JP2007217771A - Hard film coated member and its manufacturing method - Google Patents
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本願発明は、イオン注入に関すし、より詳細には、イオン注入により基体表面を強化し、被覆層との密着を強化した硬質皮膜被覆部材に関する。 The present invention relates to ion implantation, and more particularly, to a hard film-coated member in which a substrate surface is reinforced by ion implantation and adhesion with a coating layer is reinforced.
基体表面に窒素をイオン注入する技術が、以下の特許文献１から３に開示されている。 Techniques for implanting nitrogen ions into the substrate surface are disclosed in Patent Documents 1 to 3 below.
特許文献１は、超硬合金材料表面に窒素をイオン注入し、その注入層を表層より５０ｎｍ以上とする技術が開示されている。特許文献２は、超硬合金、サーメット、セラミックス、工具鋼の基材表面に窒素をイオン注入し、表面部分に改質層を形成する技術を開示している。特許文献３は、超硬合金、セラミックスなどの基材の表層内部にイオン注入し、密着性を補助する窒化層を形成する技術を開示している。そこで本願発明の目的は、耐酸化性、耐摩耗性に優れた硬質皮膜について、特に密着性を改善した硬質皮膜被覆部材を提供することである。 Patent Document 1 discloses a technique in which nitrogen is ion-implanted on the surface of a cemented carbide material and the injection layer is set to 50 nm or more from the surface layer. Patent Document 2 discloses a technique in which nitrogen is ion-implanted into the base material surfaces of cemented carbide, cermet, ceramics, and tool steel to form a modified layer on the surface portion. Patent Document 3 discloses a technique for forming a nitride layer that assists adhesion by ion implantation into the surface layer of a base material such as cemented carbide or ceramics. Accordingly, an object of the present invention is to provide a hard film-coated member having improved adhesion, particularly with respect to a hard film having excellent oxidation resistance and wear resistance.
本願発明の硬質皮膜を被覆した部材において、基体に硬質皮膜を被覆した部材において、該硬質皮膜は、金属元素とＮを有し、該基体の表面はＮ元素富化領域を有し、該Ｎ元素富化領域は該基体の表面から深さ方向に１μｍ以内に形成されていることを特徴とする硬質皮膜被覆部材である。上記構成を採用することにより、耐酸化性、耐摩耗性に優れた硬質皮膜を維持しつつ、硬質皮膜と基体間の密着性が改善され、優れた硬質皮膜被覆部材を提供することができる。 In the member coated with the hard coating of the present invention, in the member coated with the hard coating on the substrate, the hard coating has a metal element and N, the surface of the substrate has an N element-enriched region, and the N The element-enriched region is a hard coating member characterized by being formed within 1 μm in the depth direction from the surface of the substrate. By adopting the above configuration, the adhesion between the hard coating and the substrate is improved while maintaining a hard coating excellent in oxidation resistance and wear resistance, and an excellent hard coating coating member can be provided.
本願発明の硬質皮膜被覆部材において、基体のＮ元素富化領域のＮ含有量を原子％でＱ値とし、該基体の内部のＮ含有量を原子％でＰ値とした時、Ｑ＞０、Ｐ≧０、０＜（Ｑ−Ｐ）≦１０であることが好ましい。また、Ｎ元素富化領域をＸ線光電子分光分析したとき、３１から３２ｅＶの範囲と、３３から３５ｅＶの範囲とにピークを有することが好ましい。硬質皮膜被覆部材の基体は炭化タングステン基超硬合金、サーメット合金、高速度鋼、合金工具鋼の何れかであることが好ましい。より好ましくは、硬質皮膜被覆部材の製造方法において、基体表面にＮ元素のイオン注入を行う第１の工程と、硬質皮膜を被覆する第２の工程とから成り、該第１の工程において該Ｎ元素富化領域を、深さ方向に１μｍ以内の領域に調整する。 In the hard coating member of the present invention, when the N content in the N element-enriched region of the substrate is Q value in atomic% and the N content in the substrate is P value in atomic%, Q> 0, It is preferable that P ≧ 0 and 0 <(Q−P) ≦ 10. Further, when the N element-enriched region is analyzed by X-ray photoelectron spectroscopy, it is preferable to have peaks in the range of 31 to 32 eV and in the range of 33 to 35 eV. The base of the hard coating member is preferably any of tungsten carbide base cemented carbide, cermet alloy, high speed steel, and alloy tool steel. More preferably, in the method of manufacturing a hard film covering member, the method includes a first step of implanting N element ions on the surface of the substrate and a second step of covering the hard film. The element-enriched region is adjusted to a region within 1 μm in the depth direction.
