JP2007084899A - Coating member, and method for coating coating member - Google Patents
Coating member, and method for coating coating member Download PDFInfo
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本願発明は、超硬合金、サーメット、高速度鋼、ダイス鋼等を基体とし、例えば金属等の窒化物、炭化物、硫化物、硼化物、酸化物を被覆した被覆部材、被覆部材の被覆方法に関する。 The present invention relates to a coated member coated with a cemented carbide, cermet, high-speed steel, die steel or the like and coated with, for example, a nitride, carbide, sulfide, boride, or oxide of a metal, etc., and a coating method of the coated member .
皮膜の被覆過程で不可避的に混入するドロップレット若しくはマクロパーティクルの低減化技術は、特許文献１から５に開示されている。特許文献１は、コーティング層の表面に存在する直径５μｍ以上の突起状粒子が、１０個／ｍｍ２以下とする技術が開示されている。特許文献２は被覆穴あけ工具の外周マージン部の算術平均粗さＲａ値を規定する技術が開示されている。特許文献３は、突起状粒子を機械的に除去し、皮膜表面の耐摩耗性を改善する技術が開示されている。特許文献４は、突起状粒子が生じないような成膜方法として、ホロカソード法とマグネトロンスパッタ法を併用する技術が開示されている。特許文献５は、被膜の表面において、高さ０．５μｍ以上の突起の個数を規定した被覆工具に関する技術が開示されている。 Patent Documents 1 to 5 disclose techniques for reducing droplets or macro particles inevitably mixed in the coating process of the film. Patent Document 1 discloses a technique in which the number of protruding particles having a diameter of 5 μm or more present on the surface of a coating layer is 10 particles / mm 2 or less. Patent Document 2 discloses a technique for defining the arithmetic average roughness Ra value of the outer periphery margin portion of the covered drilling tool. Patent Document 3 discloses a technique for mechanically removing protruding particles and improving the wear resistance of the coating surface. Patent Document 4 discloses a technique in which a holocathode method and a magnetron sputtering method are used in combination as a film forming method that does not generate protruding particles. Patent Document 5 discloses a technique relating to a coated tool in which the number of protrusions having a height of 0.5 μm or more is defined on the surface of the coating.
皮膜の被覆過程で不可避的に混入する突起状粒子は、ドロップレット若しくはマクロパーティクルと呼ぶ場合もある。この突起状粒子は皮膜表面の面粗度を低下させ、皮膜の潤滑性や摩耗特性を劣化させる。その結果、切り屑の排出性低下による工具の折損や局部摩耗を誘発し、近年の高精度加工に於いては問題点である。そこでこれら問題点に対して改善の検討がなされている。
しかし、これらの潤滑性を改善するための単純な皮膜表面の突起状粒子の制限、もしくは皮膜表面の面粗度の規定では十分に潤滑性を改善することができない。
そこで本願発明の課題は、被覆部材が耐熱性や潤滑性に優れた表面状態となる被覆部材及び被覆部材の被覆方法を提供することである。
The protruding particles that are inevitably mixed in the coating process may be called droplets or macro particles. These protruding particles lower the surface roughness of the film surface and degrade the lubricity and wear characteristics of the film. As a result, tool breakage and local wear are induced due to reduced chip discharge, which is a problem in recent high-precision machining. Therefore, improvement of these problems has been studied.
However, it is not possible to sufficiently improve the lubricity by simply restricting the protruding particles on the surface of the film or by defining the surface roughness of the film surface in order to improve the lubricity.
Then, the subject of this invention is providing the coating | coated method of the coating | coated member and coating | coated member in which a coating | coated member becomes the surface state excellent in heat resistance and lubricity.
本願発明は、被覆部材に被覆された皮膜の金属成分は窒化物、炭化物、硫化物、硼化物、酸化物の何れか又はそれらの固溶体又は混合物であり、該皮膜表面には該固溶体又は該混合物と略同一組成の粒子を有し、該粒子は該皮膜表面から５ｎｍ以上、２００ｎｍ未満の突起状粒子であることを特徴とする被覆部材である。本構成を採用することによって耐熱性や潤滑性に優れた表面状態となる被覆部材を提供することができる。 In the present invention, the metal component of the coating coated on the coating member is any of nitride, carbide, sulfide, boride, oxide, or a solid solution or mixture thereof, and the solid solution or mixture is present on the coating surface. The coated member is characterized in that the particles are protruding particles having a particle size of approximately 5 nm or more and less than 200 nm from the surface of the coating. By employing this configuration, it is possible to provide a covering member that has a surface state excellent in heat resistance and lubricity.
