laser used for processing, the more disturbed the periodic structure is due to the influence of heat and the scattering of the laser due to the interaction with the processed evaporation.
成膜工程Ｐ１ｂは、ＤＬＣコーティングであり、例えば、プラズマイオン注入法を採用することができる。プラズマイオン注入法は、高真空中でのプラズマプロセスであるイオン化蒸着により成膜する方法である。すなわち、真空チャンバ中にトルエンガスや他の炭化水素ガスが導入され直流アーク放電プラズマ中で炭化水素イオンが励起されたラジカルが生成される。このため、炭化水素イオンは直流の負電圧にバイアスされた基板（コーティングされる部材）にバイアス電圧に応じたエネルギーで衝突し固体化し成膜する。 The film forming process P1b is DLC coating, and for example, a plasma ion implantation method can be employed. The plasma ion implantation method is a method of forming a film by ionization vapor deposition which is a plasma process in a high vacuum. In other words, toluene gas or other hydrocarbon gas is introduced into the vacuum chamber, and radicals in which hydrocarbon ions are excited in DC arc discharge plasma are generated. For this reason, hydrocarbon ions collide with a substrate (a member to be coated) biased to a negative DC voltage with energy corresponding to the bias voltage to solidify into a film.
非晶質炭素膜４のグレーティング状凹凸の周期構造３は、図６に示すように、連続的に高さが変化するものである。非晶質炭素膜（ＤＬＣ膜）の凹凸の高低差（凹部５の底部から凸部６の頂点までの高さ）が２０ｎｍ以上１００ｎｍ以下かつ非晶質炭素膜の膜厚以下とするのが好ましい。また、非晶質炭素膜（ＤＬＣ膜）の周期ピッチを１０μｍ以下とするのが好ましい。 The grating-like irregular periodic structure 3 of the amorphous carbon film 4 has a continuously changing height as shown in FIG. It is preferable that the height difference of the unevenness of the amorphous carbon film (DLC film) (height from the bottom of the concave portion 5 to the top of the convex portion 6) is not less than 20 nm and not more than 100 nm and not more than the film thickness of the amorphous carbon film. . In addition, the periodic pitch of the amorphous carbon film (DLC film) is preferably 10 μm or less.
そして、第１部材１の摺動面１ａにグレーティング状凹凸の周期構造３を有する非晶質炭素膜４を形成した後は、図３に示すように、この非晶質炭素膜４に対して、第２部材２の摺動面を摺動させる。 Then, after the amorphous carbon film 4 having the grating-like irregular structure 3 is formed on the sliding surface 1a of the first member 1, as shown in FIG. The sliding surface of the second member 2 is slid.
このため、図４に示すように、第１部材１の周期構造先端が摩耗し、この摩耗によって、ＤＬＣ由来の低硬度カーボンが生成される、また、周期構造により、微細な摩耗粉が生成され、マイルド摩耗面に似た滑らかで強固に固着した移着膜が形成される。 For this reason, as shown in FIG. 4, the tip of the periodic structure of the first member 1 is worn, and this wear produces low-hardness carbon derived from DLC, and fine wear powder is produced by the periodic structure. As a result, a smooth and firm transfer film similar to the mild wear surface is formed.
前記摺動部材の製造方法では、連続的に高さが変化するグレーティング状凹凸の周期構造３を非晶質炭素膜（ＤＬＣ膜）４に設けているため、摺動時に小さな曲率半径をもつ周期構造先端が摩耗し、なじみが進行する。この際，第１部材１から発生する微細なＤＬＣ膜４の摩耗粉はグラファイト化され、低摩擦化の実現に重要な低硬度カーボンの生成が促進される。周期構造３を有するＤＬＣ膜４は微細な加工ツールとして作用し、第２部材２からもマイルド摩耗粉のような微細な摩耗粉が発生する。また、周期構造３は第２部材２に形成される突出した移着粒子を削り落とし、トラップすることで移着粒子の成長を抑制し、摩耗粉の微細化と移着膜の平滑化に寄与する。この段階では顕著な摩擦低減効果は得られないが、周期構造３を犠牲層として摩滅させる工程において、微細な摩耗粉が延しつぶされる。これによって、強固に固着された低硬度カーボン移着層が形成されるとともにＤＬＣ膜４が平滑化する。周期構造３が消滅した後も長期に渡って摺動特性が向上する摺動部材が得られる。 In the manufacturing method of the sliding member, the periodic structure 3 with grating-like irregularities whose height continuously changes is provided on the amorphous carbon film (DLC film) 4, and therefore a period having a small radius of curvature when sliding. The tip of the structure is worn and the familiarity progresses. At this time, the wear powder of the fine DLC film 4 generated from the first member 1 is graphitized, and the generation of low-hardness carbon important for realizing low friction is promoted. The DLC film 4 having the periodic structure 3 acts as a fine processing tool, and fine wear powder such as mild wear powder is generated from the second member 2. Further, the periodic structure 3 scrapes off the protruding transfer particles formed on the second member 2 and suppresses the growth of the transfer particles by trapping, thereby contributing to the refinement of wear powder and the smoothing of the transfer film. To do. At this stage, no significant friction reducing effect is obtained, but in the process of wearing the periodic structure 3 as a sacrificial layer, fine wear powder is crushed. Thereby, a low-hardness carbon transfer layer firmly fixed is formed and the DLC film 4 is smoothed. Even after the periodic structure 3 disappears, a sliding member having improved sliding characteristics over a long period of time can be obtained.
