JP2020104209A - Surface-coated cutting tool having hard coating layer exerting excellent chipping resistance - Google Patents
Surface-coated cutting tool having hard coating layer exerting excellent chipping resistance Download PDFInfo
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本発明は、合金鋼や高炭素鋼等の高速断続切削加工であっても、硬質被覆層が優れた耐チッピング性を備えることにより、長期の使用にわたって優れた切削性能を発揮する表面被覆切削工具（以下、被覆工具ということがある）に関するものである。 The present invention provides a surface-coated cutting tool that exhibits excellent cutting performance over a long period of use by providing a hard coating layer with excellent chipping resistance even in high-speed interrupted cutting of alloy steel, high-carbon steel, etc. (Hereinafter, sometimes referred to as a coated tool).
従来、炭化タングステン（以下、ＷＣで示す）基超硬合金等の工具基体（以下、工具基体という）の表面に、硬質被覆層として、Ｔｉ−Ａｌ系の複合炭窒化物層を蒸着法により被覆形成した被覆工具があり、これらは、優れた耐摩耗性を発揮することが知られている。
ただ、前記従来のＴｉ−Ａｌ系の複合炭窒化物層を被覆形成した被覆工具は、比較的耐摩耗性に優れるものの、高速断続切削条件で用いた場合にチッピング等の異常損耗を発生しやすいことから、硬質被覆層の改善についての種々の提案がなされている。
Conventionally, a Ti-Al-based composite carbonitride layer is coated as a hard coating layer on the surface of a tool substrate (hereinafter, referred to as a tool substrate) such as a tungsten carbide (hereinafter referred to as WC)-based cemented carbide by a vapor deposition method. There are coated tools formed which are known to exhibit excellent wear resistance.
However, the above-mentioned conventional tool coated with the Ti-Al-based composite carbonitride layer is relatively excellent in wear resistance, but is prone to abnormal wear such as chipping when used under high-speed intermittent cutting conditions. Therefore, various proposals have been made for improving the hard coating layer.
例えば、特許文献１には、基体上にＣＶＤ法により成膜された、厚さが１〜１６μｍで８５体積％以上のｆｃｃのＴｉ１−ｘＡｌｘＣｙＮｚ層（０．４０≦ｘ≦０．９５、０≦ｙ≦０．１０、０．８５≦ｚ≦１．１５）を有し、該層の結晶粒界にはＴｉ１−ｏＡｌｏＣｐＮｑ（０．９５≦ｏ≦１．００、０≦ｐ≦０．１０、０．８５≦ｑ≦１．１５、ｏ−ｘ≧０．０５）が析出している被覆工具が記載されている。 For example, in Patent Document 1, a Ti 1-x Al x C y N z layer (0.40≦x) having a thickness of 1 to 16 μm and an fcc of 85 vol% or more, which is formed on a substrate by a CVD method, is disclosed. ≦ 0.95,0 ≦ y ≦ 0.10,0.85 ≦ z ≦ 1.15) has, on the layer of the grain boundaries Ti 1-o Al o C p N q (0.95 ≦ o≦1.00, 0≦p≦0.10, 0.85≦q≦1.15, ox≧0.05) are described.
また、例えば、特許文献２には、単層又は多層の層系で被覆された被覆工具であって、該層系が、少なくとも１つの硬質材料複合層を有しており、該複合層が、主相としてＮａＣｌ型の面心立方構造を有するＴｉＡｌＣＮ及び六方晶ＡｌＮを含有している被覆工具において、該ＮａＣｌ型の面心立方構造を有するＴｉＡｌＣＮが、≧０．１μｍの結晶子サイズを有する微晶質ｆｃｃ−Ｔｉ1-xＡｌxＣyＮz（ここで、ｘ＞０．７５、ｙ＝０〜０．２５で、かつｚ＝０．７５〜１である）であり、かつ、該複合層がさらに粒界領域内に非晶質炭素を０．０１％〜２０％の質量割合で含有している被覆工具が記載されている。 Further, for example, Patent Document 2 discloses a coated tool coated with a single-layer or multi-layered layer system, the layer system having at least one hard material composite layer, and the composite layer comprising: In a coated tool containing TiAlCN having a NaCl-type face-centered cubic structure and hexagonal AlN as a main phase, the TiAlCN having a NaCl-type face-centered cubic structure has a crystallite size of ≧0.1 μm. crystalline fcc-Ti 1-x Al x C y N z ( wherein, x> 0.75, with y = 0-0.25, and a z = 0.75 to) a, and the A coated tool is described in which the composite layer further contains amorphous carbon in the grain boundary region in a mass proportion of 0.01% to 20%.
前記特許文献１に記載されているＣＶＤ法で蒸着形成したＴｉ１−ｘＡｌｘＣｙＮｚ層は、Ａｌの含有割合ｘを高め、また、ＮａＣｌ型の面心立方構造の結晶粒を形成させることができることから、所定の硬さを有し耐摩耗性に優れた硬質被覆層が得られるものの、高速断続切削加工に供したとき靭性に劣ることがあった。
また、前記特許文献２に記載されている被覆工具は、切削時において微細な結晶粒を有することから耐酸化性に劣るため、満足できる切削性能を発揮するとは言えないことがあった。
Wherein the Ti 1-x Al x C y N z layer formed deposited by the CVD method disclosed in Patent Document 1, increasing the proportion x of Al, also forming a crystal grain of the face-centered cubic structure of NaCl type Therefore, although a hard coating layer having a predetermined hardness and excellent in wear resistance can be obtained, when subjected to high speed intermittent cutting, the toughness may be poor.
Further, the coated tool described in Patent Document 2 is inferior in oxidation resistance because it has fine crystal grains at the time of cutting, and therefore, it may not be said that it exhibits satisfactory cutting performance.
そこで、本発明は前記課題を解決し、硬質被覆層の耐摩耗性、靭性を改善して、合金鋼および高炭素鋼等の高速断続切削等に供した場合であっても、長期の使用にわたって優れた耐チッピング性を発揮する被覆工具を提供することを目的とする。 Therefore, the present invention solves the above problems, improves the wear resistance of the hard coating layer, toughness, even when subjected to high-speed intermittent cutting of alloy steel and high carbon steel, etc., over a long period of use It is an object to provide a coated tool that exhibits excellent chipping resistance.
本発明者は、ＴｉとＡｌとの複合窒化物層または複合炭窒化物層（以下、これらを「ＴｉＡｌＣＮ層」と表すことがある）を少なくとも含む硬質被覆層を工具基体に設けた被覆工具の耐チッピング性の改善を図るべく、特に、Ａｌの含有割合について、硬質被覆層の層厚方向の変化、ＮａＣｌ型の面心立方構造を有する結晶粒の粒界近傍領域とそれ以外の領域における関係が、耐チッピング性の向上にどのような影響を与えるかについて鋭意検討した。 The inventor of the present invention provides a coated tool in which a hard coating layer including at least a composite nitride layer of Ti and Al or a composite carbonitride layer (hereinafter, these may be referred to as “TiAlCN layer”) is provided on a tool base. In order to improve the chipping resistance, in particular, with respect to the content ratio of Al, the change in the layer thickness direction of the hard coating layer, the relation between the grain boundary vicinity region of the crystal grain having the NaCl type face-centered cubic structure and the other region However, the present inventors have diligently studied how it affects the improvement of chipping resistance.