本願発明の被覆部材について、皮膜を構成する金属成分はＳｉ、Ａｌ、Ｔｉ、Ｃｒ、Ｎｂ、Ｍｏ、Ｂ、Ｗから選択される少なくとも２種以上であること、また皮膜表面にある突起状粒子は、非金属元素の原子％を該金属元素の原子％で除した値をＲとしたとき、０．３≦Ｒ≦０．６の範囲にあることが好ましい。突起状粒子の数は、該皮膜表面の任意に選択される１０μｍ２の範囲内に５０個以上、５００個未満であることが好ましい。被覆部材の被覆方法には物理蒸着法を採用し、この物理蒸着法はスパッタリング法（以下、ＭＳ法と言う。）、により被覆することが好ましい。 Regarding the coated member of the present invention, the metal component constituting the film is at least two selected from Si, Al, Ti, Cr, Nb, Mo, B, and W, and the protruding particles on the film surface are When R is a value obtained by dividing the atomic% of the nonmetallic element by the atomic% of the metallic element, it is preferably in the range of 0.3 ≦ R ≦ 0.6. The number of protruding particles is preferably 50 or more and less than 500 within an arbitrarily selected range of 10 μm 2 on the surface of the coating. A physical vapor deposition method is employed as a coating method for the covering member, and the physical vapor deposition method is preferably coated by a sputtering method (hereinafter referred to as an MS method).
本願発明によって、耐熱性や潤滑性に優れた表面状態となる被覆部材及び被覆部材の被覆方法を提供することができた。例えば切削工具に適用した場合、被加工物の仕上げ精度向上、工具の折損、局部摩耗を著しく低減させることが可能である。近年の高精度加工に於いて、部材寿命を改善した被覆部材及び被覆部材の被覆方法を提供することが可能となった。そして本願発明は生産性向上並びにコスト低減に極めて有効である。 By this invention, the coating | coated member used as the surface state excellent in heat resistance and lubricity, and the coating | coated method of a coating | coated member were able to be provided. For example, when applied to a cutting tool, it is possible to significantly reduce the finishing accuracy of the workpiece, breakage of the tool, and local wear. In recent high-precision machining, it has become possible to provide a covering member and a covering member covering method with improved member life. The present invention is extremely effective for improving productivity and reducing costs.
本願発明は、皮膜表面を５ｎｍ以上、２００ｎｍ未満の突起状粒子であって、皮膜組成と略同一組成を有する固溶体又は混合物の突起状粒子に制限することにより、平滑性を維持しつつ、皮膜残留応力を低い状態にすることを可能にした。更に膜と基体との密着性を改善することができる。例えば切削工具に適用した場合、被加工物とは点接触のため摩擦係数を低減させることができる。更に、潤滑油や潤滑材等を皮膜表面に保持する効果に優れ耐摩耗性を改良することができる。一方、単純に皮膜のマクロパーティクルを低減させると、皮膜内の残留応力が増加し、高硬度化する。この場合には硬くて脆い特性を有する皮膜が形成され、基体との密着強度が低下する。ここで言う、本願発明の突起状粒子と、一般的に言うマクロパーティクルとは異なる形態を示すものである。突起状粒子は皮膜そのもの、或いは皮膜組成と略同一組成を有する固溶体又は混合物である。即ち、突起状粒子を構成する成分のうち、非金属元素の原子％をＹとし、金属元素の原子％をＸとしたときのＹ／Ｘの値をＲとしたとき、Ｒ値が０．３≦Ｒ≦０．６の範囲で存在するものである。これに対して、マクロパーティクルは金属成分が主体であるため、Ｒ値は０．２以下のものであって区別される。
皮膜表面の５ｎｍ以上、２００ｎｍ未満の突起状粒子は摩耗環境下において、優れた耐摩耗性を発揮する。そのメカニズムは、ナノサイズから構成される突起状粒子が硬質皮膜表面の表面積を増加させ、摩耗環境下でその界面に潤滑層を形成するためである。更にこの特徴的な突起状粒子は、金属成分としてＳｉ、Ａｌ、Ｔｉ、Ｃｒ、Ｎｂ、Ｍｏ、Ｂ、Ｗから選択される少なくとも２種以上の窒化物、炭化物、硫化物、硼化物、酸化物の何れか又はそれらの固溶体又は混合物で構成される場合に形成され、優れた耐摩耗効果を発揮するために好ましい。
The invention of the present application limits the surface of the film to protruding particles of 5 nm or more and less than 200 nm, which are solid solution or mixture having substantially the same composition as the film composition, thereby maintaining the smoothness of the film. It was possible to make the stress low. Furthermore, the adhesion between the film and the substrate can be improved. For example, when applied to a cutting tool, the coefficient of friction can be reduced due to point contact with the workpiece. Furthermore, it is excellent in the effect of retaining lubricating oil, lubricant, etc. on the surface of the film, and wear resistance can be improved. On the other hand, when the macro particles in the coating are simply reduced, the residual stress in the coating increases and the hardness increases. In this case, a hard and brittle film is formed, and the adhesion strength with the substrate is lowered. The protruding particles of the present invention referred to here and the macro particles generally referred to show different forms. The protruding particles are the film itself, or a solid solution or mixture having substantially the same composition as the film composition. That is, among the components constituting the protruding particles, when the atomic% of the nonmetallic element is Y and the atomic% of the metallic element is X, the value of Y / X is R, the R value is 0.3. It exists in the range of ≦ R ≦ 0.6. On the other hand, since the macro particle is mainly composed of a metal component, the R value is 0.2 or less and is distinguished.
