JP4631472B2 - Manufacturing method of covering member - Google Patents
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- JP4631472B2 JP4631472B2 JP2005056471A JP2005056471A JP4631472B2 JP 4631472 B2 JP4631472 B2 JP 4631472B2 JP 2005056471 A JP2005056471 A JP 2005056471A JP 2005056471 A JP2005056471 A JP 2005056471A JP 4631472 B2 JP4631472 B2 JP 4631472B2
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Description
本発明は、硬質膜により表面を被覆された被覆部材の製造方法に関する。 The present invention relates to a method for manufacturing a covering member whose surface is covered with a hard film.
耐摩耗性等を付与するために、各種工具や各種機械部品などの表面に非晶質炭素膜やＴｉＣ、ＴｉＮ等のセラミックス系の硬質膜を形成した被覆部材が、幅広い分野で用いられている。特に、非晶質炭素（Diamond Like Carbon ：以下、「ＤＬＣ」と記載）からなる硬質膜は、耐摩耗性に優れ、相手攻撃性が低いため、各種摺動部材や工具類の被覆膜として利用されている。たとえば、特許文献１には、サーメット製の基材を熱処理した後、プラズマＣＶＤ法（ＣＶＤ：Chemical Vapor Deposition ）により基材の表面にＤＬＣ膜を形成する被覆部材の製造方法が開示されている。 In order to impart wear resistance and the like, covering members in which amorphous carbon films and ceramic hard films such as TiC and TiN are formed on the surfaces of various tools and various machine parts are used in a wide range of fields. . In particular, a hard film made of amorphous carbon (Diamond Like Carbon: hereinafter referred to as “DLC”) is excellent in wear resistance and has low opponent attack, so that it can be used as a coating film for various sliding members and tools. It's being used. For example, Patent Document 1 discloses a method for manufacturing a covering member in which a DLC film is formed on the surface of a base material by a plasma CVD method (CVD: Chemical Vapor Deposition) after heat-treating the base material made of cermet.
ところが、プラズマＣＶＤ法による成膜は処理温度が高く、通常、ＤＬＣ膜を成膜する際には５００℃以上で成膜が行われる。５００℃以上の処理では、ほとんどの鋼材が焼鈍されるため、鋼からなる部材にＤＬＣ膜を形成すると強度が低下するという問題がある。そのため、鋼材にＤＬＣ膜を形成した場合には、表面硬度は向上するが、繰り返しの使用によりＤＬＣ膜が剥離してしまうと、硬度の低い鋼材表面が露出するため、耐久性が悪いものであった。
本発明は、上記の問題点に鑑み、鋼からなる基材にＤＬＣ膜を形成しても、基材の強度が低下せず、高強度の被覆部材を得ることができる被覆部材の製造方法を提供することを目的とする。 In view of the above problems, the present invention provides a method for manufacturing a covering member that can obtain a high-strength covering member without lowering the strength of the base material even if a DLC film is formed on the base material made of steel. The purpose is to provide.
本発明者らは、様々な鋼材にＤＬＣ膜の成膜を試みたところ、Ｍｏを含有する鋼からなる基材では、成膜後の基材の強度の低下が見られない、もしくは、強度が向上する場合があることに着目した。 The inventors of the present invention have attempted to form a DLC film on various steel materials. With a base material made of steel containing Mo, the strength of the base material after film formation is not reduced, or the strength is low. We focused on the fact that it might improve.
そこで、本発明の被覆部材の製造方法は、少なくともＭｏを含有する鋼からなる基材に焼入れする焼入れ工程と、該基材の表面にプラズマＣＶＤ法により非晶質炭素膜（ＤＬＣ膜）を形成して該基材を焼戻しする焼戻し工程と、からなることを特徴とする。 Therefore, the manufacturing method of the covering member of the present invention includes a quenching process in which a base material made of steel containing at least Mo is quenched, and an amorphous carbon film (DLC film) is formed on the surface of the base material by a plasma CVD method. And a tempering step of tempering the base material.