その結果、ＴｉＡｌＣＮ層におけるＡｌの含有割合に関し、
（１）被覆層の層厚方向において、工具表面に向かって増加し、かつ、
（２）工具基体表面に平行な方向（被覆層の層厚方向に垂直な方向）において、ＮａＣｌ型の面心立方構造を有する結晶粒の粒界近傍領域と該領域でない領域の間に所定の関係が成立するとき、
ＴｉＡｌＣＮ層の耐摩耗性、靭性が改善されて、合金鋼および炭素鋼等の高速断続切削等に供した場合であっても、長期の使用にわたって優れた耐チッピング性を発揮するという新規な知見を得た。
なお、ＴｉＡｌＣＮ層は、微量のＯやＣｌ等の不可避的に含まれる元素を有していても後述する発明の効果は損なわれない。
As a result, regarding the Al content in the TiAlCN layer,
(1) Increasing toward the tool surface in the layer thickness direction of the coating layer, and
(2) In a direction parallel to the tool substrate surface (direction perpendicular to the layer thickness direction of the coating layer), a predetermined distance is provided between a grain boundary vicinity region of crystal grains having a NaCl-type face-centered cubic structure and a region other than the grain boundary. When the relationship is established,
A new finding that the TiAlCN layer has improved wear resistance and toughness and exhibits excellent chipping resistance over long-term use even when subjected to high-speed intermittent cutting of alloy steel and carbon steel. Obtained.
It should be noted that the TiAlCN layer does not impair the effects of the invention described later even if it has a trace amount of elements such as O and Cl that are inevitably contained.
本発明は、前記知見に基づいてなされたものであって、
「（１）工具基体の表面に、硬質被覆層が設けられた表面被覆切削工具において、
（ａ）前記硬質被覆層は、平均層厚１．０〜２０．０μｍのＴｉとＡｌの複合窒化物層または複合炭窒化物層を少なくとも含み、
（ｂ）前記複合窒化物層または複合炭窒化物層は、ＮａＣｌ型の面心立方構造を有する複合窒化物または複合炭窒化物の結晶粒の占める割合が８０面積％以上であり、
（ｃ）前記複合窒化物層または複合炭窒化物層について該層の縦断面を観察した場合に、前記複合窒化物層または複合炭窒化物層内の前記ＮａＣｌ型の面心立方構造を有する結晶粒は、平均粒子幅Ｗが０．１０〜２．００μｍ、平均アスペクト比Ａが２．０〜１０．０であり、
（ｄ）前記複合窒化物層または複合炭窒化物層は、
組成式：（Ｔｉ１−ＸＡｌＸ）（ＣＹＮ１−Ｙ）
で表した場合、０．５μｍの間隔で該層を層厚方向に複数の区間に分割したとき、各区間におけるＡｌのＴｉとＡｌの合量に占める平均含有割合Ｘａｖｇが０．６０≦Ｘａｖｇ≦０．９５を満足し、また、該層全体におけるＣのＣとＮの合量に占める平均含有割合Ｙａｖｇが０．０００≦Ｙａｖｇ≦０．００５を満足し、（但し、Ｘａｖｇ、Ｙａｖｇはいずれも原子比）
（ｅ）前記複合窒化物層または複合炭窒化物層において、前記Ａｌの平均含有割合Ｘａｖｇが該層の層厚方向において工具表面に向かって増加し、
（ｆ）前記複合窒化物層または複合炭窒化物層において、前記ＮａＣｌ型の面心立方構造を有する隣り合う２つの結晶粒の粒界から粒内に１０ｎｍ入り込んだ曲線ｍに囲まれた範囲を領域α、該曲線ｍと粒界に囲まれた範囲を領域βとし、前記工具基体表面に平行に複数の前記隣り合う結晶粒の粒界を貫通する線分を、前記層の厚さを６等分する間隔で５本引いたとき、層厚方向で最も工具基体側端面に近い線分Ｌ１および中央に位置する線分Ｌ３上のいずれにおいても、
関係式：Ｘαａｖｇ≦０．９０のときＸαａｖｇ＋０．１０≦Ｘβａｖｇ≦１．００、０．９０＜ＸαａｖｇのときＸαａｖｇ＋０．０５≦Ｘβａｖｇ≦１．００（ただし、Ｘαａｖｇ及びＸβａｖｇはそれぞれ前記領域αおよび前記領域βにおけるＡｌのＴｉとＡｌの合量に占める含有割合の平均値）
を満足する、
ことを特徴とする表面被覆切削工具。
（２）前記複合窒化物層または複合炭窒化物層について、該層の縦断面を観察した場合に、前記複合窒化物層または複合炭窒化物層内の前記ＮａＣｌ型の面心立方構造を有する個々の結晶粒の粒界に存在する、ウルツ鉱型構造を有する結晶粒の面積割合は５．０面積％以下であり、該結晶粒の平均粒径Ｒは０．５０μｍ以下であることを特徴とする前記（１）に記載の表面被覆切削工具。」
である。
The present invention was made based on the above findings,
"(1) In a surface-coated cutting tool in which a hard coating layer is provided on the surface of a tool base,
(A) The hard coating layer includes at least a composite nitride layer or a composite carbonitride layer of Ti and Al having an average layer thickness of 1.0 to 20.0 μm,
(B) In the composite nitride layer or the composite carbonitride layer, the ratio of the crystal grains of the composite nitride or the composite carbonitride having the NaCl-type face-centered cubic structure is 80 area% or more,
(C) A crystal having the NaCl-type face-centered cubic structure in the composite nitride layer or the composite carbonitride layer, when the longitudinal section of the composite nitride layer or the composite carbonitride layer is observed. The particles have an average particle width W of 0.10 to 2.00 μm and an average aspect ratio A of 2.0 to 10.0,
(D) The composite nitride layer or the composite carbonitride layer is
Compositional formula: (Ti 1-X Al X )(C Y N 1-Y )
When the layer is divided into a plurality of sections in the layer thickness direction at intervals of 0.5 μm, the average content ratio X avg of Al in Ti and Al in each section is 0.60≦X. avg ≤ 0.95, and the average content Y avg of C in the total amount of C and N in the entire layer satisfies 0.000 ≤ Y avg ≤ 0.005 (provided that X avg , Y avg are all atomic ratios)
(E) In the composite nitride layer or the composite carbonitride layer, the average content ratio X avg of Al increases toward the tool surface in the layer thickness direction of the layer,
(F) In the composite nitride layer or the composite carbonitride layer, a range surrounded by a curve m in which 10 nm is inserted into the grain from the grain boundary of two adjacent crystal grains having the NaCl-type face-centered cubic structure A region α, a region surrounded by the curve m and the grain boundary is defined as a region β, and a line segment penetrating the grain boundaries of the plurality of adjacent crystal grains in parallel to the tool base surface has a layer thickness of 6 When five lines are drawn at equal intervals, both on the line segment L1 closest to the tool base side end face and the line segment L3 located at the center in the layer thickness direction,
Relationship: Xα avg Xα avg + 0.10 ≦ when ≦ 0.90 Xβ avg ≦ 1.00,0.90 <When Xα avg Xα avg + 0.05 ≦ Xβ avg ≦ 1.00 ( provided that, X [alpha avg and Xβ avg is the average value of the content ratio of Al in the total amount of Ti and Al in the regions α and β, respectively.
Satisfy,
A surface-coated cutting tool characterized in that
(2) The composite nitride layer or the composite carbonitride layer has the NaCl-type face-centered cubic structure in the composite nitride layer or the composite carbonitride layer when the longitudinal section of the layer is observed. The area ratio of the crystal grains having a wurtzite structure present at the grain boundaries of the individual crystal grains is 5.0 area% or less, and the average grain size R of the crystal grains is 0.50 μm or less. The surface-coated cutting tool according to (1) above. "
Is.