Protruding particles having a thickness of 5 nm or more and less than 200 nm on the surface of the film exhibit excellent wear resistance in a wear environment. The mechanism is that projecting particles composed of nano-size increase the surface area of the hard coating surface and form a lubricating layer at the interface in a wear environment. Further, this characteristic protruding particle has at least two types of nitride, carbide, sulfide, boride, oxide selected from Si, Al, Ti, Cr, Nb, Mo, B, and W as a metal component. It is preferable in that it is formed of any one of the above or a solid solution or a mixture thereof and exhibits an excellent wear resistance effect.
本願発明の皮膜表面にある５ｎｍ以上、２００ｎｍ未満の突起状粒子は、皮膜表面の任意に選択される１０μｍ２の範囲に、５０個以上、５００個未満で構成される場合、優れた耐摩耗効果を発揮するため好ましい形態である。突起状粒子が任意に選択される１０μｍ２の範囲に、５０個未満の場合、耐摩耗性は改善されない。また５００個以上から構成される場合、皮膜が極めて脆くなり、耐剥離性が急激に低下し異常摩耗が進行する。但し、本願発明の突起状粒子は被加工物に接する部材表面のうち、どの部位であってもその効果を発揮することができ、必ずしも部材全体にわたって本願発明を満足する必要は無い。 Protruding particles of 5 nm or more and less than 200 nm on the film surface of the present invention have an excellent wear resistance effect when they are composed of 50 or more and less than 500 particles in the arbitrarily selected range of 10 μm 2 on the film surface. This is a preferable form. In the range of 10 μm 2 where the protruding particles are arbitrarily selected, when the number is less than 50, the wear resistance is not improved. Further, when it is composed of 500 or more, the coating becomes extremely brittle, the peel resistance rapidly decreases, and abnormal wear proceeds. However, the projecting particles of the present invention can exert the effect at any part of the surface of the member in contact with the workpiece, and it is not always necessary to satisfy the present invention over the entire member.
被覆部材の用途は、切削工具、金型、軸受け、ダイス、ロール等、高硬度が要求される耐摩耗部材である。切削工具としてはエンドミル、ドリル、ホブ、リーマ、ルーター、カッター、クリスマスカッター、ブローチ、刃先交換型切削インサート等の切削工具が最適である。これらの被覆部材は特に耐摩耗性の改善効果が大きく工具寿命が向上する。特に切削工具が転削工具であり、その部材直径が１ｍｍ未満の工具において、耐摩耗性の改善が著しく好ましい。
本願発明の物理蒸着による皮膜の被覆方法は、表面平滑性及び潤滑性の観点からＭＳ法であることが好ましい。フィルター方式アークイオンプレーティング法（以下、ＦＡＩＰ法と言う。）、プラズマ化学蒸着法（以下、ＰＣＶＤ法と言う。）との組み合せにより被覆することもできる。以下、本願発明を実施例に基づいて説明するが、本願発明は下記実施例に限定されるものではなく、使用分野により適宜変更することができる。
The use of the covering member is a wear-resistant member that requires high hardness, such as a cutting tool, a die, a bearing, a die, and a roll. Cutting tools such as an end mill, a drill, a hob, a reamer, a router, a cutter, a Christmas cutter, a broach, and a cutting edge exchangeable cutting insert are optimal as the cutting tool. These covering members are particularly effective in improving the wear resistance and improve the tool life. In particular, the cutting tool is a turning tool, and in a tool having a member diameter of less than 1 mm, improvement in wear resistance is remarkably preferable.