本願発明によって、耐酸化性、耐摩耗性に優れた硬質皮膜を維持しつつ、硬質皮膜と基体間の密着性が改善され、優れた硬質皮膜被覆部材と、その製造方法を提供することができた。 According to the present invention, while maintaining a hard film excellent in oxidation resistance and abrasion resistance, adhesion between the hard film and the substrate is improved, and an excellent hard film coated member and a method for producing the same can be provided. It was.
本願発明の硬質皮膜被覆部材は、密着性を改善させるために、例えばイオン注入法を用いて基体表面にあらかじめＮを含有するように調整し、その後、物理蒸着（以下、ＰＶＤと記す。）法等により硬質皮膜を被覆したものである。硬質皮膜直下の基体表面には、Ｎ元素富化領域が基体の表面から深さ方向に１μｍ以内に形成されている必要がある。この理由は、ＰＶＤ法による硬質皮膜被覆の前処理として、あらかじめ超硬合金の基体表面にＮを含有させることで、基体表面近傍の酸化物が除去されるからである。また、基体表面の１部が窒化されることにより、例えばＰＶＤ法によって硬質皮膜が被覆され、この硬質皮膜は４ａ、５ａ、６ａ族、Ａｌ、Ｂ、Ｓｉから選択される１種以上の金属元素、Ｎと、Ｃ、Ｏから選択される１種以上の非金属元素を有してもよい。例えば、ＰＶＤ法によってＴｉＮやＴｉ（ＣＮ）、（ＴｉＡｌ）Ｎ、（ＴｉＡｌＳｉ）（ＯＮ）などのＮを含む硬質皮膜の結晶が、基体表面近傍の結晶とエピタキシャル関係になりやすい。その結果、基体と硬質皮膜との界面の密着強度が向上する。一方、基体表面に酸化物が存在すると、ＰＶＤ法で被覆するときに印加するバイアス電圧が、有効に作用しない。また絶縁性を有し、被覆対象以外の部分へ放電を発生して、品質上並びに成膜装置に大きな損傷をもたらす。ＰＶＤ法により硬質皮膜を被覆する際の密着性阻害因子の１つには、基体表面に形成される酸化物がある。Ｎ元素富化領域の厚さは、深さ方向の厚さで、少なくとも１ｎｍ以上である。好ましくは１０ｎｍ以上の領域に形成されていることである。これにより、上記効果が有効に作用する。量産製造安定性を考慮すると、確認のしやすい１０ｎｍ以上が好ましい。また、Ｎ元素富化領域の厚さが１μｍを超えて存在する場合、基体表面の靭性が低下する不都合がある。従って、ＰＶＤ法で硬質皮膜を被覆しても密着性は改善されるものの、耐欠損特性が大幅に低下する。そこで、Ｎ元素富化領域は基体の表面から深さ方向に１μｍ以内と設定した。 In order to improve the adhesion, the hard coating member of the present invention is adjusted to contain N in advance on the substrate surface using, for example, an ion implantation method, and then physical vapor deposition (hereinafter referred to as PVD) method. Etc., which are coated with a hard film. An N element-enriched region needs to be formed within 1 μm in the depth direction from the surface of the substrate on the surface of the substrate just below the hard coating. This is because the oxide in the vicinity of the substrate surface is removed by preliminarily containing N in the substrate surface of the cemented carbide as a pretreatment for coating the hard film by the PVD method. Further, by nitriding a part of the substrate surface, a hard film is coated by, for example, the PVD method, and this hard film is one or more metal elements selected from 4a, 5a, 6a group, Al, B, and Si. , N, and one or more nonmetallic elements selected from C and O may be included. For example, crystals of a hard film containing N such as TiN, Ti (CN), (TiAl) N, and (TiAlSi) (ON) are likely to have an epitaxial relationship with crystals near the substrate surface by the PVD method. As a result, the adhesion strength at the interface between the substrate and the hard coating is improved. On the other hand, when an oxide is present on the substrate surface, the bias voltage applied when coating by the PVD method does not work effectively. In addition, it has an insulating property, and a discharge is generated in a portion other than the object to be coated, resulting in serious damage in terms of quality and the film forming apparatus. One of the adhesion inhibiting factors when coating a hard film by the PVD method is an oxide formed on the surface of the substrate. The thickness of the N element-enriched region is at least 1 nm or more in the depth direction. Preferably, it is formed in a region of 10 nm or more. Thereby, the said effect acts effectively. Considering mass production stability, 10 nm or more which is easy to confirm is preferable. Further, when the thickness of the N element-enriched region exceeds 1 μm, there is a disadvantage that the toughness of the substrate surface is lowered. Therefore, even when the hard film is coated by the PVD method, the adhesion is improved, but the fracture resistance is greatly lowered. Therefore, the N element-enriched region was set within 1 μm in the depth direction from the surface of the substrate.