本発明の被覆工具は、硬質被膜層が優れた耐チッピング性を備え、合金鋼および高炭素鋼等の高速断続切削等に供した場合であっても、長期の使用にわたって優れた切削性能を発揮する。 The coated tool of the present invention has excellent chipping resistance in the hard coating layer, and exhibits excellent cutting performance over long-term use even when subjected to high-speed intermittent cutting of alloy steel and high-carbon steel, etc. To do.
本発明について、以下に詳細に説明する。なお、明細書および特許請求の範囲において数値範囲を「〜」で表現するときは、その上限値及び下限値を含んでいる。 The present invention will be described in detail below. In addition, when a numerical range is expressed by "to" in the specification and claims, the upper limit and the lower limit are included.
ＴｉＡｌＣＮ層の平均層厚：
本発明のＴｉＡｌＣＮ層は、硬さが高く、優れた耐摩耗性を有するが、特に平均層厚が１．０〜２０．０μｍのとき、その効果が際立って発揮される。これは、平均層厚が１．０μｍ未満では、層厚が薄いため長期の使用にわたっての耐摩耗性を十分確保することができず、一方、その平均層厚が２０．０μｍを超えると、ＴｉＡｌＣＮ層の結晶粒が粗大化しやすくなり、チッピングを発生しやすくなる。
したがって、その平均層厚を１．０〜２０．０μｍと定めた。より好ましくは３．０〜１５．０μｍである。
Average layer thickness of TiAlCN layer:
The TiAlCN layer of the present invention has high hardness and excellent wear resistance, but when the average layer thickness is 1.0 to 20.0 μm, the effect is remarkably exhibited. This is because if the average layer thickness is less than 1.0 μm, it is not possible to ensure sufficient wear resistance over long-term use because the layer thickness is thin, while if the average layer thickness exceeds 20.0 μm, TiAlCN The crystal grains of the layer are likely to become coarse and chipping is likely to occur.
Therefore, the average layer thickness is set to 1.0 to 20.0 μm. More preferably, it is 3.0 to 15.0 μm.
ＴｉＡｌＣＮ層内のＮａＣｌ型の面心立方構造を有する結晶粒の面積割合：
本発明のＴｉＡｌＣＮ層におけるＮａＣｌ型の面心立方構造を有する結晶粒の面積割合が８０面積％以上であることが好ましい。これにより、高硬度であるＮａＣｌ型の面心立方構造を有する結晶粒の面積比率がウルツ鉱型構造の結晶粒（六方晶結晶粒ということがある）に比べて相対的に高くなり、ＴｉＡｌＣＮ層の硬さが向上し、耐摩耗性が向上する。この面積率は、より好ましくは９０面積％以上である。
ここで、面積割合は、工具基体表面に垂直な方向の断面、すなわち、縦断面に対して求める。
Area ratio of crystal grains having a NaCl-type face-centered cubic structure in the TiAlCN layer:
The area ratio of the crystal grains having the NaCl-type face-centered cubic structure in the TiAlCN layer of the present invention is preferably 80 area% or more. As a result, the area ratio of the crystal grains having a NaCl-type face-centered cubic structure with high hardness is relatively higher than that of the wurtzite-type crystal grains (sometimes referred to as hexagonal crystal grains), and the TiAlCN layer Hardness is improved and wear resistance is improved. This area ratio is more preferably 90 area% or more.
Here, the area ratio is obtained for a cross section in a direction perpendicular to the tool base surface, that is, a vertical cross section.
ＮａＣｌ型の面心立方構造を有する結晶粒の平均粒子幅とアスペクト比：
本発明のＴｉＡｌＣＮ層の縦断面を観察した際に、ＮａＣｌ型の面心立方構造を有する結晶粒は、平均粒子幅Ｗが０．１０〜２．００μｍ、平均アスペクト比Ａが２．０〜１０．０である場合に、結晶粒の硬さおよび靭性が向上する。
すなわち、平均粒子幅Ｗが０．１０μｍ未満であると耐摩耗性が低下し、平均粒子幅Ｗが２．００μｍを超えると靱性が低下する。
また、平均アスペクト比Ａが２．０未満であると、アスペクト比が小さな等軸結晶の脱落が生じ、十分な耐摩耗性を発揮することができなくなり、一方、平均アスペクト比Ａが１０．０を超えると結晶粒そのものの強度を保つことができず、かえって、耐チッピング性が低下するため好ましくない。より好ましい平均アスペクト比Ａは、３．０〜８．０である。
ここで、平均粒子幅および平均アスペクト比は、ともに、結晶粒の面積を測定し面積平均として求める。すなわち、観察視野内の少なくとも２０以上の結晶粒の粒子幅Ｗ１〜Ｗｎ（ｎ≧２０）および面積Ｓ１〜Ｓｎを求めて、数１（数式１）により面積加重平均し、前記結晶粒の平均粒子幅Ｗとする。また、同様にして前記結晶粒のアスペクト比Ａ１〜Ａｎ（ｎ≧２０）を求め、数２（数式２）により面積加重平均して、前記結晶粒の平均アスペクト比Ａとする。平均粒子幅Ｗ、平均アスペクト比Ａはそれぞれ以下のような式に基づき算出できる。
When observing the longitudinal section of the TiAlCN layer of the present invention, the crystal grains having a NaCl-type face-centered cubic structure have an average grain width W of 0.10 to 2.00 μm and an average aspect ratio A of 2.0 to 10. When it is 0.0, hardness and toughness of crystal grains are improved.
That is, if the average particle width W is less than 0.10 μm, the wear resistance decreases, and if the average particle width W exceeds 2.00 μm, the toughness decreases.
Further, when the average aspect ratio A is less than 2.0, equiaxed crystals having a small aspect ratio fall off and sufficient abrasion resistance cannot be exhibited, while the average aspect ratio A is 10.0. If it exceeds, the strength of the crystal grains themselves cannot be maintained and, on the contrary, the chipping resistance decreases, which is not preferable. A more preferable average aspect ratio A is 3.0 to 8.0.
Here, both the average particle width and the average aspect ratio are obtained as the average area by measuring the area of crystal grains. That is, the particle widths W 1 to W n (n≧20) and the areas S 1 to S n of at least 20 or more crystal grains in the observation visual field are obtained, and the area weighted average is calculated by the mathematical formula 1 (Formula 1) to obtain the crystal. The average particle width W of the particles is set. In addition, similarly, the aspect ratios A 1 to A n (n≧20) of the crystal grains are obtained, and area weighted averaging is performed according to Formula 2 (Mathematical Formula 2) to obtain the average aspect ratio A of the crystal grains. The average particle width W and the average aspect ratio A can be calculated based on the following equations.