The coating method of the film by physical vapor deposition of the present invention is preferably the MS method from the viewpoint of surface smoothness and lubricity. It can also be coated by a combination of a filter type arc ion plating method (hereinafter referred to as FAIP method) and a plasma chemical vapor deposition method (hereinafter referred to as PCVD method). Hereinafter, although this invention is demonstrated based on an Example, this invention is not limited to the following Example, It can change suitably by the field of use.
基体として、Ｃｏ含有量：８重量％、Ｃｒ含有量：０．７重量％、ＶＣ含有量：０．２重量％、硬度がＨＲＡ９４．２の超硬合金を用い、Ｒ０．１ｍｍ、２枚刃ボールエンドミル、ドリルを作成した。基体は脱脂洗浄を実施し、ＭＳ装置の容器内の冶具に配置した。冶具は３回転／分で自公転する。基体の温度は５５０℃となるよう加熱、排気を行った。Ａｒガスを容器内に導入し、容器内に設けられたカソード電極とアノード電極の間で放電によってＡｒのイオン化を行った。同時に基体にパルス状のバイアス電圧を印加した。このパルス状のバイアス電圧は、負バイアス電圧が２００Ｖ、９０％、正バイアス電圧が０Ｖ、１０％、周波数を２０ｋＨｚとした。イオン化されたＡｒは基体に衝突し、基体のクリーニング及び活性化処理を行った。このとき、基体のクリーニング効率や活性度をより高めるためにＸｅ、Ｋｒ、Ｈ２等を複合的に用いることも有効である。Ａｒ及びもしくはその他のガス及び反応ガスとして窒素を容器内に導入し、全体の圧力を５８０ｍＰａ、バイアス電圧を−１００Ｖに設定した。容器内に複数配置したＭＳ蒸発源に設置された皮膜の金属成分となるターゲット１つあたり４ｋＷの電力を供給し、ターゲット上でスパッタ放電を行い、バイアス電圧が印加された基体上に層厚で約３μｍの皮膜の形成を行った。このとき必要に応じ最下層を形成した。Ｎ、Ｃ、Ｏ、Ｂ、Ｓを皮膜内に含有させる手段としては、導入ガスとして添加する以外にも、ターゲットに添加する方法、成膜圧力レベル、窒素との混合ガスとして添加することも可能である。
ターゲット１及びターゲット２には、原子％比でＴｉ／Ｓｉ＝７５／２５のターゲットを設置し、ターゲット３及びターゲット４には、原子％比でＡｌ／Ｔｉ＝５５／４５のターゲットを設置し、まず初めにターゲット３及びターゲット４により（ＡｌＴｉ）Ｎを２μｍ、続いてターゲット１及びターゲット２により（ＴｉＳｉ）Ｎを１μｍ積層した硬質皮膜を被覆し、これを本発明例１とした。表１、２に本発明例１の皮膜組成、膜厚、成膜方法、突起状粒子の凹凸、数、皮膜硬度、面粗さ、最下層の情報、層構造等を示す。最下層は、必要に応じて皮膜の下地層として採用した。
表１、２に示す様に、種々組成、膜厚等に変更を施した本発明例２から３０を作成した。これらは特に断りがない限り、本発明例１に準ずる方法により作成した。表１中に記載する基体は全てＣｒ：０．７重量％含有の基体を使用した。また、成膜方法の欄でＭＳはスパッタリング法、ＦＡＩＰはファイルターアークイオンプレーティング法、ＰＣＶＤはプラズマ化学蒸着を示す。最下層は、必要に応じて皮膜の下地層として採用した。
比較例も表１、２に併記する。比較例３１から３３は通常のＡＩＰ法、比較例３４、３５はＭＳ法により被覆を行った。
As the substrate, a cemented carbide having a Co content of 8% by weight, a Cr content of 0.7% by weight, a VC content of 0.2% by weight and a hardness of HRA 94.2, R0.1 mm, 2 blades A ball end mill and drill were created. The substrate was degreased and cleaned and placed on a jig in the container of the MS apparatus. The jig revolves at 3 revolutions / minute. The substrate was heated and exhausted so that the temperature of the substrate was 550 ° C. Ar gas was introduced into the container, and Ar was ionized by discharge between a cathode electrode and an anode electrode provided in the container. At the same time, a pulsed bias voltage was applied to the substrate. The pulsed bias voltage was set such that the negative bias voltage was 200 V, 90%, the positive bias voltage was 0 V, 10%, and the frequency was 20 kHz. The ionized Ar collided with the substrate, and the substrate was cleaned and activated. At this time, it is also effective to use Xe, Kr, H 2 and the like in combination in order to further increase the cleaning efficiency and activity of the substrate. Ni was introduced into the container as Ar and / or other gas and reaction gas, the whole pressure was set to 580 mPa, and the bias voltage was set to −100V. A power of 4 kW is supplied to each target, which is a metal component of the film placed in the MS evaporation source disposed in the container, and sputter discharge is performed on the target, and the layer thickness is applied to the substrate on which a bias voltage is applied. A film having a thickness of about 3 μm was formed. At this time, a lowermost layer was formed as necessary. As a means for containing N, C, O, B, and S in the film, in addition to adding as an introduction gas, a method of adding to a target, a film forming pressure level, and a mixed gas with nitrogen can also be added. It is.