また、グレーティング状の凹凸の周期構造形成を行った後、非晶質炭素膜４を成膜することで、形態が異なるだけで通常のＤＬＣ膜４と組成的には同一な周期構造を有するＤＬＣ膜４を形成できる。したがって，硬度低下などの物性変化を生じることなく、ＤＬＣ膜本来の特性を維持したものとなる。なお、ＤＬＣ膜４の硬度が低下すると、ＤＬＣ膜４の微細な加工ツールとしての作用が低下し、移着粒子の成長抑制や摩耗粉の微細化に支障が生じるため、周期構造３が消滅した後も長期に渡って摺動特性が向上する摺動部材が得られない。 In addition, after forming the periodic structure of the grating-like irregularities, the amorphous carbon film 4 is formed, so that the DLC having the same periodic structure in composition as the normal DLC film 4 is different only in form. The film 4 can be formed. Therefore, the original characteristics of the DLC film are maintained without causing changes in physical properties such as a decrease in hardness. Note that when the hardness of the DLC film 4 is lowered, the function of the DLC film 4 as a fine processing tool is lowered, and the growth of transfer particles and the miniaturization of wear powder are hindered, so the periodic structure 3 disappears. A sliding member whose sliding characteristics are improved over a long period of time cannot be obtained.
非晶質炭素膜（ＤＬＣ膜）４の凹凸が２０ｎｍ以上１００ｎｍ以下かつ非晶質炭素膜の膜厚以下とすることで、微細な摩耗粉の発生と周期構造の摩滅を基材が露出することなく効率的に実現できる。 When the irregularity of the amorphous carbon film (DLC film) 4 is 20 nm or more and 100 nm or less and less than the film thickness of the amorphous carbon film, the substrate is exposed to generation of fine wear powder and wear of the periodic structure. Can be realized efficiently.
非晶質炭素膜（ＤＬＣ膜）４の周期ピッチを１０μｍ以下とすることで，低硬度カーボンの生成促進と移着粒子の成長抑制により、マイルド摩耗面に似た移着層を形成することができる。 By setting the periodic pitch of the amorphous carbon film (DLC film) 4 to 10 μm or less, a transfer layer similar to a mild wear surface can be formed by promoting the generation of low hardness carbon and suppressing the growth of transfer particles. it can.
加工闘値近傍の照射強度で 直線偏光のレーザを照射し、その照射部分をオーバーラップさせながら走査して、自己組織的に形成するものでは、機械加工では困難なサブミクロンの周期ピッチと凹凸深さをもつ周期構造３を容易に得ることができる。 With a linearly polarized laser beam irradiated at an irradiation intensity in the vicinity of the processing threshold, and scanning with overlapping irradiation parts, it is difficult to machine with submicron periodic pitch and uneven depth, which is difficult to machine. A periodic structure 3 having a thickness can be easily obtained.
以上、本発明の実施形態につき説明したが、本発明は前記実施形態に限定されることなく種々の変形が可能であって、例えば、前記実施形態では、第１部材１を平板体にて構成し、第２部材２をピン部材にて構成したが、第１部材１と第２部材２の形状としても、図例のものに限らず、他の種々の形状のものにて構成できる。 As mentioned above, although it demonstrated per embodiment of this invention, this invention is not limited to the said embodiment, A various deformation | transformation is possible, for example, in the said embodiment, the 1st member 1 is comprised with a flat body. Although the second member 2 is constituted by a pin member, the shapes of the first member 1 and the second member 2 are not limited to those shown in the drawings, and can be constituted by other various shapes.