Ｎ含有量のＰ値、Ｑ値は、Ｑ＞０、Ｐ≧０、０＜（Ｑ−Ｐ）≦１０、であることが好ましい。この理由は、基体表面近傍の機械的強度、靭性を確保するためである。（Ｑ−Ｐ）値が１０を超えて大きいと、基体表面は高硬度化するものの靭性が低下し、その上に硬質膜を被覆しても界面直下が脆化しているために、耐衝撃強度が低下するため不都合である。更に、（Ｑ−Ｐ）＞０．１、であることが好ましい。Ｎ元素富化領域をＸ線光電子分光分析（以下、ＸＰＳ分析と記す。）をしたとき、３１から３２ｅＶの範囲と、３３から３５ｅＶの範囲とにピークを有することが好ましい。この理由は、超硬合金の主成分となるＷＣにＮが注入された場合にＷ（ＣＮ）化合物が形成され、これがピークとして現われるからである。基体は炭化タングステン基超硬合金、サーメット合金、高速度鋼、合金工具鋼の何れかであることが好ましい。この理由は、基体にＮを注入したときに、基体表面近傍にある化合物がＮと結びつき易いからである。しかし、サーメット合金の場合、Ｔｉ（ＣＮ）など１部Ｎが含まれた化合物が使用されている。そこで、他の炭化物であるＷＣ、ＴｉＣ、ＮｂＣ、Ｃｒ２Ｃ３、ＴａＣなどが、更にＮと結びつくことで、被覆される硬質皮膜の密着性が向上する。より好ましくは、ＷＣが主体に製造される超硬合金が望ましい。 The P value and Q value of the N content are preferably Q> 0, P ≧ 0, and 0 <(Q−P) ≦ 10. The reason for this is to ensure mechanical strength and toughness in the vicinity of the substrate surface. If the (QP) value is greater than 10, the toughness of the substrate surface is increased, but the toughness is reduced. Even if a hard film is coated on the surface, the area immediately below the interface becomes brittle. Is inconvenient. Furthermore, it is preferable that (QP)> 0.1. When the N element-enriched region is subjected to X-ray photoelectron spectroscopy analysis (hereinafter referred to as XPS analysis), it preferably has peaks in the range of 31 to 32 eV and in the range of 33 to 35 eV. This is because a W (CN) compound is formed when N is injected into WC, which is the main component of the cemented carbide, and this appears as a peak. The substrate is preferably any one of tungsten carbide base cemented carbide, cermet alloy, high speed steel, and alloy tool steel. This is because when N is injected into the substrate, a compound in the vicinity of the substrate surface is likely to be associated with N. However, in the case of a cermet alloy, a compound containing 1 part N such as Ti (CN) is used. Thus, other carbides such as WC, TiC, NbC, Cr 2 C 3 , TaC and the like are further combined with N, thereby improving the adhesion of the hard film to be coated. More preferably, a cemented carbide made mainly of WC is desirable.