Target 1 and target 2 are provided with a target of Ti / Si = 75/25 in atomic percent ratio, target 3 and target 4 are provided with a target of Al / Ti = 55/45 in atomic percent ratio, First, the target 3 and the target 4 were coated with a hard film in which (AlTi) N was laminated at 2 μm, and then the target 1 and the target 2 were laminated with 1 μm of (TiSi) N. Tables 1 and 2 show the coating composition, the film thickness, the film forming method, the unevenness of the protruding particles, the number, the coating hardness, the surface roughness, the information on the lowermost layer, the layer structure, etc. The lowermost layer was adopted as an underlayer for the film as required.
As shown in Tables 1 and 2, Invention Examples 2 to 30 in which various compositions and film thicknesses were changed were prepared. These were prepared by a method according to Inventive Example 1 unless otherwise specified. The substrates described in Table 1 were all substrates containing 0.7% by weight of Cr. In the column of the film formation method, MS indicates sputtering, FAIP indicates filer arc ion plating, and PCVD indicates plasma chemical vapor deposition. The lowermost layer was adopted as an underlayer for the film as required.
Comparative examples are also shown in Tables 1 and 2. Comparative Examples 31 to 33 were coated by a normal AIP method, and Comparative Examples 34 and 35 were coated by an MS method.
皮膜表面の突起状粒子の観察方法について述べる。図１は本発明例１、図２は比較例３１の皮膜表面の走査型電子顕微鏡写真を示す。本発明例１の皮膜表面にはマクロパーティクルはほとんど存在していない。一方、比較例３１の皮膜表面には複数のマクロパーティクルが存在していた。更に、図３は図１の拡大写真を、図４は図２の拡大写真を示す。本発明例１の皮膜表面は、複数の突起状粒子で構成され、本願発明の皮膜の特徴的な表面形態を示す。この突起状粒子は摩耗環境下において、優れた耐摩耗性を発揮する。一方、比較例３１の皮膜表面は、突起状粒子は存在していない。
皮膜表面の突起状粒子の測定方法について述べる。図５は図３に対応した箇所の原子間力顕微鏡写真を、図６は図４に対応した箇所の原子間力顕微鏡写真を示す。図５と図６の比較から、本発明例１の皮膜表面は突起状粒子で構成されていることが分かる。図７、図８は、図５の表面の凹凸を定量的に測定した結果を示す。本発明例１の皮膜表面には約１００ｎｍ未満の微細な凹凸が存在していた。一方、図９、図１０は、図６の表面の凹凸を定量的に示す。比較例３１の皮膜表面には２００ｎｍ未満の凹凸は存在していなかった。図１１は本発明例１の皮膜表面について倍率１万倍の拡大写真を示す。１０μｍ２範囲内にある突起状粒子の数は、写真内の任意の位置に１０μｍ２の領域を設け、その範囲内にある界面が存在する粒子の数を測定した。この方法により、突起状粒子の数が５０個以上、３５００個未満であることを確認した。ここで、本願発明の耐摩耗皮膜表面の５ｎｍ以上、２００ｎｍ未満の凹凸を有する突起状粒子の形成、１０μｍ２範囲の突起状粒子の数、表面粗さ、及び皮膜内の酸素含有量は被覆条件、ターゲット、被覆前処理により総合的に決定される。
A method for observing the protruding particles on the surface of the film will be described. 1 shows a scanning electron micrograph of the coating surface of Example 1 of the present invention and FIG. There are almost no macro particles on the surface of the coating of Example 1 of the present invention. On the other hand, a plurality of macro particles were present on the coating surface of Comparative Example 31. 3 shows an enlarged photograph of FIG. 1, and FIG. 4 shows an enlarged photograph of FIG. The coating surface of Example 1 of the present invention is composed of a plurality of protruding particles and exhibits a characteristic surface form of the coating of the present invention. The protruding particles exhibit excellent wear resistance in a wear environment. On the other hand, no protruding particles are present on the coating surface of Comparative Example 31.