この際、前記焼戻し工程は、前記基材の温度を５００〜６２０℃にして前記非晶質炭素膜を形成する工程であるのが望ましい。なお、「前記基材の温度を５００〜６２０℃にして」とは、基材の少なくとも表面部が５００〜６２０℃となった状態を指す。 At this time, the tempering step is preferably a step of forming the amorphous carbon film by setting the temperature of the base material to 500 to 620 ° C. “The temperature of the substrate is set to 500 to 620 ° C.” refers to a state where at least the surface portion of the substrate is 500 to 620 ° C.
また、前記鋼は、工具鋼であるのが好ましい。また、前記基材は、鍛造用工具であるのが好ましい。 The steel is preferably tool steel. The substrate is preferably a forging tool.
本発明の被覆部材の製造方法によれば、上記の焼戻し工程において、プラズマＣＶＤ法によるＤＬＣ膜の成膜温度が上記基材の焼戻し温度に達するため、焼戻し処理とプラズマＣＶＤ処理とを同時に行うことができる。すなわち、本発明の被覆部材の製造方法を用いれば、強度低下を引き起こすことなく、鋼材へのＤＬＣ膜の形成が可能となる。その上、基材に対するＤＬＣの成膜と焼戻しとを一工程にできるため、製造工程が簡略化される。 According to the manufacturing method of the covering member of the present invention, in the tempering step, since the film forming temperature of the DLC film by the plasma CVD method reaches the tempering temperature of the base material, the tempering process and the plasma CVD process are performed simultaneously. Can do. That is, if the manufacturing method of the covering member of the present invention is used, a DLC film can be formed on a steel material without causing a decrease in strength. In addition, since the DLC film formation and tempering on the substrate can be performed in one step, the manufacturing process is simplified.
また、基材の温度を５００〜６２０℃にしてＤＬＣ膜を形成することにより、Ｍｏを含有する鋼からなる基材は、良好に硬化する。 Moreover, the base material which consists of steel containing Mo is hardened | cured favorably by setting the temperature of a base material to 500-620 degreeC, and forming a DLC film.
そして、特に、工具鋼からなる基材を用いれば、焼戻し工程において、焼戻しを行いつつ、その表面にＤＬＣを成膜でき、各種工具に高い強度を付与した被覆部材が得られる。また、基材が鍛造用工具であれば、表面に形成されたＤＬＣ膜と焼戻しによる基材の硬化とで、相手攻撃性が低く耐久性に優れた工具となる。 In particular, if a base material made of tool steel is used, a DLC film can be formed on the surface of the tool while tempering in the tempering step, and a coating member having high strength applied to various tools can be obtained. Further, if the base material is a forging tool, the DLC film formed on the surface and the hardening of the base material by tempering result in a tool with low opponent attack and excellent durability.
本発明の被覆部材の製造方法は、主として、焼入れ工程と、焼戻し工程と、からなる。なお、焼入れ工程は、通常の鋼材に対して行われる「焼入れ」と同様の処理であるが、本発明の被覆部材の製造方法は、焼入れ工程後に行う焼戻し工程に特色がある。 The manufacturing method of the covering member of the present invention mainly includes a quenching step and a tempering step. In addition, although a hardening process is the process similar to "hardening" performed with respect to a normal steel material, the manufacturing method of the coating | coated member of this invention has the feature in the tempering process performed after a hardening process.