周期構造形成工程Ｐ１ａに使用するレーザとしては、フェムト秒レーザ、ピコ秒レーザ、及びナノ秒レーザといったパルスレーザを使用することができる。また、摩耗工程Ｐ２において、第１部材１側を固定して第２部材２を第１部材１に対して摺動させても、逆に、第２部材２側を固定して第１部材１を第２部材２に対して摺動させても、第１部材１と第２部材２とを摺動させてもよい。 As a laser used for the periodic structure forming step P1a, a pulse laser such as a femtosecond laser, a picosecond laser, and a nanosecond laser can be used. Further, in the wear process P2, even if the first member 1 side is fixed and the second member 2 is slid with respect to the first member 1, conversely, the second member 2 side is fixed and the first member 1 is fixed. The first member 1 and the second member 2 may be slid with respect to the second member 2.
また、摺動方向として、周期構造３の配向方向に対して、平行方向であっても、直交方向であっても、さらには、所定角度（例えば、４５度程度）に傾斜したものであってもよい。また、摺動方向として直線状ではなく、円形や楕円形状であってもよい。摺動時の荷重、摺動ストローク、往復周波数等も任意に設定できる。 In addition, the sliding direction may be parallel or orthogonal to the orientation direction of the periodic structure 3, and may be inclined at a predetermined angle (for example, about 45 degrees). Also good. Further, the sliding direction is not linear but may be circular or elliptical. The load during sliding, sliding stroke, reciprocating frequency, etc. can be arbitrarily set.
ところで、ＤＬＣコーティングの処理には、化学蒸着（CVD，Chemical Vapor Deposition）法および物理蒸着（PVD，Physical Vapor Deposition）法によるプラズマ技術等がある。このため、本発明では、プラズマCVD法、イオン化蒸着法、スパッタ法、アークイオンプレーティング法の従来からある種々の方法で、非晶質炭素膜を形成することができる。 By the way, in the processing of DLC coating, there are a plasma technique using a chemical vapor deposition (CVD) method and a physical vapor deposition (PVD) method. Therefore, in the present invention, the amorphous carbon film can be formed by various conventional methods such as plasma CVD, ionized vapor deposition, sputtering, and arc ion plating.
周期構造を有するＤＬＣ膜の作成およびその摺動特性を評価し、移着膜制御による低摩擦化について検証した。 The creation of a DLC film having a periodic structure and its sliding characteristics were evaluated, and the low friction by the transfer film control was verified.
まず、周期構造を有するＤＬＣ膜を作成した。この場合、バフ研磨したＳＵＳ４４０Ｃ基板(算術平均粗さ：Ｒａ０．０２μｍ)にフェムト秒レーザを加工しきい値近傍のエネルギー密度で照射し，グレーティング状の周期構造(ピッチ約７００ｎｍ，深さ約２００ｎｍ)を形成した後、プラズマイオン注入法でａ−Ｃ:ＨのＤＬＣ膜を成膜した。原料ガスにはトルエン(Ｃ7Ｈ8)を用い、中間層としてＳｉ／Ｃ傾斜層を設けた。中間層の膜厚は２５０ｎｍ，中間層を含むＤＬＣの膜厚は１μｍとした。すなわち、基材の上にこの中間層が形成され、この中間層の上にＤＬＣ膜が成膜される。成膜後のＤＬＣ表面のＡＦＭ像および断面プロファイルを前記図６に示している。 First, a DLC film having a periodic structure was prepared. In this case, a buffed SUS440C substrate (arithmetic average roughness: Ra 0.02 μm) is irradiated with a femtosecond laser at an energy density in the vicinity of the processing threshold, and a grating-like periodic structure (pitch: about 700 nm, depth: about 200 nm) Then, an aC: H DLC film was formed by plasma ion implantation. Toluene (C 7 H 8 ) was used as the source gas, and a Si / C gradient layer was provided as an intermediate layer. The thickness of the intermediate layer was 250 nm, and the thickness of the DLC including the intermediate layer was 1 μm. That is, the intermediate layer is formed on the base material, and the DLC film is formed on the intermediate layer. FIG. 6 shows the AFM image and cross-sectional profile of the DLC surface after film formation.