基体表面にＮを含有させるには、イオン注入法を用い、減圧下においてＮを含有させることが好ましい。この理由は、Ｎイオン注入を行うことにより、基体表面に圧縮応力が付与され、その直上に、圧縮応力を有するＰＶＤ皮膜の被覆することにより、界面に発生する歪が少なく、密着性が向上するからである。これに対し、未処理の基体表面に、圧縮応力を有するＰＶＤ皮膜を被覆すると、ＰＶＤ皮膜の結晶格子に歪が発生する。この歪のために界面における密着性が改善されない。また、Ｎイオン注入を行うことにより、基体表面の１部が窒化されるため、特にＮを含む硬質皮膜の被覆においては、基体表面の結晶格子縞と硬質皮膜の格子縞とが連続するようになり、密着性が向上する。更に、イオン注入法の検討の結果、Ｎイオンを基体表面に注入することにより、表面の酸素が減る傾向を示すことを見出した。これに対して、例えば基体が超硬合金のとき、Ｎを含有した粉末原料を用いると、基体全体にＮを含有することになってしまう。その結果、基体そのものの靭性が低下する。また、超硬合金を用いた切削工具の激しい使用環境下では、容易にチッピングが発生し、大きな欠損を誘発する。更に、基体表面に軟化層が形成し、基体の塑性変形性や耐摩耗特性が低下する。このほかに鋼の表面処理では窒化処理法がある。しかし、基体表面に酸化物が形成しやすく、ＰＶＤ法による被覆時に悪影響を及ぼすため、不都合である。基体表面にＮイオンを注入するときの印加バイアス電圧は、１ｋｅＶから２００ｋｅＶまでの範囲が望ましい。イオン注入は、一般に１０ｋｅＶ以上のバイアス電圧を印加するが、本願発明では、１ｋｅＶ以上から注入可能である。１ｋｅＶを印加した場合、基体表面に富化されたＮは０．０１％であった。Ｎは分析の難しい元素であるが、２次イオン質量分析を用いることによって、ｐｐｍオーダーでの検出も可能である。極微量のＮ注入でも密着性向上の効果を有するが、量産において汎用的にＮが検出可能になるように５０ｋｅＶ以上で印加することが好ましい。しかし、２００ｋｅＶを超えるバイアス電圧では、Ｎイオンが基体表面に衝突するときのエネルギーが大きくなりすぎる。従って、イオン注入はなされるが、表面に空孔が発生し、表面粗さが悪くなり、その後の硬質皮膜の被覆により、基体表面と硬質皮膜界面に歪が発生し、密着性が低下するので好ましくない。一方、１ｋｅＶ未満でのＮイオン注入では、基体表面にＮがほとんど検出されず、その上に硬質皮膜を被覆すると密着性向上の効果が確認できない。本願発明を実施するにあたり、被覆装置はイオン注入と硬質皮膜が被覆可能な設備が併設されていることが好ましい。しかし、イオン注入を行った後、別の装置で硬質皮膜を被覆しても、同様の効果が得られる。Ｎイオン注入後のイオンプレーティングなどのＰＶＤ法にて硬質皮膜を考慮し、加熱状態でイオン注入を行うことによって、密着性が著しく向上する。従って、イオン注入とその後の硬質皮膜の被覆を同一装置で行う場合は、加熱状態でイオン注入することが望ましい。 In order to contain N on the surface of the substrate, it is preferable to contain N under reduced pressure by using an ion implantation method. The reason for this is that compressive stress is applied to the surface of the substrate by performing N ion implantation, and the PVD film having compressive stress is coated directly on the surface to thereby reduce the strain generated at the interface and improve the adhesion. Because. On the other hand, when a PVD film having a compressive stress is coated on the surface of the untreated substrate, distortion occurs in the crystal lattice of the PVD film. This distortion does not improve the adhesion at the interface. Further, by performing N ion implantation, a portion of the surface of the base is nitrided, so that the crystal lattice stripes on the surface of the base and the lattice stripes of the hard coating become continuous, particularly in the coating of the hard film containing N. Adhesion is improved. Furthermore, as a result of the examination of the ion implantation method, it has been found that the surface oxygen tends to decrease when N ions are implanted into the substrate surface. On the other hand, for example, when the substrate is a cemented carbide, if a powder raw material containing N is used, the entire substrate will contain N. As a result, the toughness of the substrate itself decreases. In addition, chipping easily occurs under a severe usage environment of a cutting tool using a cemented carbide and induces a large defect. Furthermore, a softening layer is formed on the surface of the base, and the plastic deformability and wear resistance of the base are reduced. In addition, there is a nitriding method for surface treatment of steel. However, it is inconvenient because an oxide is easily formed on the surface of the substrate and adversely affects the coating by the PVD method. The applied bias voltage when N ions are implanted into the substrate surface is preferably in the range of 1 keV to 200 keV. In ion implantation, a bias voltage of 10 keV or more is generally applied, but in the present invention, implantation can be performed from 1 keV or more. When 1 keV was applied, N enriched on the substrate surface was 0.01%. N is an element that is difficult to analyze, but detection