ＴｉＡｌＣＮ層の組成：
本発明のＴｉＡｌＣＮ層の組成は、
組成式：（Ｔｉ１−ＸＡｌＸ）（ＣＹＮ１−Ｙ）で表したとき、
工具基体側端面から測定間隔が０．５μｍとなるように層厚方向にｎ個に分割した区間ごとにＡｌのＴｉとＡｌの合量に占める平均含有割合（以下、「Ａｌの平均含有割合」という）Ｘａｖｇを求めた場合、各区間のＸａｖｇが０．６０≦Ｘａｖｇ≦０．９５（ただし、Ｘａｖｇは原子比）を満足するように組成を制御する。
また、本発明のＴｉＡｌＣＮ層全体におけるＣのＣとＮの合量に占める平均含有割合（以下、「Ｃの平均含有割合」という）Ｙａｖｇが０．０００≦Ｙａｖｇ≦０．００５（ただし、Ｙａｖｇは原子比）を満足するように組成を制御する。
その理由は、以下のとおりである。
Ａｌの平均含有割合Ｘａｖｇが０．６０未満であると、ＴｉＡｌＣＮ層は硬さが劣るため、合金鋼や高炭素鋼等の高速断続切削に供した場合には、耐摩耗性が十分でなく、一方、Ａｌの平均含有割合Ｘａｖｇが０．９５を超えると六方晶のＴｉＡｌＣＮ結晶粒が析出し、耐摩耗性が低下する。したがって、０．６０≦Ｘａｖｇ≦０．９５としたが、より好ましくは０．７０≦Ｘａｖｇ≦０．９５である。
また、Ｃの平均含有割合Ｙａｖｇを０．０００≦Ｙａｖｇ≦０．００５と定めた理由は、前記範囲において靱性や耐チッピング性を保ちつつ硬さを向上させることができるためである。
Composition of TiAlCN layer:
The composition of the TiAlCN layer of the present invention is
Compositional formula: (Ti 1-X Al X )(C Y N 1-Y )
The average content ratio in the total amount of Ti and Al of Al in each of n sections divided in the layer thickness direction so that the measurement interval is 0.5 μm from the tool base side end surface (hereinafter, “average content ratio of Al”). When X avg is obtained, the composition is controlled so that X avg of each section satisfies 0.60≦X avg ≦0.95 (where X avg is an atomic ratio).
Further, the average content ratio of C in the total amount of C and N in the entire TiAlCN layer of the present invention (hereinafter referred to as “average content ratio of C”) Y avg is 0.000≦Y avg ≦0.005 (however, Y avg controls the composition so as to satisfy the atomic ratio.
The reason is as follows.
If the average content ratio X avg of Al is less than 0.60, the TiAlCN layer has poor hardness, and therefore, when subjected to high-speed intermittent cutting of alloy steel, high carbon steel, etc., wear resistance is insufficient. On the other hand, when the average content ratio Xavg of Al exceeds 0.95, hexagonal TiAlCN crystal grains are precipitated and wear resistance is reduced. Therefore, although 0.60≦X avg ≦0.95 is set, 0.70≦X avg ≦0.95 is more preferable.
Further, the reason why the average content ratio Y avg of C is set to 0.000≦Y avg ≦0.005 is that hardness can be improved while maintaining toughness and chipping resistance in the above range.
ＴｉＡｌＣＮ層の層厚方向のＡｌの平均含有割合：
層厚方向において工具基体側端面から工具表面側に向かって、ＴｉＡｌＣＮ層の前記区間ごとのＡｌの平均含有割合が増加すると、ＴｉＡｌＣＮ層の耐チッピング性が向上する。
ここで、Ａｌの平均含有割合が増加しているとは、工具基体側端面に比して工具表面側のＡｌの含有割合が増加していることをいう。
Average Al content in the thickness direction of the TiAlCN layer:
When the average content ratio of Al in each of the sections of the TiAlCN layer increases from the end surface on the tool substrate side in the layer thickness direction toward the tool surface side, the chipping resistance of the TiAlCN layer improves.
Here, the increase in the average content ratio of Al means that the content ratio of Al on the tool surface side is increased as compared with the end surface on the tool base side.
ＴｉＡｌＣＮ層のＮａＣｌ型の面心立方構造を有する結晶粒における粒界近傍領域と該領域でない領域の間におけるＡｌの平均含有割合の関係：
図1に示すように、ＮａＣｌ型の面心立方構造を有する結晶粒の粒界から粒内に１０ｎｍ入り込んだ曲線ｍに囲まれた範囲を領域α、ｍと粒界に囲まれた範囲を領域βとし、工具基体表面に平行に、５個以上の隣り合うＮａＣｌ型の面心立方構造を有する結晶粒の粒界を貫通する線分を、ＴｉＡｌＣＮ層の厚さを６等分する間隔で５本引いたとき、層厚方向で最も工具基体側端面に近い線分（Ｌ１）および中央に位置する線分（Ｌ３：Ｌ１から工具表面側に数えて３本目）上のいずれにおいても、
関係式：Ｘαａｖｇ≦０．９０のとき、Ｘαａｖｇ＋０．１０≦Ｘβａｖｇ≦１．００、０．９０＜Ｘαａｖｇのとき、Ｘαａｖｇ＋０．０５≦Ｘβａｖｇ≦１．００
を満足すると、靭性が向上し、優れた耐チッピング性を発揮する。
ここで、線分Ｌ１およびＬ３上において、Ｘαａｖｇは領域α、Ｘβａｖｇは領域βにおけるＡｌの平均含有割合をいい、Ｌ１およびＬ３が引かれる結晶粒は、完全に同じ、一部が同じ（図１を参照）、同じものがないのいずれでもよい。
前記関係式を満足すると、靭性が向上し、優れた耐チッピング性を発揮する。
The relation of the average content ratio of Al between the region near the grain boundary and the region other than the region in the crystal grain having the NaCl-type face-centered cubic structure of the TiAlCN layer:
As shown in FIG. 1, a region surrounded by a curve m in which the grain boundary of a crystal grain having a NaCl-type face-centered cubic structure is inserted 10 nm into the grain is a region α, and a region surrounded by m and the grain boundary is a region. Let β be parallel to the surface of the tool base, and line segments penetrating the grain boundaries of five or more adjacent crystal grains of the NaCl-type face-centered cubic structure at intervals of dividing the thickness of the TiAlCN layer into 6 equal parts. When the main line is drawn, both on the line segment (L1) closest to the tool base side end face in the layer thickness direction and on the line segment located at the center (L3: the third line counting from the L1 to the tool surface side),
Relational expression: when Xα avg ≦0.90, Xα avg +0.10≦Xβ avg ≦1.00, and when 0.90<Xα avg , Xα avg +0.05≦Xβ avg ≦1.00
When satisfying, the toughness is improved and excellent chipping resistance is exhibited.
Here, on the line segments L1 and L3, Xα avg is the average content ratio of Al in the region α and Xβ avg is the region β, and the crystal grains from which L1 and L3 are drawn are completely the same, and partly the same ( (See FIG. 1), or they may not be the same.
When the above relational expression is satisfied, toughness is improved and excellent chipping resistance is exhibited.
Ｘαａｖｇ及びＸβａｖｇの値は、工具基体表面に平行な線分である前記Ｌ１およびＬ３において、透過型電子顕微鏡（Ｔｒａｎｓｍｉｓｓｉｏｎ Ｅｌｅｃｔｒｏｎ Ｍｉｃｒｏｓｃｏｐｅ：ＴＥＭ）を用いたエネルギー分散型Ｘ線分光法（Ｅｎｅｒｇｙ Ｄｉｓｐｅｒｓｉｖｅ Ｘ−ｒａｙ Ｓｐｅｃｔｒｏｍｅｔｒｙ：ＥＤＳ）によるスポット分析をα領域では１ヵ所以上（図１では●の箇所。２箇所以上のときは粒子間で等間隔が好ましい）、β領域では１ヵ所（図１では×の箇所：隣接するＮａＣｌ型の面心立方構造の結晶粒の粒界同士が接する箇所）で行い平均値として求める。
なお、前記線分Ｌ１およびＬ３を引いたとき、隣接するＮａＣｌ型の面心立方構造の結晶粒の間に六方晶結晶粒が存在する場合は、この六方晶結晶粒に隣接するいずれかのＮａＣｌ型の面心立方構造の結晶粒の前記領域βに含め、また、前記×の箇所はこの六方晶結晶粒を前記β領域に含めないＮａＣｌ型の面心立方構造の結晶粒の粒界と、この結晶粒界に前記六方晶結晶粒が接する箇所とする。
The values of Xα avg and Xβ avg are the energy-dispersive X-ray spectroscopy (Energy Dispersive X) using a transmission electron microscope (TEM) at L1 and L3, which are line segments parallel to the tool substrate surface. Spot analysis by -ray Spectrometry (EDS) was performed at 1 place or more in the α region (indicated by ● in Fig. 1. At two or more places, it is preferable that the particles be equidistant), and in 1 region in the β region (indicated by × in Fig. 1). Location: location where adjacent grain boundaries of the crystal grains of the NaCl-type face-centered cubic structure contact each other) to obtain an average value.