ＤＬＣ表面には深さ５０ｎｍ前後の周期構造形状が認められる。周期構造形成後にＤＬＣを成膜しているため、図６に示す周期構造ＤＬＣはレーザ未照射基板に成膜したものと形態が異なるだけで組成的には同一である。 Periodic structure shapes with a depth of around 50 nm are observed on the DLC surface. Since the DLC film is formed after the formation of the periodic structure, the periodic structure DLC shown in FIG. 6 is the same in composition only in the form different from that formed on the laser non-irradiated substrate.
算術平均粗さＲａは、図８に示すように、粗さ曲線からその平均線の方向に基準長さだけを抜き取り、この抜取り部分の平均線ｍの方向にX軸を、縦倍率の方向にY軸を取り、粗さ曲線をｙ=ｆ（ｘ）で表したときに、次の数１の式によって求められる値をマイクロメートル（μｍ）で表したものをいう。
実験方法としては、ピンオンプレート試験装置を用いて往復摺動実験を行った。ピン試験片（第２部材２）の材質はＳＵＪ２とし，先端形状は曲率半径５ｍｍの半球形とした。プレート試験片（第１部材１）は周期構造ＤＬＣおよびバフ研磨面に成膜した鏡面ＤＬＣの2種類とした。ここで、周期構造ＤＬＣとは、摺動面にグレーティング状凹凸の周期構造３を有する非晶質炭素膜４を有するものであり、鏡面ＤＬＣは、鏡面に仕上げた摺動面にＤＬＣ膜を形成したものである。 As an experimental method, a reciprocating sliding experiment was performed using a pin-on-plate test apparatus. The material of the pin test piece (second member 2) was SUJ2, and the tip shape was a hemisphere with a radius of curvature of 5 mm. Two types of plate test pieces (first member 1) were the periodic structure DLC and the mirror surface DLC formed on the buffed surface. Here, the periodic structure DLC has an amorphous carbon film 4 having a periodic structure 3 with grating-like irregularities on the sliding surface, and the mirror surface DLC forms a DLC film on the sliding surface finished as a mirror surface. It is a thing.
周期構造ＤＬＣに対する摺動方向は，周期構造の配向方向に対して、平行(周期平行ＤＬＣ)および直交(周期直交ＤＬＣ)の２方向とした。摺動条件は荷重５Ｎ、ストローク２０ｍｍ，往復周波数０．５Ｈｚとし、１００００往復までの摺動抵抗をロードセルにより測定した。 The sliding directions with respect to the periodic structure DLC were two directions parallel (periodic parallel DLC) and orthogonal (periodic orthogonal DLC) to the orientation direction of the periodic structure. The sliding conditions were a load of 5 N, a stroke of 20 mm, a reciprocation frequency of 0.5 Hz, and the sliding resistance up to 10,000 reciprocations was measured with a load cell.
各種ＤＬＣ膜の摩擦係数を図９と図１０に示す。摩擦係数は、５００往復までは、鏡面ＤＬＣ＞周期ＤＬＣであり、１０００往復〜５０００往復までは、鏡面ＤＬＣ＜周期ＤＬＣであり、７０００往復を越えれば、鏡面ＤＬＣ＞周期ＤＬＣであり、１００００往復では、鏡面ＤＬＣ＞周期直交ＤＬＣ≫周期平行ＤＬＣである。すなわち、周期平行ＤＬＣおよび周期直交ＤＬＣはいずれも１０００往復〜５０００往復付近まで鏡面ＤＬＣより高い摩擦係数を示した。１００００往復では，周期直交ＤＬＣは鏡面ＤＬＣの摩擦係数を６％下回るだけであったが、周期平行ＤＬＣは鏡面ＤＬＣに対して４０％を超える顕著な摩擦低減効果が得られた。 The friction coefficients of various DLC films are shown in FIGS. The friction coefficient is specular DLC> period DLC up to 500 reciprocations, specular DLC <period DLC from 1000 reciprocations to 5000 reciprocations, and specular DLC> period DLC over 7000 reciprocations. , Mirror surface DLC> periodic orthogonal DLC >> periodic parallel DLC. That is, both the period parallel DLC and the period orthogonal DLC showed a higher coefficient of friction than that of the mirror DLC from 1000 round trips to 5000 round trips. At 10,000 reciprocations, the periodic orthogonal DLC was only 6% below the friction coefficient of the mirror DLC, but the period parallel DLC had a remarkable friction reduction effect exceeding 40% with respect to the mirror DLC.