焼入れ工程は、鋼からなる基材に焼入れをする工程である。この際、焼入れされる基材は、少なくともＭｏを含有する鋼からなる。Ｍｏを含有する鋼は、焼戻し温度が５００℃以上であるため、後述する焼戻し工程において好適である。Ｍｏを含有する鋼としては、炭素工具鋼、合金工具鋼、高速度鋼、超硬合金などの工具鋼や、クロムモリブデン鋼、ニッケルクロムモリブデン鋼などの、構造用合金鋼などが使用可能である。具体的には、ＳＫＤ１１（ＪＩＳ記号、Ｍｏ含有量：０．８〜１．２質量％）、ＳＫＨ５１（Ｍｏ：４．７０〜５．２０質量％）、ＳＫＤ６１（Ｍｏ：１．０〜１．５質量％）、ＳＣＭ４１５（Ｍｏ：０．１５〜０．３０質量％）、ＳＣＭ８２２（Ｍｏ：０．３５〜０．４５質量％）、また、Ｍｏを２．０〜４．０質量％含有する特殊鋼（特開２００２−１２９２０１号公報参照）などが挙げられる。すなわち、基材は、Ｍｏを０．１５質量％以上含有する鋼性の基材であるのが好ましく、より好ましくは０．８質量％以上、さらに好ましくは１．０質量％以上である。 The quenching step is a step of quenching a base material made of steel. At this time, the base material to be quenched is made of steel containing at least Mo. Since steel containing Mo has a tempering temperature of 500 ° C. or higher, it is suitable for the tempering step described later. As steels containing Mo, tool steels such as carbon tool steel, alloy tool steel, high speed steel and cemented carbide, and structural alloy steels such as chromium molybdenum steel and nickel chrome molybdenum steel can be used. . Specifically, SKD11 (JIS symbol, Mo content: 0.8 to 1.2 mass %), SKH51 (Mo: 4.70 to 5.20 mass %), SKD61 (Mo: 1.0 to 1. mass %). 5 mass %), SCM415 (Mo: 0.15 to 0.30 mass %), SCM822 (Mo: 0.35 to 0.45 mass %), and 2.0 to 4.0 mass % of Mo. Special steel (see JP 2002-129201 A) and the like can be mentioned. That is, the substrate is preferably a steel substrate containing 0.15% by mass or more of Mo, more preferably 0.8% by mass or more, and still more preferably 1.0% by mass or more.
Ｍｏの含有量が上記の値以上であれば、Ｍｏの添加の効果により基材の耐摩耗性が向上し、後述の焼戻し工程において良好に基材が硬化するため、好ましい。なお、Ｍｏの含有量が１０質量％以下であれば、結晶粒界での炭化物の過度の生成を抑制することができ、基材の靱性が保持されるため、好ましい。 If the content of Mo is equal to or greater than the above value, the wear resistance of the base material is improved by the effect of addition of Mo, and the base material is cured well in the tempering step described later, which is preferable. In addition, if content of Mo is 10 mass % or less, since the excessive production | generation of the carbide | carbonized_material in a crystal grain boundary can be suppressed and the toughness of a base material is hold | maintained, it is preferable.
また、基材の形状に特に限定はないため、軸受け部材や歯車、金型、また、鍛造用工具、切削工具、治具、ダイス、パンチ、ローラー、ベアリング、転造工具、刃物などに用いることができる。後に詳説する焼戻し工程で基材の表面に形成されるＤＬＣ膜は摩擦係数が小さく相手攻撃性が低く、また、焼戻し工程により基材が高強度となるため、本発明の製造方法で得られる被覆部材は、上記の工具などに好適に用いられる。 In addition, since there is no particular limitation on the shape of the base material, it is used for bearing members, gears, dies, forging tools, cutting tools, jigs, dies, punches, rollers, bearings, rolling tools, blades, etc. Can do. The DLC film formed on the surface of the base material in the tempering process described in detail later has a low coefficient of friction and low partner attack, and the base material becomes high strength by the tempering process, so that the coating obtained by the production method of the present invention The member is preferably used for the above-described tool or the like.
焼戻し工程は、基材の表面にプラズマＣＶＤ法によりＤＬＣ膜を形成して基材を焼戻しする工程である。焼戻し工程では、ＤＬＣ膜の形成と焼戻しとを、基材に対して同時に行う。 The tempering step is a step of tempering the substrate by forming a DLC film on the surface of the substrate by plasma CVD. In the tempering step, the DLC film is formed and tempered simultaneously on the substrate.