in the ppm order is also possible by using secondary ion mass spectrometry. Even a very small amount of N injection has an effect of improving adhesion, but it is preferably applied at 50 keV or more so that N can be detected for general use in mass production. However, when the bias voltage exceeds 200 keV, the energy when N ions collide with the substrate surface becomes too large. Accordingly, although ion implantation is performed, vacancies are generated on the surface, the surface roughness is deteriorated, and the subsequent coating of the hard film causes distortion at the substrate surface and the interface of the hard film, so that the adhesiveness is decreased. Absent. On the other hand, in N ion implantation at less than 1 keV, N is hardly detected on the surface of the substrate, and if a hard film is coated thereon, the effect of improving adhesion cannot be confirmed. In carrying out the present invention, it is preferable that the coating apparatus is additionally provided with equipment capable of coating ion implantation and hard coating. However, the same effect can be obtained by coating the hard film with another apparatus after ion implantation. Adhesion is remarkably improved by performing ion implantation in a heated state in consideration of a hard film by a PVD method such as ion plating after N ion implantation. Therefore, when ion implantation and the subsequent coating of the hard film are performed with the same apparatus, it is desirable to perform ion implantation in a heated state.
イオン注入装置とアークイオンプレーティング（以下、ＡＩＰと記す。）を用いて、処理を行った。まず基体の超硬合金製インサート表面上にＮイオン注入を行った。イオン注入の印加電圧は１００ｋｅＶ、基体温度は２００から４００℃に維持した。イオン注入後、装置から基体を取り出した。そしてＡＩＰ装置内に装填し、（ＴｉＡｌ）Ｎ系硬質皮膜を被覆した。蒸発源には（ＴｉＡｌ）Ｎ皮膜の金属成分である、Ｔｉ、Ａｌを１００ａｔ％とした場合、Ｔｉ：５０ａｔ％、Ａｌ：５０ａｔ％となるようにターゲット組成を調整した。これによって、Ｔｉ−Ａｌ合金ターゲット種が限定されるものではない。また、その他の膜種については、必要な金属ターゲットを作成して使用した。反応ガスは、Ｎ２ガス、ＣＨ４ガス、Ａｒ／Ｏ２混合ガスを使用し、所定量の酸素や炭素が含まれる硬質皮膜を作成した。被覆条件は、基体温度を４００℃、バイアス電圧を、−４０Ｖから−１５０Ｖの範囲で印加した。皮膜は、（ＴｉＡｌ）Ｎ成膜以外に、ＴｉＮや（ＣｒＡｌ）Ｎ、（ＴｉＡｌＳｉ）Ｎ、（ＴｉＡｌＮｂ）Ｎも準備した。皮膜は、密着性が課題となっている皮膜を選定した。上記手法により本発明例１から１０、比較例１１から２０を作成した。表１に本発明例及び比較例、従来例の基体処理条件、皮膜等を示した。 Processing was performed using an ion implantation apparatus and arc ion plating (hereinafter referred to as AIP). First, N ion implantation was performed on the surface of the cemented carbide insert of the substrate. The applied voltage for ion implantation was maintained at 100 keV, and the substrate temperature was maintained at 200 to 400 ° C. After the ion implantation, the substrate was taken out from the apparatus. And it loaded in the AIP apparatus and coat | covered the (TiAl) N type | system | group hard film. As the evaporation source, when Ti and Al, which are metal components of the (TiAl) N film, are 100 at%, the target composition was adjusted so that Ti: 50 at% and Al: 50 at%. This does not limit the Ti—Al alloy target species. For other film types, necessary metal targets were prepared and used. The reaction gas, using N2 gas, CH4 gas, Ar / O 2 mixed gas to prepare a hard coating that contains a predetermined amount of oxygen and carbon. The coating conditions were a substrate temperature of 400 ° C. and a bias voltage in the range of −40V to −150V. In addition to (TiAl) N film formation, TiN, (CrAl) N, (TiAlSi) N, and (TiAlNb) N were also prepared. As the film, a film whose adhesion is a problem was selected. Inventive Examples 1 to 10 and Comparative Examples 11 to 20 were prepared by the above method. Table 1 shows the substrate processing conditions, films, etc. of the present invention example, comparative example, and conventional example.