A method for measuring the protruding particles on the film surface will be described. 5 shows an atomic force micrograph of a location corresponding to FIG. 3, and FIG. 6 shows an atomic force micrograph of a location corresponding to FIG. From the comparison between FIG. 5 and FIG. 6, it can be seen that the coating surface of Example 1 of the present invention is composed of protruding particles. 7 and 8 show the results of quantitative measurement of the irregularities on the surface of FIG. On the surface of the film of Example 1 of the present invention, fine irregularities of less than about 100 nm were present. On the other hand, FIGS. 9 and 10 quantitatively show the irregularities on the surface of FIG. There were no irregularities of less than 200 nm on the surface of the film of Comparative Example 31. FIG. 11 shows an enlarged photograph of the surface of the film of Example 1 of the present invention at a magnification of 10,000 times. As for the number of protruding particles in the 10 μm 2 range, a region of 10 μm 2 was provided at an arbitrary position in the photograph, and the number of particles having an interface in the range was measured. By this method, it was confirmed that the number of protruding particles was 50 or more and less than 3500. Here, the formation of protruding particles having irregularities of 5 nm or more and less than 200 nm on the surface of the wear-resistant coating of the present invention, the number of protruding particles in the 10 μm 2 range, the surface roughness, and the oxygen content in the coating are the coating conditions , Target, and pre-coating pre-treatment.
本発明例１から３０、比較例３１から３５の皮膜を被覆工具に適用し、耐摩耗性を評価するために切削評価を実施した。切削評価条件を以下に示す。切削評価結果は、逃げ面摩耗幅が０．１ｍｍに達した時の切削長、もしくは不安定な加工状態として、例えば火花発生、異音、加工面のむしれ、焼け、折損等などの状態に達した時の切削長を切削寿命とした。表１中では１０ｍまたは１０穴以下を切り捨てて表示した。
（切削試験１）
工具：Ｒ０．１ｍｍ、２枚刃ボールエンドミル
切削方法：底面超高速仕上げ加工
被削材：冷間ダイス鋼、ＨＲＣ６０
切り込み：軸方向、０．０１ｍｍ、径方向、０．０１ｍｍ
主軸回転数：５０ｋｍｉｎ−１
テーブル送り：１ｍ／ｍｉｎ
切削油：無し、ドライ切削
（切削試験２）
工具：Ｒ５ｍｍ、２枚刃ボールエンドミル
切削方法：底面超高速仕上げ加工
被削材：冷間ダイス鋼、ＨＲＣ６０
切り込み：軸方向、０．０１ｍｍ、径方向、０．０１ｍｍ
主軸回転数：３０ｋｍｉｎ−１
テーブル送り：５ｍ／ｍｉｎ
切削油：無し、ドライ切削
（切削試験３）
工具：φ６ｍｍ、２枚刃ソリッドドリル
切削方法：止まり穴加工
被削材：ＳＣＭ４４０、ＨＲＣ３０
切削速度：１５０ｍ／ｍｉｎ−１
送り速度：０．１ｍｍ／ｒｅｖ
切削油：水溶性切削液の外部給油
The coatings of Invention Examples 1 to 30 and Comparative Examples 31 to 35 were applied to a coated tool, and cutting evaluation was performed in order to evaluate wear resistance. The cutting evaluation conditions are shown below. The result of cutting evaluation is that the cutting length when the flank wear width reaches 0.1 mm, or an unstable machining state, such as the occurrence of sparks, abnormal noise, flaking of the machining surface, burning, breakage, etc. The cutting length when reaching the cutting life was defined as the cutting life. In Table 1, 10 m or 10 holes or less are cut off and displayed.