図１１に各種ＤＬＣ膜に１００００往復させたピン試験片（第２部材２）の摺動面写真を示し、図１２はピン試験片の摺動面プロファイル図を示している。図１１から、鏡面ＤＬＣは摩耗粉が大量・広範囲に付着していることがわかり、周期平行ＤＬＣは摩耗粉の幅方向への広がりが少ないことがわかる。また、図１２から、鏡面ＤＬＣは金属接触によるピン試験片の摩耗発生があり、摩擦係数が低い周期平行ＤＬＣは移着膜が薄く平滑で明色部の比率が高いことがわかる。すなわち、鏡面ＤＬＣに摺動させたピン中央部は大部分の移着膜が剥離し、ピン試験片の摩耗面が露出していた。一方、周期直交ＤＬＣおよび周期平行ＤＬＣに摺動させたピン中央部には明色の移着膜が生成されており、後者の移着膜は平滑で明色の比率が高くなった。なお、図１２（ａ）では摩擦係数μが０．１９６であり、図１２（ｂ）では摩擦係数μが０．１８６であり、図１２（ｃ）では摩擦係数μが０．１１１であった。 FIG. 11 shows a sliding surface photograph of a pin test piece (second member 2) reciprocated 10,000 times on various DLC films, and FIG. 12 shows a sliding surface profile diagram of the pin test piece. From FIG. 11, it can be seen that the mirror surface DLC has a large amount and a wide range of wear powder, and the period parallel DLC has a small spread in the width direction of the wear powder. From FIG. 12, it can be seen that the mirror surface DLC has wear of the pin test piece due to metal contact, and the periodic parallel DLC with a low friction coefficient has a thin transfer film and a smooth ratio with a high light color portion. That is, most of the transfer film peeled off at the center of the pin slid on the mirror surface DLC, and the wear surface of the pin test piece was exposed. On the other hand, a bright transfer film was formed at the center of the pin slid in the periodic orthogonal DLC and the periodic parallel DLC, and the latter transfer film was smooth and the ratio of the bright color was high. In FIG. 12A, the friction coefficient μ is 0.196, in FIG. 12B, the friction coefficient μ is 0.186, and in FIG. 12C, the friction coefficient μ is 0.111. .
図１３(ストローク２０ｍｍ、１００００往復)からわかるように、摩耗生成物は、鏡面ＤＬＣでは周囲に大量に付着し、周期直交ＤＬＣでは周囲に中量に付着し、周期平行ＤＬＣでは周囲に少量が付着していた。なお、摺動痕幅は、鏡面ＤＬＣ、周期直交ＤＬＣ、及び周期平行ＤＬＣともに約１３０μｍである。摺動痕深さは、鏡面ＤＬＣでは１３９ｎｍであり、周期直交ＤＬＣでは１５３ｎｍであり、周期平行ＤＬＣでは６５ｎｍである。 As can be seen from FIG. 13 (stroke 20 mm, 10000 reciprocation), a large amount of wear product adheres to the periphery in the mirror DLC, a medium amount to the periphery in the period orthogonal DLC, and a small amount to the periphery in the period parallel DLC. Was. The sliding trace width is about 130 μm for both the mirror surface DLC, the periodic orthogonal DLC, and the periodic parallel DLC. The sliding trace depth is 139 nm for mirror DLC, 153 nm for periodic orthogonal DLC, and 65 nm for periodic parallel DLC.
ＤＬＣ膜摺動痕周囲の摩耗粉の様子を図１４(ストローク２０ｍｍ、１００００往復)に示す。鏡面ＤＬＣでは移着粒子が成長し、大量の摩耗粉（シビア摩耗粉）が生じた。一方、周期ＤＬＣでは摩耗粉が微細化し、摩耗量が低減された。特に周期平行ＤＬＣでは大幅に摩耗粉が減少した。摺動面内の周期構造にはトラップされた摩耗粉が観察された。周期構造は突出した移着粒子を削り落とし、トラップすることで移着粒子の成長を抑制し、摩耗粉の微細化と移着膜の平滑化に寄与したと推察される.周期平行ＤＬＣでは摩耗粉を摺動面内に拘束する作用が大きいため、摺動痕周囲に散逸する摩耗粉が大幅に減少したと考えられる。 The appearance of the wear powder around the DLC film sliding trace is shown in FIG. 14 (stroke 20 mm, 10,000 reciprocations). In the mirror surface DLC, transfer particles grew and a large amount of wear powder (severe wear powder) was generated. On the other hand, in the period DLC, the wear powder became finer and the amount of wear was reduced. In particular, in the case of the periodic parallel DLC, the wear powder was greatly reduced. Trapped wear powder was observed in the periodic structure in the sliding surface. It is inferred that the periodic structure scraped the protruding transfer particles and trapped them, thereby suppressing the growth of transfer particles and contributing to the refinement of wear powder and smoothing of the transfer film. It is considered that the amount of abrasion powder that dissipates around the sliding trace is greatly reduced because the action of restraining the powder in the sliding surface is large.