表１に示す本発明例２と従来例２５について、図１に被覆を行う前の表面状態をＸＰＳ分析した結果を示す。本発明例２は、１２０ｋｅＶでＮイオン注入を施したものであり、一方の従来例２５は未処理品である。図１より、Ｎイオン注入を行った本発明例２は、Ｎイオン注入を行っていない従来例２５と比較してＷ−Ｏ結合を示すピーク強度が低かった。これは、超硬合金表面上の酸素量が低下していると考えられる。本発明例２は、Ｗ−Ｃ結合を示すピークが、３２、３４ｅＶ付近のＷ−Ｎのピークに近い位置にシフトしていることから、Ｎイオン注入を行うことで、超硬合金表面が部分的に窒化されていることがわかった。本発明例２は、ＡＩＰ法によって（ＴｉＡｌＳ）（ＣＮ）被覆を行った。超硬合金と硬質皮膜との界面状態を透過電子顕微鏡（以下、ＴＥＭと記す。）を用いて観察した結果を図２に示す。図２より、本発明例２は、Ｎイオン注入された超硬合金のＷＣ主体の粒子と、硬質皮膜の結晶との間で、整合性の有ることが確認された。これが密着性の向上に有効であった考えられる。注入されたＮイオンが超硬合金の基体内部方向にどの程度入り込んでいるかを、オージェ分析を用いて調査した。その結果を図３に示す。図３より、本発明例２は、超硬合金表面から内部に向かって０．４μｍの深さまでＮが存在していることがわかった。一方、比較例１８、１９は、バイアス電圧が大きかったため、２．８μｍ、２μｍと深くまでＮイオンが注入されていた。 FIG. 1 shows the results of XPS analysis of the surface state before coating for Invention Example 2 and Conventional Example 25 shown in Table 1. Inventive Example 2 is obtained by performing N ion implantation at 120 keV, while Conventional Example 25 is an untreated product. As shown in FIG. 1, Example 2 of the present invention in which N ions were implanted had a lower peak intensity showing W—O bonds than Conventional Example 25 in which N ions were not implanted. This is considered that the amount of oxygen on the surface of the cemented carbide decreases. In Example 2 of the present invention, the peak showing the WC bond is shifted to a position close to the W-N peak in the vicinity of 32, 34 eV. Was found to be nitrided. In Invention Example 2, (TiAlS) (CN) coating was performed by the AIP method. The result of observing the interface state between the cemented carbide and the hard film using a transmission electron microscope (hereinafter referred to as TEM) is shown in FIG. From FIG. 2, it was confirmed that Example 2 of the present invention has consistency between the WC-based particles of the cemented carbide in which N ions are implanted and the crystal of the hard coating. This is considered to be effective in improving the adhesion. The degree of penetration of the implanted N ions into the inside of the cemented carbide substrate was investigated using Auger analysis. The result is shown in FIG. From FIG. 3, it was found that in Example 2 of the present invention, N was present from the cemented carbide surface to the depth of 0.4 μm toward the inside. On the other hand, in Comparative Examples 18 and 19, since the bias voltage was large, N ions were implanted as deep as 2.8 μm and 2 μm.