(Cutting test 1)
Tool: R0.1mm, 2-flute ball end mill Cutting method: Ultra-high-speed bottom machining Work material: Cold die steel, HRC60
Cutting: axial direction, 0.01 mm, radial direction, 0.01 mm
Spindle speed: 50kmin- 1
Table feed: 1m / min
Cutting oil: None, dry cutting (cutting test 2)
Tool: R5mm, 2-flute ball end mill Cutting method: Ultra-high speed finishing at the bottom Work material: Cold die steel, HRC60
Cutting: axial direction, 0.01 mm, radial direction, 0.01 mm
Spindle speed: 30kmin- 1
Table feed: 5m / min
Cutting oil: None, dry cutting (cutting test 3)
Tool: φ6mm, 2-flute solid drill Cutting method: blind hole processing Material: SCM440, HRC30
Cutting speed: 150 m / min −1
Feeding speed: 0.1mm / rev
Cutting oil: External lubrication of water-soluble cutting fluid
本発明例１と比較例３１を比較すると、皮膜組成ほぼ同一であが、ＡＩＰ法で被覆した比較例３１はマクロパーティクルが多数存在し、面粗さの数値が大きかった。また突起状粒子が存在しないため、耐摩耗性が劣っていた。同様に、本発明例１１に対する比較例３２、本発明例１９に対する比較例３３においても同じ現象が確認できた。ＭＳ法を採用した本発明例１から２８にＦＡＩＰ法を用いた本発明例２９及びＦＡＩＰ法とＰＣＶＤ法とを併用した複合プロセスの本発明例３０も含めると、ＡＩＰ法で被覆した比較例は何れも本発明例よりも劣る結果となった。また本願発明の構成を達成する上で、ＭＳ法が最適であった。本発明例１から本発明例６、比較例３４、比較例３５を比較した。突起状粒子の凹凸状態と個数について比較することができる。本発明例１から本発明例６は夫々の評価試験１から３について優れた結果を示した。また突起状粒子は、最上層の皮膜と略同一組成を有し、突起状粒子の凹凸は５ｎｍ以上、２００ｎｍ以下であった。これらの本発明例から、突起状粒子の個数を５０個以上、３５００個未満とする条件が適していることを確認した。一方、比較例３４は、突起状粒子の凹凸が５ｎｍよりも低くなる場合であり耐摩耗性の改善は認められなかった。比較例３５は、突起状粒子の凹凸が２５０ｎｍの場合であり耐摩耗性の改善は確認されなかった。本発明例７の皮膜硬度は７２ＧＰａ、本発明例８の皮膜硬度は２８ＧＰａの場合である。皮膜硬度としては７２ＧＰａでも許容範囲である。７５ＧＰａを超えると被覆後に剥離が生じ、耐摩耗性の評価ができない。皮膜硬度が２８ＧＰａの場合は、耐摩耗性が低下する傾向にある。好ましい皮膜硬度は３０ＧＰａ以上、７５ＧＰａ以下である。本発明例９、本発明例１０は、面粗度が本発明例１と比較するとやや劣る。本願発明の好ましい面粗度の範囲は、０．５μｍＲｙ以下、且つ０．０５μｍＲａ以下である。本発明例１２は、（ＴｉＳｉ）（ＮＯ）皮膜単一層の場合を示す。本発明例１と比較した場合、２層以上の積層膜として構成した方が、耐摩耗性に優れる結果となった。本発明例１４は、最下層を約２００ｎｍ被覆した後、膜厚が約２０００ｎｍまで最下層及び被覆層の両方の蒸発源を同時に稼動させ、被覆部材が回転機構を有していることから、実際にはナノ厚さの積層膜となっていた。その後、１０００ｎｍの最上層を被覆し、総膜厚を３０００ｎｍとした。混合積層膜を用いることにより、耐摩耗性を更に改善することが可能であり、好ましい本願発明の構成である。本発明例２１も本発明例１４と同様な成膜方法により作成した。本発明例２０と比較しても耐摩耗性に優れていた。 本発明例１５は、皮膜組成が（ＳｉＷ）Ｎ、本発明例１６は（ＳｉＣｒ）Ｎ、本発明例１７は（ＳｉＴｉ）Ｎ、本発明例１８は（ＳｉＡｌＣｒ）（ＮＯ）、本発明例２２は（ＳｉＮｂ）Ｎ、本発明例２３、本発明例２４は（ＳｉＣｒＢ）Ｎ、本願発明例２５は（ＳｉＢ）（ＮＯＣ）、本発明例２６は（ＳｉＡｌ）（ＮＯ）、本発明例２７は（ＳｉＴｉＭｏ）（ＮＯＳ）の場合を示した。これらは何れも比較例３１、比較例３２、比較例３３に比べて、耐摩耗性に優れていた。特に本発明例２７の（ＳｉＴｉＭｏ）（ＮＯＳ）の被覆方法は、被覆装置内に複数配置したターゲットのうちＳｉＴｉターゲットとＭｏＳ２ターゲットを設置した蒸発源を同時に稼動させて成膜を行った。この場合、ＳｉＴｉを高濃度で含有する層と、ＭｏＳを高濃度で含有する層との積層膜となっていると考えられる。本発明例２８は、基体にＶを含有しない場合を示す。本発明例１と比較すると、Ｖを含有した方が耐摩耗性に優れる結果となった。本願発明の皮膜と基体成分の相乗効果により、耐摩耗性を改善した結果である。基体のＶ含有量、Ｃｒ含有量が２．６重量％以上含有する場合は、切削初期でチッピングが発生し、耐摩耗性の評価ができなかった。 When Example 1 of the present invention and Comparative Example 31 were compared, the film composition was almost the same, but Comparative Example 31 coated with the AIP method had a large number of macroparticles and a large surface roughness value. Moreover, since there were no protruding particles, the wear resistance was poor. Similarly, the same phenomenon could be confirmed in Comparative Example 32 for Invention Example 11 and Comparative Example 33 for Invention Example 19. Including the present invention example 29 using the FAIP method and the present invention example 30 of the combined process using the FAIP method and the PCVD method in the present invention examples 1 to 28 employing the MS method, the comparative example coated with the AIP method is In either case, the results were inferior to those of the examples of the present invention. Further, the MS method was optimal in achieving the configuration of the present invention. Invention Example 1 to Invention Example 6, Comparative Example 34, and Comparative Example 35 were compared. It can compare about the uneven | corrugated state and number of protrusion-like particles. Invention Example 1 to Invention Example 6 showed excellent results for the respective evaluation tests 1 to 3. Further, the protruding particles had substantially the same composition