ここで、図１は、ＤＬＣ成膜温度に対する基材の硬さ（ビッカース硬さ）を示すグラフである。以下、「ＤＬＣ膜の成膜温度」とは、基材の少なくとも表面の温度である。ＤＬＣ膜を成膜する基材として、Ｍｏを含有しないＳＫＤ１と、Ｍｏを含有するＳＫＤ１１と、を用いた。Ｍｏを含有しないＳＫＤ１では、ＤＬＣの成膜時の熱によりセメンタイトが生成され、成膜温度が高いほど基材の硬さが低下（脆化）する傾向にある。一方、Ｍｏを含有するＳＫＤ１１では、５００〜５５０℃の範囲で、基材の硬さが向上する温度範囲が存在する。これは、Ｍｏ2 Ｃ等の合金炭化物の析出によりセメンタイトが母相中に固溶する、いわゆる「二次硬化」により鋼の強度が向上するためである。 Here, FIG. 1 is a graph showing the hardness (Vickers hardness) of the substrate with respect to the DLC film formation temperature. Hereinafter, “the deposition temperature of the DLC film” is the temperature of at least the surface of the substrate. As the base material on which the DLC film was formed, SKD1 containing no Mo and SKD11 containing Mo were used. In SKD1 that does not contain Mo, cementite is generated by the heat during DLC film formation, and the hardness of the substrate tends to decrease (brittle) as the film formation temperature increases. On the other hand, in SKD11 containing Mo, there is a temperature range in which the hardness of the substrate is improved in the range of 500 to 550 ° C. This is because the strength of the steel is improved by so-called “secondary hardening” in which cementite is dissolved in the matrix phase by precipitation of alloy carbide such as Mo 2 C.
なお、ＳＫＤ１１では、５００〜５５０℃でのＤＬＣ膜の成膜により、Ｈｖ２５０からＨｖ３００程度にまで基材の強度が向上する。すなわち、基材の少なくとも表面部の温度が５００〜５５０℃で成膜を行えば、ＤＬＣ膜の形成された被覆部材の表面のみでなく、基材の表面部まで硬度が向上する。一方、ＳＫＤ１を同様の温度で成膜した場合には、Ｈｖ１５０程度まで低下する。 In SKD11, the strength of the base material is improved from Hv250 to about Hv300 by forming the DLC film at 500 to 550 ° C. That is, when film formation is performed at a temperature of at least the surface portion of the base material at 500 to 550 ° C., the hardness is improved not only on the surface of the covering member on which the DLC film is formed but also on the surface portion of the base material. On the other hand, when the SKD1 is formed at the same temperature, it decreases to about Hv150.
本発明では、上記の現象を利用して、プラズマＣＶＤ法による基材表面へのＤＬＣの成膜と、基材の焼戻しと、を焼戻し工程において同時に行った。すなわち、ＤＬＣ膜の成膜を、基材の焼戻し温度にて行った。通常、プラズマＣＶＤ法によるＤＬＣ膜の成膜は、５００℃以上の高温で行われるが、５００℃以上の焼戻しにより二次硬化が生じるＭｏを含有する鋼からなる基材に対して成膜を行うことで、ＤＬＣの成膜と焼戻し処理を同時に行うことが可能となる。その結果、基材の表面に硬質のＤＬＣ膜が形成されるとともに、基材の強度も向上する。 In the present invention, using the above phenomenon, the DLC film formation on the substrate surface by the plasma CVD method and the tempering of the substrate were simultaneously performed in the tempering step. That is, the DLC film was formed at the tempering temperature of the substrate. Usually, the DLC film is formed by plasma CVD at a high temperature of 500 ° C. or higher. However, the DLC film is formed on a base material made of Mo-containing steel that undergoes secondary hardening by tempering at 500 ° C. or higher. This makes it possible to perform DLC film formation and tempering simultaneously. As a result, a hard DLC film is formed on the surface of the substrate, and the strength of the substrate is improved.