図１５(ストローク２０ｍｍ、１０往復)に示すように，鏡面ＤＬＣでは移着粒子の除去，トラップ作用がないため、僅か１０往復で大きく成長した摩耗粉が生成された。ＥＤＸ分析の結果、摩耗粉はピン由来の金属酸化物が主体であった。また、微細な摩耗粉の方が高い酸素含有率を示した。 As shown in FIG. 15 (stroke 20 mm, 10 reciprocations), the mirror surface DLC has no removal of trapped particles and no trapping action, so that a large amount of wear powder was generated after only 10 reciprocations. As a result of EDX analysis, the wear powder was mainly composed of pin-derived metal oxides. The fine wear powder showed a higher oxygen content.
図１６に移着膜剥離部のＳＥＭ画像を示す。剥離した移着膜断面から移着膜は２層構造であることがわかる。第１層は金属酸化物(ピンの摩耗粉)とカーボンの混合物、第２層はＤＬＣ由来のカーボン移着物と思われる。図１７（鏡面ＤＬＣ）および図１８（周期平行ＤＬＣ）にピン摺動痕のＳＥＭ画像とＥＤＸ分析による酸素分布を示す。ＳＥＭ画像の黒い部分はカーボン移着物である。鏡面ＤＬＣでは２０００往復から１００００往復までの間に第１層から剥離し、酸素量が減少した。周期平行ＤＬＣでは、酸素に富んだ微細な摩耗粉が延しつぶされ、マイルド摩耗面に似た第１層が１００００往復まで強固に固着していることが確認された。マイルド摩耗面に似た第１層は強固にカーボン移着物をピンに固着させるバインダーの働きをしていると考えられる。周期平行ＤＬＣは２０００往復あたりから平滑化の進行が認められた。周期平行ＤＬＣの低摩擦化の原因は強固に固着されたカーボン移着膜の生成とＤＬＣ膜・移着膜の平滑化であると考えられる。 FIG. 16 shows an SEM image of the transfer film peeling portion. It can be seen from the cross section of the peeled transfer film that the transfer film has a two-layer structure. The first layer appears to be a mixture of metal oxide (pin wear powder) and carbon, and the second layer is a DLC-derived carbon transfer. FIG. 17 (mirror surface DLC) and FIG. 18 (periodic parallel DLC) show the SEM image of the pin sliding trace and the oxygen distribution by EDX analysis. The black part of the SEM image is a carbon transfer product. The mirror surface DLC peeled off from the first layer between 2000 reciprocations and 10,000 reciprocations, and the amount of oxygen decreased. In the periodic parallel DLC, it was confirmed that fine wear powder rich in oxygen was crushed and the first layer similar to the mild wear surface was firmly fixed up to 10,000 reciprocations. It is considered that the first layer similar to the mild wear surface functions as a binder that firmly fixes the carbon transfer material to the pin. Periodic parallel DLC showed smoothening from around 2000 round trips. The cause of the low friction of the periodic parallel DLC is considered to be the generation of the carbon transfer film firmly fixed and the smoothing of the DLC film / transfer film.