次に、インサートホーニング部に皮膜剥離の有無を観察することができる切削諸元にて、剥離の有無を確認した。評価は、刃先の欠損又は摩耗等により工具が切削不能となるまで加工を行い、使用不能になったときの切削可能距離を工具寿命とした。表２に切削試験の結果を示した。
（切削諸元）
工具：特殊正面フライス
インサート形状：ＳＥＥ５３タイプ特殊形状
切削方法：ダウンカット方式
被削材形状：巾１００ｍｍ×長さ２５０ｍｍ
被削材：ＳＫＤ６１、硬さ、ＨＲＣ４２、ダイカスト金型用鋼種
切り込み量：２．０ｍｍ
切削速度：１５０ｍ／ｍｉｎ
１刃送り量：０．２ｍｍ／刃
切削油：なし
Next, the presence or absence of peeling was confirmed with the cutting specifications that can observe the presence or absence of film peeling on the insert honing portion. The evaluation was performed until the tool became uncut due to chipping or wear of the blade edge, and the cutting possible distance when the tool became unusable was defined as the tool life. Table 2 shows the results of the cutting test.
(Cutting specifications)
Tool: Special face milling insert shape: SEE53 type special shape Cutting method: Down-cut method Workpiece shape: width 100mm x length 250mm
Work material: SKD61, Hardness, HRC42, Steel type for die casting mold Cutting depth: 2.0mm
Cutting speed: 150 m / min
1-blade feed amount: 0.2 mm / blade Cutting oil: None
表２より、本発明例１から１０は、硬質皮膜被覆前のＮイオン注入により、切削性能が向上することがわかった。これは、硬質皮膜の密着性が向上しているために、切削加工により溶着現象を引き起こしても皮膜剥離が抑制されたからである。その結果、優れた切削性能が得られた。本発明例は、硬質皮膜の高い密着性が要求される加工において、その効果を発揮することがわかった。本発明例２、５は、６５ｍ、６１ｍの良好な切削寿命を示した。切削初期から欠損時までインサート刃先部における硬質皮膜の剥離がほとんど観察されず、正常摩耗が推移し寿命に至った。本発明例２は、（ＴｉＡｌ）Ｎ皮膜の硬度や潤滑特性を改善させるためにＣを添加し、更に潤滑特性を向上させるためにＳを添加した。溶着が発生する被加工物の加工では、硬質皮膜の密着性が十分に確保できてなければならない。また、潤滑特性も重要である。その点で本発明例２は、硬質皮膜に添加したＣやＳが相乗効果を示し、良好な結果を得ることができた。これは、密着性を改善することで、硬質皮膜の特性が十分に発揮されたからである。超硬合金の表面にＮイオン注入するときに印加するバイアス電圧が、１ｋｅＶから２００ｋｅＶまでの範囲であれば、その上に被覆する硬質皮膜の密着性が十分に確保された。従って、十分に満足の行く性能が引き出された。本発明例１、３、６と比較例１１、１３、１６を比較する。何れも硬質皮膜に略同一組成の（ＴｉＡｌ）Ｎを適用したが、被覆される前のＮイオン注入条件、即ちバイアス電圧によって、切削性能が大きく変化することがわかった。単に硬質皮膜を被覆する前にＮイオンを注入すれば良いのではなく、適正な添加条件が選定されることが非常に重要であった。本願発明は、硬質皮膜の被覆前にＮイオン注入を好適な状態と条件で行い、優れた密着性を得ることができた。密着性が改善されることによって、硬質皮膜の優れた特性を十分に引き出すことが可能となった。一方、比較例、従来例は、硬質皮膜の機械的特性の優れるものもあり、評価初期段階では摩耗が少なかった。しかし、次第に刃先温度が上昇し、溶着現象が発生し始めると、硬質皮膜が大きく剥離し、突発的に欠損に至ってしまった。比較例１８、１９は、バイアス電圧が大きく、２．８μｍ、２μｍと深くまでＮイオンが注入されていたことが原因で、基体表面の靭性が損なわれ、切削評価開始後１分もたたないうちに欠損した。 From Table 2, it was found that in the inventive examples 1 to 10, the cutting performance was improved by N ion implantation before the hard coating was coated. This is because the adhesion of the hard film is improved, and the film peeling is suppressed even if the welding phenomenon is caused by cutting. As a result, excellent cutting performance was obtained. It turned out that the example of this invention exhibits the effect in the process for which the high adhesiveness of a hard film is requested | required. Inventive Examples 2 and 5 showed good cutting lives of 65 m and 61 m. From the beginning of cutting to the time of chipping, almost no peeling of the hard coating was observed at the insert edge, and normal wear changed and the service life was reached. In Invention Example 2, C was added to improve the hardness and lubrication characteristics of the (TiAl) N film, and S was added to further improve the lubrication characteristics. In the processing of workpieces where welding occurs, sufficient adhesion of the hard coating must be ensured. Lubrication characteristics are also important. In that respect, Example 2 of the present invention showed a synergistic effect with C and S added to the hard film, and was able to obtain good results. This is because the characteristics of the hard