焼戻し工程での焼戻し温度（すなわち、ＤＬＣ膜の成膜温度）は、基材に二次硬化が生じる温度範囲であれば、特に限定はない。ただし、温度が高すぎる場合には、粒界に析出する炭化物が増加して、靱性が低下するため、具体的には、５００〜６２０℃でＤＬＣ膜を成膜すればよい。 The tempering temperature in the tempering step (that is, the film forming temperature of the DLC film) is not particularly limited as long as it is in a temperature range where secondary curing occurs on the substrate. However, when the temperature is too high, carbides precipitated at the grain boundaries increase and the toughness decreases, and specifically, a DLC film may be formed at 500 to 620 ° C.
ＤＬＣ膜を形成するプラズマＣＶＤ法としては、直流プラズマＣＶＤ法を用いるとよい。直流プラズマＣＶＤ法では、直流電源に結線された電位差のある二つの電極の間に電力を加えてグロー放電を生じさせ、このグロー放電を利用して、電極間に導入した処理ガスをプラズマ化させ、マイナス電位側の電極にＤＬＣ膜を堆積させる。この際、基材をマイナス極に結線し、基材全体をグロー放電させて成膜するので、グロー放電により基材の温度は上昇し、基材全体を焼戻し温度にまで良好に到達させることができる。 As a plasma CVD method for forming the DLC film, a direct current plasma CVD method may be used. In the DC plasma CVD method, a glow discharge is generated by applying electric power between two electrodes having a potential difference connected to a DC power source, and the process gas introduced between the electrodes is converted into plasma by using this glow discharge. Then, a DLC film is deposited on the negative potential side electrode. At this time, since the base material is connected to the negative electrode and the entire base material is glow-discharged to form a film, the glow discharge increases the temperature of the base material and allows the base material to reach the tempering temperature satisfactorily. it can.
また、ＤＬＣ膜としては、堆積密度の高いＤＬＣ膜や、珪素を含有するＤＬＣ−Ｓｉ膜などの耐摩耗性に優れたＤＬＣ膜を形成するのがよい。 Further, as the DLC film, it is preferable to form a DLC film having excellent wear resistance such as a DLC film having a high deposition density or a DLC-Si film containing silicon.
なお、本発明の被覆部材の製造方法は、上記実施の形態に限定されるものではなく、ＤＬＣ膜の密着性を向上させるために基材の表面を粗面化する表面処理や、基材の表面を硬化させる窒化処理や浸炭処理などを、適宜行っても良い。 In addition, the manufacturing method of the coating | coated member of this invention is not limited to the said embodiment, The surface treatment which roughens the surface of a base material in order to improve the adhesiveness of a DLC film, Nitriding treatment or carburizing treatment for hardening the surface may be appropriately performed.
以下に、本発明の被覆部材の製造方法の実施例を比較例と共に説明する。 Below, the Example of the manufacturing method of the coating | coated member of this invention is described with a comparative example.
［実施例１］
以下の方法により、表面にＤＬＣ−Ｓｉ膜（珪素含有非晶質炭素膜）をもつ等速ジョイント用鍛造工具（以下「ＣＶＪ用鍛造工具」と記載）を製造した。
[Example 1]
A forging tool for a constant velocity joint (hereinafter referred to as “forging tool for CVJ”) having a DLC-Si film (silicon-containing amorphous carbon film) on the surface was produced by the following method.
所定の形状をもつＳＫＨ５１からなる鋼材を１２１０℃で１．５分間保持後、急冷して焼入れを行った。次に、焼入れした鋼材をプラズマ電源のマイナス極に結線し、プラス極（接地電極）に結線した成膜炉内に配置し、直流プラズマＣＶＤ法によりＤＬＣ−Ｓｉ膜を成膜した。この際、成膜温度を５００℃（鋼材の表面を測定）とし、成膜終了後、鋼材を急冷して、鋼材に焼戻しを行った。得られたＤＬＣ−Ｓｉ膜の膜厚は、３μｍであった。 A steel material made of SKH51 having a predetermined shape was held at 1210 ° C. for 1.5 minutes and then quenched and quenched. Next, the quenched steel material was connected to the negative electrode of the plasma power source and placed in a film forming furnace connected to the positive electrode (ground electrode), and a DLC-Si film was formed by DC plasma CVD. At this time, the film formation temperature was 500 ° C. (the surface of the steel material was measured), and after the film formation was completed, the steel material was quenched and tempered. The film thickness of the obtained DLC-Si film was 3 μm.