When the line segments L1 and L3 are drawn, if hexagonal crystal grains are present between adjacent crystal grains of the NaCl-type face-centered cubic structure, any of the NaCl adjacent to the hexagonal crystal grains Included in the region β of the crystal grains of the face-centered cubic structure of the type, and the × portion is the grain boundary of the crystal grains of the NaCl-type face-centered cubic structure not including the hexagonal crystal grains in the β region, The position where the hexagonal crystal grains are in contact with this crystal grain boundary is set.
ＮａＣｌ型の面心立方構造を有する結晶粒の粒界間に存在する六方晶結晶粒：
本発明のＴｉＡｌＣＮ層の縦断面を観察した場合に、該層内のＮａＣｌ型の面心立方構造を有する個々の結晶粒の粒界部に六方晶結晶粒が存在するとき（存在することは必須ではない）、該結晶粒の面積割合は５．０面積％以下であり、該結晶粒の平均粒径Ｒは０．５０μｍ以下であることが望ましい。
すなわち、ＮａＣｌ型の面心立方構造を有する結晶粒の粒界に所定の六方晶結晶粒が所定量存在すれば、合金鋼や高炭素鋼の高速断続切削加工であっても、ＴｉＡｌＣＮ層が優れた耐チッピング性を備えることができる。このとき、六方晶結晶粒の面積割合が５面積％を超えると硬さが低下して好ましくない場合があり、また、平均粒径Ｒが０．５０μｍを超えると硬さが低下し、耐摩耗性が十分でないときがある。
Hexagonal crystal grains existing between the grain boundaries of crystal grains having a NaCl-type face-centered cubic structure:
When observing the longitudinal section of the TiAlCN layer of the present invention, when hexagonal crystal grains are present in the grain boundary portion of the individual crystal grains having the NaCl-type face-centered cubic structure in the layer (the existence is essential. However, the area ratio of the crystal grains is 5.0 area% or less, and the average grain size R of the crystal grains is preferably 0.50 μm or less.
That is, if a predetermined amount of hexagonal crystal grains are present at the grain boundaries of the crystal grains having a NaCl-type face-centered cubic structure, the TiAlCN layer is excellent even in high-speed intermittent cutting of alloy steel or high carbon steel. It can be provided with chipping resistance. At this time, if the area ratio of the hexagonal crystal grains exceeds 5 area %, the hardness may be decreased, which is not preferable, and if the average grain size R exceeds 0.50 μm, the hardness may be decreased and the wear resistance may be reduced. There are times when the sex is not sufficient.
工具基体：
工具基体は、この種の工具基体として従来公知の基材であれば、本発明の目的を達成することを阻害するものでない限り、いずれのものも使用可能である。一例を挙げるならば、超硬合金（ＷＣ基超硬合金、ＷＣの他、Ｃｏを含み、あるいはＴｉ、Ｔａ、Ｎｂ等の炭窒化物を添加したものも含むもの等）、サーメット（ＴｉＣ、ＴｉＮ、ＴｉＣＮ等を主成分とするもの等）、セラミックス（炭化チタン、炭化珪素、窒化珪素、窒化アルミニウム、酸化アルミニウムなど）、ｃＢＮ焼結体、またはダイヤモンド焼結体のいずれかであることが好ましい。
Tool base:
As the tool base, any base can be used as long as it is a base conventionally known as a tool base of this type, as long as it does not impair the achievement of the object of the present invention. To give an example, cemented carbide (WC-based cemented carbide, WC, or the like that contains Co or the addition of carbonitrides such as Ti, Ta, Nb, etc.), cermet (TiC, TiN , TiCN, etc.), ceramics (titanium carbide, silicon carbide, silicon nitride, aluminum nitride, aluminum oxide, etc.), cBN sintered body, or diamond sintered body.
製造方法：
本発明のＴｉＡｌＣＮ層の成膜方法は、例えば、以下のとおりである。後述するガス群Ａとガス群Ｂを用い、第１回から第ｎ回までの成膜を行う。第ｎ回の成膜で目標とするＴｉＡｌＣＮ層の層厚を得る。各回の成膜は、成膜回数の増加に応じてガス群ＢのＡｌＣｌ３／ＴｉＣｌ４（容量％の比）の値を増加させながら成膜を行う過程１と、粒界にＡｌの平均含有割合の高いＴｉＡｌＣＮを偏析させる過程２とからなる。各回の成膜は、過程１を一定時間行い、続いてこれの半分の時間で過程２を行う。なお、過程２では、過程１で成膜された層の表面に新たな層の堆積はほとんどなされず、層厚の変化は無視できる。
ガス群Ａとガス群Ｂの組成を以下に示す（過程の記載がないものは、過程１および２で共通である）。
ガス群Ａ： ＮＨ３：２．０〜５．０％（過程１）、０．１〜０．３％（過程２）、
Ｈ２：６５〜７５％
ガス群Ｂ： ＡｌＣｌ３：０．５０〜０．９０％、
ＴｉＣｌ４：０．０５〜０．３０％（過程１）、
０．０３〜０．０５％（過程２）、
Ｎ２：０．０〜１２．０％、Ｃ２Ｈ４：０．０〜０．５％、Ｈ２：残
反応ガス組成の％は、ガス群Ａおよびガス群Ｂをあわせた全体に対する容量％である。
反応雰囲気圧力： ４．０〜５．０ｋＰａ
反応雰囲気温度： ７００〜９００℃
供給周期： １．０〜５．０秒
１周期当たりのガス供給時間： ０．１５〜０．２５秒
ガス群Ａとガス群Ｂの供給の位相差： ０．１０〜０．２０秒
ここで、過程１においてガス群ＢのＡｌＣｌ３／ＴｉＣｌ４（容量％の比）の値を増加させながら成膜するとは、第１回目の成膜から第ｎ回目の成膜に至る各回の成膜において、回数の増加に応じてＡｌＣｌ３／ＴｉＣｌ４（容量％の比）の値を増加すればよく、成膜回数毎の当該増加の量が同じであっても、異なっていてもかまわない。また、各回の過程１の成膜時間中にＡｌＣｌ３／ＴｉＣｌ４（容量％の比）の値が線形に増加してもよいし、過程１の成膜時間中に前回の過程１のＡｌＣｌ３／ＴｉＣｌ４（容量％の比）の値よりも増加した一定値に保ってもよい。本明細書では、線形に増加すること、一定値に保つことを、それぞれ、線形増加、ステップ状増加という。線形増加、ステップ状増加の具体的例は、実施例で説明する。
Production method:
The method for forming the TiAlCN layer of the present invention is as follows, for example. Using a gas group A and a gas group B described later, film formation is performed from the first time to the n-th time. The target thickness of the TiAlCN layer is obtained by the n-th film formation. Each time the film formation is performed, the film formation process is performed while increasing the value of AlCl 3 /TiCl 4 (volume ratio) of the gas group B according to the increase in the number of film formation, and the average content of Al in the grain boundaries. Step 2 of segregating a high proportion of TiAlCN. In each film formation, step 1 is performed for a certain period of time, and then step 2 is performed for half the time. In step 2, a new layer is hardly deposited on the surface of the layer formed in step 1, and the change in layer thickness can be ignored.