図１９に周期平行ＤＬＣの往復動回数と摩擦係数との関係を示し、図１９（ａ）の楕円内の範囲は移着膜生成過程を示し、図１９（ｂ）の楕円内の範囲は移着膜領域拡大過程を示し、図１９（ｃ）の楕円内の範囲は低摩擦化過程を示している。また、図２０は周期平行ＤＬＣの摺動面を示し、１０往復させた場合である。図２１は周期平行ＤＬＣの摺動面プロファイルを示し、（ａ）は１０往復時の摺動面プロファイル図であり、（ｂ）は２０００往復時の摺動面プロファイル図であり、（ｃ）は１００００往復時の摺動面プロファイル図である。 FIG. 19 shows the relationship between the number of reciprocations of the periodic parallel DLC and the friction coefficient. The range in the ellipse in FIG. 19A shows the transfer film generation process, and the range in the ellipse in FIG. The film deposition region expansion process is shown, and the range within the ellipse in FIG. 19C shows the low friction process. FIG. 20 shows a sliding surface of the periodic parallel DLC, and is a case where the reciprocation is performed 10 times. FIG. 21 shows a sliding surface profile of a periodic parallel DLC, (a) is a sliding surface profile diagram during 10 reciprocations, (b) is a sliding surface profile diagram during 2000 reciprocations, and (c) is It is a sliding face profile figure at the time of 10,000 reciprocations.
図２０では、摩耗粉トラップが移着粒子の成長を抑制し、摩耗粉微細化に寄与することが分かり、図２１（ａ）では、周期構造の多刃工具作用によりピン移着膜は平滑化することが分かる。図２１（ｂ）では、半分程度の周期構造が摩耗にて平滑化していることが分かる。図２１（ｃ）では、大半の周期構造が摩耗にて平滑化していることが分かる。 In FIG. 20, it can be seen that the wear powder trap suppresses the growth of transfer particles and contributes to the refinement of the wear powder. In FIG. 21A, the pin transfer film is smoothed by the multi-blade tool action of the periodic structure. I understand that In FIG. 21B, it can be seen that about half of the periodic structure is smoothed by wear. In FIG. 21C, it can be seen that most of the periodic structures are smoothed by wear.
周期構造を有するDLC膜の摺動特性を評価した結果、以下の結論を得た。
（１）周期平行ＤＬＣは鏡面ＤＬＣに対して摩耗粉が微細化し、４０％を超える摩擦低減効果が得られる。
（２）周期平行ＤＬＣの移着膜は、酸素に富んだ金属酸化物含有層とカーボン移着層の2層構造となる。
（３）周期平行ＤＬＣの低摩擦化要因は強固に固着されたカーボン移着膜の生成とＤＬＣ膜・移着膜の平滑化であると考えられる。
As a result of evaluating the sliding characteristics of the DLC film having a periodic structure, the following conclusions were obtained.
(1) The periodic parallel DLC has a finer abrasion powder than the mirror surface DLC, and a friction reduction effect exceeding 40% is obtained.
(2) The transfer film of the periodic parallel DLC has a two-layer structure of a metal oxide-containing layer rich in oxygen and a carbon transfer layer.
(3) It is considered that the factor for reducing the friction of the periodic parallel DLC is the generation of the carbon transfer film firmly adhered and the smoothing of the DLC film / transfer film.
１ 第１部材
１ａ 摺動面
２ 第２部材
２ａ 摺動面
３ 周期構造部
４ 非晶質炭素（ＤＬＣ）
５ 凹部
６ 凸部
Ｐ１ 膜形成工程
Ｐ１ａ 周期構造形成工程
Ｐ１ｂ 成膜工程
Ｐ２ 摩耗工程
DESCRIPTION OF SYMBOLS 1 1st member 1a Sliding surface 2 2nd member 2a Sliding surface 3 Periodic structure part 4 Amorphous carbon (DLC)
5 Concave portion 6 Convex portion P1 Film forming process P1a Periodic structure forming process P1b Film forming process P2 Wear process
Claims (6)
第１部材の摺動面と第２部材の摺動面とを相対的に摺動させて，前記周期構造を犠牲層として摩滅させ、かつ、前記非晶質炭素膜から発生する摩耗粉をグラファイト化させて低硬度カーボンを生成させるとともに第２部材からも摩耗粉を発生させて移着層を形成する摩耗工程とを備えたことを特徴とする摺動部材の製造方法。 A film forming step of forming an amorphous carbon film having a periodic structure of grating-like irregularities in which the height of the convex portion is a non-flat surface and the height continuously changes on the sliding surface of the first member;
The sliding surface of the first member and the sliding surface of the second member are relatively slid to wear the periodic structure as a sacrificial layer , and wear powder generated from the amorphous carbon film is graphite. And producing a low hardness carbon, and generating a wear layer from the second member to form a transfer layer, and a method for manufacturing a sliding member.
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