［比較例１］
ＤＬＣ−Ｓｉ膜のかわりに、プラズマＣＶＤ法により成膜温度７００℃で３μｍのＴｉＣ膜を成膜した他は、実施例１と同様にして、比較例のＣＶＪ用鍛造工具を作製した。
[Comparative Example 1]
A forging tool for CVJ as a comparative example was produced in the same manner as in Example 1 except that a 3 μm TiC film was formed by a plasma CVD method at a film forming temperature of 700 ° C. instead of the DLC-Si film.
［評価］
実施例１および比較例１のＣＶＪ用鍛造工具について、耐久試験を行った。耐久試験は、両者を同じ条件の下で使用し、工具の先端の摩耗量が５μｍ以上となるまでの使用回数を、その工具の使用寿命とした。表１に、結果を示す。
[Evaluation]
The durability test was performed on the forged tools for CVJ of Example 1 and Comparative Example 1. In the durability test, both were used under the same conditions, and the number of uses until the amount of wear at the tip of the tool reached 5 μm or more was defined as the service life of the tool. Table 1 shows the results.
ＤＬＣ−Ｓｉ膜の成膜とともに鋼材が二次硬化した実施例１のＣＶＪ用鍛造工具は、鋼材の表面硬度が高く耐久性に優れる。一方、７００℃でＴｉＣ膜を成膜した比較例１では、成膜時に高温にさらされたことによって、表面硬度が低下した。また、ＤＬＣ−Ｓｉ膜を成膜した実施例１のＣＶＪ用鍛造工具は、ＴｉＣ膜を形成した比較例１よりも、耐摩耗性に優れる。 The forging tool for CVJ of Example 1 in which the steel material is secondarily cured with the formation of the DLC-Si film has high surface hardness of the steel material and excellent durability. On the other hand, in Comparative Example 1 in which the TiC film was formed at 700 ° C., the surface hardness was lowered by being exposed to a high temperature during the film formation. In addition, the forging tool for CVJ of Example 1 in which the DLC-Si film is formed is more excellent in wear resistance than Comparative Example 1 in which the TiC film is formed.
［実施例２］
所定の形状をもつＳＫＤ１１からなる鋼材を１０４０℃で５０分間保持後、急冷して焼入れを行った。次に、実施例１と同様にして、ＤＬＣ−Ｓｉ膜を成膜し、表面にＤＬＣ−Ｓｉ膜をもつ試験片を作製した。
[Example 2]
A steel material made of SKD11 having a predetermined shape was held at 1040 ° C. for 50 minutes and then quenched and quenched. Next, in the same manner as in Example 1, a DLC-Si film was formed, and a test piece having a DLC-Si film on the surface was produced.
ＤＬＣ−Ｓｉ膜を形成する鋼材の表面に対し、成膜前後の鋼材（試験片）の表面硬さ（ビッカース硬さ）を測定（ＪＩＳ Ｚ ２２４４に準拠）した。測定結果を図２に示す。５００℃の成膜により鋼材に二次硬化が生じ、また、表面がＤＬＣ−Ｓｉ膜により覆われたため、成膜後の表面硬度が大きく向上した。 The surface hardness (Vickers hardness) of the steel material (test piece) before and after film formation was measured (based on JIS Z 2244) with respect to the surface of the steel material forming the DLC-Si film. The measurement results are shown in FIG. Secondary hardening occurred in the steel material by the film formation at 500 ° C., and the surface was covered with the DLC-Si film, so that the surface hardness after the film formation was greatly improved.
Claims (7)
該基材の表面にプラズマＣＶＤ法により非晶質炭素膜を形成して該基材を焼戻しする焼戻し工程と、からなることを特徴とする被覆部材の製造方法。 A quenching step of quenching at least a base material made of steel containing Mo;
And a tempering step in which an amorphous carbon film is formed on the surface of the base material by a plasma CVD method and the base material is tempered.
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