The compositions of the gas group A and the gas group B are shown below (those with no description of steps are common to steps 1 and 2).
Gas Group A: NH 3: 2.0~5.0% (step 1), 0.1% to 0.3% (step 2),
H 2: 65~75%
Gas group B: AlCl 3 : 0.50 to 0.90%,
TiCl 4: 0.05~0.30% (process 1),
0.03 to 0.05% (process 2),
N 2: 0.0~12.0%, C 2 H 4: 0.0~0.5%, H 2:% residual reaction gas composition, capacity for total combined gas group A and Gas group B %.
Reaction atmosphere pressure: 4.0 to 5.0 kPa
Reaction atmosphere temperature: 700 to 900°C
Supply cycle: 1.0 to 5.0 seconds Gas supply time per cycle: 0.15 to 0.25 seconds Phase difference between supply of gas group A and gas group B: 0.10 to 0.20 seconds where In the process 1, the film formation is performed while increasing the value of AlCl 3 /TiCl 4 (volume% ratio) of the gas group B means that in each film formation from the first film formation to the nth film formation. The value of AlCl 3 /TiCl 4 (ratio of volume%) may be increased according to the increase in the number of times, and the amount of increase may be the same or different for each number of film formations. Furthermore, AlCl 3 / TiCl 4 to a value of (volume% ratio) may be increased linearly, AlCl 3 of the previous process 1 during the film formation process 1 time during the deposition time of each round of the process 1 /TiCl 4 (ratio of% by volume) may be maintained at a constant value increased. In the present specification, increasing linearly and maintaining a constant value are called linear increase and stepwise increase, respectively. Specific examples of the linear increase and the stepwise increase will be described in Examples.
本発明の被覆工具を実施例により具体的に説明する。
なお、以下の実施例では、工具基体として、ＷＣ基超硬合金を用いた場合について説明するが、ＴｉＣＮ基サーメット、ｃＢＮ基超高圧焼結体等の前記した他の材を工具基体として用いた場合も同様である。また、ドリルやエンドミルに適用した場合も同様である。
The coated tool of the present invention will be specifically described with reference to examples.
In the following examples, the case where a WC-based cemented carbide is used as the tool substrate will be described. However, the above-mentioned other materials such as TiCN-based cermet and cBN-based ultra-high pressure sintered body were used as the tool substrate. The same applies to the case. The same applies when applied to a drill or end mill.
原料粉末として、いずれも１〜３μｍの平均粒径を有するＷＣ粉末、ＴｉＣ粉末、ＺｒＣ粉末、ＴａＣ粉末、ＮｂＣ粉末、Ｃｒ３Ｃ２粉末、ＴｉＮ粉末およびＣｏ粉末を用意し、これら原料粉末を、表１に示される配合組成に配合し、さらにワックスを加えてアセトン中で２４時間ボールミル混合し、減圧乾燥した後、９８ＭＰａの圧力で所定形状の圧粉体にプレス成形し、このプレス成形体を５Ｐａの真空中、１３７０〜１４７０℃の範囲内の所定の温度に１時間保持の条件で真空焼結し、焼結後、ＩＳＯ規格ＳＥＥＮ１２０３ＡＦＳＮのインサート形状をもったＷＣ基超硬合金製の工具基体Ａ〜Ｃ、および、ＩＳＯ規格ＣＮＭＧ１２０４１２のインサート形状をもったＷＣ基超硬合金製の工具基体Ｄ〜Ｆをそれぞれ製造した。 As raw material powders, WC powders, TiC powders, ZrC powders, TaC powders, NbC powders, Cr 3 C 2 powders, TiN powders, and Co powders each having an average particle diameter of 1 to 3 μm are prepared, and these raw material powders are prepared. Compounded to the compounding composition shown in Table 1, wax was added, ball milled in acetone for 24 hours, dried under reduced pressure, and then press-molded at a pressure of 98 MPa into a green compact having a predetermined shape. A tool base made of WC-based cemented carbide having an insert shape of ISO standard SEEN1203AFSN after being vacuum-sintered under a condition of holding at a predetermined temperature within a range of 1370 to 1470° C. for 1 hour in a vacuum of 5 Pa. A to C and tool bases D to F made of WC-based cemented carbide having insert shapes of ISO standard CNMG120412 were manufactured, respectively.
次に、これらの工具基体Ａ〜Ｆの表面に、ＣＶＤ装置を用いて、表２、４に示される形成条件Ａ〜Ｈにより、ＴｉＡｌＣＮ層を形成した。
Ａ１〜Ｈ１、Ａ２〜Ｈ２は、それぞれ、前述の過程１、過程２にそれぞれ相当する。また、区間１とは第１回目の成膜をいい、区間ｎとは目標層厚となる最終の成膜、すなわち、第ｎ回目の成膜である。ｎの値は表４に示されている。ガス群ＢにおけるＡｌＣｌ３／ＴｉＣｌ４（容量％の比）の値を第１回目の成膜から第ｎ回目の成膜まで、表２に示す態様で増加させた。態様の詳細は後述する。
前記の過程１では、表２、表４に示される形成条件を示す形成記号Ａ〜Ｈ、Ａ１〜Ｈ１、すなわち、ガス群ＡとしてＮＨ３：２．０〜５．０％、Ｈ２：６５〜７５％、ガス群ＢとしてＡｌＣｌ３：０．５０〜０．９０％、ＴｉＣｌ４：０．０５〜０．３０％、Ｎ２：０．０〜１２．０％、Ｃ２Ｈ４：０．０〜０．５％、Ｈ２：残（％は、ガス群Ａおよびガス群Ｂを合わせた全体に対する容量％）、反応雰囲気圧力：４．０〜５．０ｋＰａ、反応雰囲気温度：７００〜９００℃、供給周期１．０〜５．０秒、１周期当たりのガス供給時間０．１５〜０．２５秒、ガス群Ａとガス群Ｂの供給の位相差０．１０〜０．２０秒とし、所定時間、ＣＶＤ法により、成膜を行った。前記の過程２では、表２、表４に示される形成条件を示す形成記号Ａ〜Ｈ、Ａ２〜Ｈ２、すなわち、ガス群ＡとしてＮＨ３：０．１〜０．３％、Ｈ２：６５〜７５％、ガス群ＢとしてＡｌＣｌ３：０．５０〜０．９０％、ＴｉＣｌ４：０．０３〜０．０５％、Ｎ２：０．０〜１２．０％、Ｃ２Ｈ４：０．０〜０．５％、Ｈ２：残（％は、ガス群Ａおよびガス群Ｂを合わせた全体に対する容量％）、反応雰囲気圧力：４．０〜５．０ｋＰａ、反応雰囲気温度：７００〜９００℃、供給周期１．０〜５．０秒、１周期当たりのガス供給時間０．１５〜０．２５秒、ガス群Ａとガス群Ｂの供給の位相差０．１０〜０．２０秒とし、所定時間、ＣＶＤ法により、ＴｉＡｌＣＮの粒界偏析を行った。
前記の条件でＴｉＡｌＣＮ層を形成することにより、表５に示す本発明被覆工具１〜１６を製造した。
Next, a TiAlCN layer was formed on the surfaces of these tool substrates A to F using a CVD apparatus under the formation conditions A to H shown in Tables 2 and 4.
A1 to H1 and A2 to H2 correspond to the above-described step 1 and step 2, respectively. Further, the section 1 is the first film formation, and the section n is the final film formation with the target layer thickness, that is, the nth film formation. The values of n are shown in Table 4. The value of AlCl 3 /TiCl 4 (volume% ratio) in the gas group B was increased in the manner shown in Table 2 from the first film formation to the nth film formation. Details of the embodiment will be described later.