film were sufficiently exhibited by improving the adhesion. When the bias voltage applied when N ions are implanted into the surface of the cemented carbide is in the range of 1 keV to 200 keV, the adhesion of the hard coating coated thereon is sufficiently secured. Therefore, sufficiently satisfactory performance was drawn. Invention Examples 1, 3, and 6 are compared with Comparative Examples 11, 13, and 16. In each case, (TiAl) N having the same composition was applied to the hard coating, but it was found that the cutting performance greatly varies depending on the N ion implantation conditions before coating, that is, the bias voltage. Rather than simply implanting N ions before coating the hard coating, it was very important to select the proper addition conditions. The present invention was able to obtain excellent adhesion by performing N ion implantation in a suitable state and conditions before coating with the hard coating. By improving the adhesion, the excellent properties of the hard coating can be fully extracted. On the other hand, some of the comparative examples and the conventional examples have excellent mechanical properties of the hard coating, and wear was small at the initial stage of evaluation. However, as the cutting edge temperature gradually increased and the welding phenomenon began to occur, the hard coating was largely peeled off, resulting in a sudden loss. In Comparative Examples 18 and 19, the bias voltage was large and N ions were implanted deeply to 2.8 μm and 2 μm, so the toughness of the substrate surface was impaired, and it took less than 1 minute after the start of cutting evaluation. I lost it.
Claims (5)
It consists of a first step of implanting N element ions on the surface of the substrate and a second step of covering the hard film, and in the first step, the N element-enriched region is within 1 μm in the depth direction. A manufacturing method of a hard coat covering member characterized by adjusting to a field.
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Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JP2011005582A (en) * | 2009-06-25 | 2011-01-13 | Kyocera Corp | Cutting tool |
| JP2011089199A (en) * | 2009-09-28 | 2011-05-06 | Hitachi Metals Ltd | Hard film excellent in lubricating characteristic, application method of the same, and tool for metal plastic working |
| WO2021187508A1 (en) * | 2020-03-19 | 2021-09-23 | 株式会社プラズマ総合研究所 | Nitriding treatment method and tungsten carbide-based cemented carbide alloy |
-
2006
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Cited By (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JP2011005582A (en) * | 2009-06-25 | 2011-01-13 | Kyocera Corp | Cutting tool |
| JP2011089199A (en) * | 2009-09-28 | 2011-05-06 | Hitachi Metals Ltd | Hard film excellent in lubricating characteristic, application method of the same, and tool for metal plastic working |
| WO2021187508A1 (en) * | 2020-03-19 | 2021-09-23 | 株式会社プラズマ総合研究所 | Nitriding treatment method and tungsten carbide-based cemented carbide alloy |
| CN115298348A (en) * | 2020-03-19 | 2022-11-04 | 株式会社等离子体综合研究所 | Nitriding method and tungsten carbide series super hard alloy |
| CN115298348B (en) * | 2020-03-19 | 2024-10-29 | 株式会社等离子体综合研究所 | Nitriding method and tungsten carbide-based cemented carbide |
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