as the uppermost film, and the unevenness of the protruding particles was 5 nm or more and 200 nm or less. From these examples of the present invention, it was confirmed that the condition that the number of protruding particles was 50 or more and less than 3500 was suitable. On the other hand, in Comparative Example 34, the unevenness of the protruding particles was lower than 5 nm, and no improvement in wear resistance was observed. In Comparative Example 35, the unevenness of the protruding particles was 250 nm, and no improvement in wear resistance was confirmed. The film hardness of Invention Example 7 is 72 GPa, and the film hardness of Invention Example 8 is 28 GPa. As the film hardness, 72 GPa is acceptable. If it exceeds 75 GPa, peeling occurs after coating, and wear resistance cannot be evaluated. When the film hardness is 28 GPa, the wear resistance tends to decrease. The preferred film hardness is 30 GPa or more and 75 GPa or less. Invention Example 9 and Invention Example 10 are slightly inferior in surface roughness to Invention Example 1. The preferable surface roughness range of the present invention is 0.5 μmRy or less and 0.05 μmRa or less. Invention Example 12 shows the case of a (TiSi) (NO) coating single layer. When compared with Example 1 of the present invention, a configuration in which two or more laminated films were formed resulted in excellent wear resistance. In Example 14 of the present invention, since the lowermost layer and the coating layer were operated at the same time until the film thickness was about 2000 nm after the lowermost layer was coated by about 200 nm, and the coating member had a rotation mechanism, It was a nano-thick laminated film. Thereafter, the uppermost layer of 1000 nm was covered, and the total film thickness was 3000 nm. By using the mixed laminated film, it is possible to further improve the wear resistance, which is a preferable configuration of the present invention. Invention Example 21 was also produced by the same film forming method as that of Invention Example 14. Even compared with Example 20 of the present invention, the wear resistance was excellent. Invention Example 15 has a coating composition of (SiW) N, Invention Example 16 has (SiCr) N, Invention Example 17 has (SiTi) N, Invention Example 18 has (SiAlCr) (NO), and Invention Example 22 Is (SiNb) N, Invention Example 23, Invention Example 24 is (SiCrB) N, Invention Example 25 is (SiB) (NOC), Invention Example 26 is (SiAl) (NO), and Invention Example 27 is The case of (SiTiMo) (NOS) is shown. These were all excellent in wear resistance as compared with Comparative Example 31, Comparative Example 32, and Comparative Example 33. In particular, the coating method of (SiTiMo) (NOS) of Example 27 of the present invention was performed by simultaneously operating an evaporation source having a SiTi target and a MoS2 target among a plurality of targets arranged in the coating apparatus. In this case, it is thought that it is a laminated film of a layer containing SiTi at a high concentration and a layer containing MoS at a high concentration. Invention Example 28 shows a case where V is not contained in the substrate. Compared with Example 1 of the present invention, the results containing V were superior in wear resistance. This is a result of improving the wear resistance by the synergistic effect of the coating of the present invention and the base component. When the V content and Cr content of the substrate were 2.6% by weight or more, chipping occurred at the beginning of cutting, and the wear resistance could not be evaluated.
Claims (5)
The covering member according to claim 1, wherein the coating method is a sputtering method.
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