In the above process 1, formation symbols A to H and A1 to H1 showing the formation conditions shown in Tables 2 and 4, that is, NH 3 as the gas group A: 2.0 to 5.0%, H 2 : 65. ˜75%, as gas group B AlCl 3 : 0.50 to 0.90%, TiCl 4 : 0.05 to 0.30%, N 2 : 0.0 to 12.0%, C 2 H 4 :0. 0.0 to 0.5%, H 2 : balance (% is the volume% with respect to the total of the gas group A and the gas group B), reaction atmosphere pressure: 4.0 to 5.0 kPa, reaction atmosphere temperature: 700 to 900° C., supply cycle 1.0 to 5.0 seconds, gas supply time per cycle 0.15 to 0.25 seconds, phase difference between supply of gas group A and gas group B 0.10 to 0.20 seconds Then, the film formation was performed by the CVD method for a predetermined time. Wherein the step 2 of Table 2, forming symbols A~H showing the formation conditions shown in Table 4, A2～H2, i.e., NH 3 as a gas group A: 0.1~0.3%, H 2: 65 ˜75%, AlCl 3 as gas group B: 0.50 to 0.90%, TiCl 4 : 0.03 to 0.05%, N 2 : 0.0 to 12.0%, C 2 H 4 :0. 0.0 to 0.5%, H 2 : balance (% is the volume% with respect to the total of the gas group A and the gas group B), reaction atmosphere pressure: 4.0 to 5.0 kPa, reaction atmosphere temperature: 700 to 900° C., supply cycle 1.0 to 5.0 seconds, gas supply time per cycle 0.15 to 0.25 seconds, phase difference between supply of gas group A and gas group B 0.10 to 0.20 seconds Then, the grain boundary segregation of TiAlCN was performed by the CVD method for a predetermined time.
The coated tools 1 to 16 of the present invention shown in Table 5 were manufactured by forming the TiAlCN layer under the above conditions.
ここで、表２、３に示されている、ＡｌＣｌ３／ＴｉＣｌ４の比の増加の態様について、線形増加、ステップ状増加とは次のとおりである。線形増加とは、第ｉ回目の成膜時のＡｌＣｌ３／ＴｉＣｌ４の比の値が、第ｉ−１回目の成膜時のＡｌＣｌ３／ＴｉＣｌ４の比の値からこのＡｌＣｌ３／ＴｉＣｌ４の比の値に増加量を加えた値まで成膜期間中に線形に増加することをいう。また、ステップ状増加とは、第ｉ回目の成膜時のＡｌＣｌ３／ＴｉＣｌ４の比の値が第ｉ−１回目の成膜時のＡｌＣｌ３／ＴｉＣｌ４の比の値に増加量を加えた値の一定値とすることをいう。
なお、増加量とは、増加量＝（第ｎ回目の成膜におけるＡｌＣｌ３／ＴｉＣｌ４の比の値−第１回目の成膜におけるＡｌＣｌ３／ＴｉＣｌ４の比の値）／（ｎ−１）で求める値をいう。
Here, regarding the mode of increasing the ratio of AlCl 3 /TiCl 4 shown in Tables 2 and 3 , the linear increase and the stepwise increase are as follows. The linear increase, the value of the ratio of the i-th AlCl 3 / TiCl 4 during film formation, the AlCl 3 / TiCl 4 from the value of the ratio of AlCl 3 / TiCl 4 at the i-1 th deposition It means that the value increases linearly during the film-forming period up to a value obtained by adding the amount of increase to the value of the ratio. Further, the step increases, increasing amounts of added value of the ratio of the i-th AlCl 3 / TiCl 4 at the time of film formation is the value of the ratio of the (i-1) th AlCl 3 / TiCl 4 at the time of film formation It means a constant value.
Note that the amount of increase means the amount of increase=(value of ratio of AlCl 3 /TiCl 4 in n-th film formation−value of ratio of AlCl 3 /TiCl 4 in first film formation)/(n−1) ) Refers to the value obtained.
さらに、比較の目的で、工具基体Ａ〜Ｆの表面に表３、表４に示される形成条件を示す形成記号ａ〜ｈでＣＶＤ法により成膜を行うことによって、表６に示される平均層厚を有するＴｉＡｌＣＮ層を含む硬質被覆層を蒸着形成して比較被覆工具１〜１６を製造した。
なお、ｂ１〜ｆ１、ｂ２〜ｆ２は、それぞれ、前述の過程１、過程２に相当し、区間１は第１回目の成膜、区間ｎは最終の成膜、すなわち、第ｎ回目の成膜である。区間の表示のないものは成膜期間中のガス組成の変化がないものである。
Further, for the purpose of comparison, by forming a film on the surfaces of the tool bases A to F by the CVD method with the formation symbols a to h indicating the formation conditions shown in Tables 3 and 4, the average layer shown in Table 6 is obtained. Comparative coated tools 1-16 were prepared by depositing a hard coating layer including a TiAlCN layer having a thickness.
It should be noted that b1 to f1 and b2 to f2 correspond to the above-described steps 1 and 2, respectively, and the section 1 is the first film formation and the section n is the final film formation, that is, the nth film formation. Is. In the case where no section is displayed, the gas composition does not change during the film formation period.
本発明のＴｉＡｌＣＮ層の平均層厚は、それぞれ、本発明被覆工具１〜１６、比較被覆工具１〜１６の構成層の工具基体表面に垂直な方向の断面（縦断面、層厚方向の断面）を、走査型電子顕微鏡を用いて適切な倍率(倍率５０００倍)を選択して観察し、観察視野内の５点の層厚を測って平均して求めた。 The average layer thickness of the TiAlCN layer of the present invention is a cross section in the direction perpendicular to the tool substrate surface of the constituent layers of the present coated tools 1 to 16 and comparative coated tools 1 to 16 (longitudinal section, section in the layer thickness direction). Was observed by selecting an appropriate magnification (magnification: 5000 times) using a scanning electron microscope, and the layer thickness at 5 points in the observation visual field was measured and averaged.
また、本発明のＴｉＡｌＣＮ層におけるＮａＣｌ型の面心立方構造を有する結晶粒の面積割合、粒子幅Ｗおよびアスペクト比Ａは、研磨して作製した、前記ＴｉＡｌＣＮ層の工具基体表面に垂直な方向の断面（縦断面、層厚方向の断面）に対して測定範囲を、工具基体表面に平行な方向（層厚方向に垂直な方向）に１００μｍ、工具基体表面と垂直な方向に層厚分の長さの範囲の四角形とし、電子線後方散乱回折（Ｅｌｅｃｔｒｏｎ Ｂａｃｋｓｃａｔｔｅｒ Ｄｉｆｆｒａｃｔｉｏｎ：ＥＢＳＤ）装置を用いて、前記測定範囲に７０度の入射角度で１５ｋＶの加速電圧の電子線を１ｎＡの照射電流で、電子線を０．０１μｍ間隔で照射して得られるＥＢＳＤ像に基づいて、個々の結晶粒の結晶構造を解析することにより求めた。すなわち、隣接する測定点（ピクセル）間で５度以上の方位差がある場合、そこを粒界と定義し、さらに粒界で囲まれた領域を１つの結晶粒と定義する。ただし、隣接するピクセル全てと５度以上の方位差がある単独に存在するピクセルは結晶粒とせず、２ピクセル以上が連結しているものを結晶粒として取り扱う。次に、ある結晶粒の層厚方向の最大長さをｌ、該結晶粒の面積をＳとして求めて、該結晶粒の粒子幅ｗはｗ＝Ｓ／ｌとして、さらに、アスペクト比ａはｌ／ｗとして算出する。このようにして算出した任意の２０個の結晶粒の粒子幅およびアスペクト比を面積平均し、平均粒子幅Ｗおよび平均アスペクト比Ａを求めた。 Further, the area ratio, the grain width W and the aspect ratio A of the crystal grains having the NaCl-type face-centered cubic structure in the TiAlCN layer of the present invention are measured in a direction perpendicular to the tool base surface of the TiAlCN layer, which is produced by polishing. The measurement range is 100 μm in the direction parallel to the tool base surface (direction perpendicular to the layer thickness direction) and the length of the layer thickness in the direction perpendicular to the tool base surface, with respect to the cross section (vertical cross section, cross section in the layer thickness direction). In the measurement range, an electron beam with an acceleration voltage of 15 kV and an accelerating voltage of 15 kV is applied to the measurement range using an electron backscatter diffraction (EBSD) device with an irradiation current of 1 nA. Was determined by analyzing the crystal structure of each crystal grain based on the EBSD image obtained by irradiating the crystal at 0.01 μm intervals. That is, when there is an orientation difference of 5 degrees or more between adjacent measurement points (pixels), that is defined as a grain boundary, and a region surrounded by the grain boundaries is defined as one crystal grain. However, a single pixel having an orientation difference of 5 degrees or more with all adjacent pixels is not a crystal grain, and a pixel in which two or more pixels are connected is treated as a crystal grain. Next, the maximum length of a certain crystal grain in the layer thickness direction is 1, the area of the crystal grain is S, the grain width w of the crystal grain is w=S/l, and the aspect ratio a is l. Calculate as /w. The average particle width W and average aspect ratio A were obtained by averaging the particle widths and aspect ratios of the 20 crystal grains thus calculated.
本発明のＴｉＡｌＣＮ層の層厚方向の区間ごとのＡｌの平均含有割合（Ｘａｖｇ）について、該層を測定間隔が０．５μｍとなるように層厚方向、すなわち、工具基体側端面から工具表面に向かって、順にｍ個の区間（区間１、区間２、・・・区間ｍ）に分割し、それぞれの区間に対して、ＥＤＳ（スポット径０．２μｍ）を用いて測定した。すなわち、工具基体表面に垂直な方向の断面（縦断面、層厚方向の断面）を研磨した試料において、電子線を試料縦断面側から照射し、該層を測定間隔が０．５μｍとなるように層厚方向に分割したときの各区間におけるＡｌの含有割合を、工具基体表面に平行な方向に５点測定し、得られた特性Ｘ線の解析結果の平均から求めた。
ここで、区間ｉに対するＡｌの平均含有割合（Ｘａｖｇ）をＸｉとするとき、Ａｌの平均含有割合がＴｉＡｌＣＮ層の層厚方向において工具表面に向かって単調増加するとは、すべての区間（区間１、区間２、・・・区間ｍ）においてＸｉ＜Ｘｉ＋１となることをいう。
Regarding the average content ratio (X avg ) of Al for each section of the TiAlCN layer of the present invention in the layer thickness direction, the layer is measured in the layer thickness direction, that is, from the tool substrate side end surface to the tool surface so that the measurement interval is 0.5 μm. Toward m., it was divided into m sections (section 1, section 2,... Section m) in sequence, and each section was measured using EDS (spot diameter 0.2 μm). That is, in a sample in which a cross section perpendicular to the tool base surface (longitudinal cross section, cross section in the layer thickness direction) is polished, an electron beam is irradiated from the sample vertical cross section side so that the measurement interval of the layer becomes 0.5 μm. The content ratio of Al in each section when divided in the layer thickness direction was measured at 5 points in the direction parallel to the surface of the tool substrate, and was obtained from the average of the analysis results of the obtained characteristic X-rays.
Here, when the average content ratio (X avg ) of Al to the section i is Xi, it means that the average content rate of Al monotonically increases toward the tool surface in the layer thickness direction of the TiAlCN layer in all sections (section 1 , Section 2,... Section m), Xi<Xi+1.
Ｃの平均含有割合Ｙａｖｇについては、二次イオン質量分析（Ｓｅｃｏｎｄａｒｙ Ｉｏｎ Ｍａｓｓ Ｓｐｅｃｔｒｏｍｅｔｒｙ：ＳＩＭＳ）により求めた。イオンビームを試料縦断面側から２０μｍ×２０μｍの範囲に照射し、スパッタリング作用によって放出された成分について層厚方向の濃度測定を行った。Ｃの平均含有割合ＹａｖｇはＴｉＡｌＣＮ層の層厚方向の平均値を示す。 The average content ratio Y avg of C was determined by secondary ion mass spectrometry (Secondary Ion Mass Spectrometry: SIMS). The ion beam was irradiated to a range of 20 μm×20 μm from the side of the longitudinal section of the sample, and the concentration of the component released by the sputtering action was measured in the layer thickness direction. The average content ratio C avg of C represents the average value in the layer thickness direction of the TiAlCN layer.
また、領域αのＡｌの平均含有割合Ｘαａｖｇ、領域βのＡｌの平均含有割合Ｘβａｖｇは、ＴＥＭを用いたＥＤＳ（スポット径０．０１μｍ）により測定した。 The average Al content Xα avg in the region α and the average Al content Xβ avg in the region β were measured by EDS (spot diameter 0.01 μm) using a TEM.
六方晶結晶粒の占める面積割合については、測定範囲を、工具基体表面に平行な方向（層厚方向に垂直な方向）に１００μｍ、工具基体表面と垂直な方向に層厚分の長さの範囲の四角形とし、前記ＴｉＡｌＣＮ層の工具基体表面に垂直な方向の断面（縦断面、層厚方向の断面）を研磨し、ＥＢＳＤを用いて、前記測定範囲に７０度の入射角度で１５ｋＶの加速電圧の電子線を１ｎＡの照射電流で、電子線を０．０１μｍ間隔で前記断面研磨面の測定範囲内に存在する結晶粒個々に照射して得られるＥＢＳＤ像に基づいて、個々の結晶粒の結晶構造を解析することで隣り合うＮａＣｌ型の面心立方構造を有する結晶粒の粒界部に存在する結晶粒が六方晶であることを同定し、その結晶粒の占める面積割合を求めた。なお、前記測定範囲はＬ１、Ｌ３の線分を引いた箇所を含むものである。
さらに該結晶粒の平均粒径Ｒは、該結晶粒が見出されるＮａＣｌ型の面心立方構造を有する結晶粒の粒界のうち、複数の観察視野から任意の粒界３か所を選び、選んだ粒界に存在する個々の該結晶粒の面積を求め、その面積と等しい面積を持つ円の直径を算出し、平均粒径Ｒとした。
以上の結果を、表５、６に示す。
Regarding the area ratio of the hexagonal crystal grains, the measurement range is 100 μm in the direction parallel to the tool base surface (direction perpendicular to the layer thickness direction), and the range of the length of the layer thickness in the direction perpendicular to the tool base surface. And a cross section of the TiAlCN layer in the direction perpendicular to the tool substrate surface (longitudinal section, section in the layer thickness direction) is polished, and an acceleration voltage of 15 kV is applied to the measurement range at an incident angle of 70 degrees using EBSD. Of the individual crystal grains based on the EBSD image obtained by irradiating each of the crystal grains existing in the measurement range of the cross-section polished surface with the electron beam of 1 nA at an irradiation current of 1 nA. By analyzing the structure, it was identified that the crystal grains existing in the grain boundary part of the crystal grains having the NaCl-type face-centered cubic structure adjacent to each other were hexagonal crystals, and the area ratio occupied by the crystal grains was obtained. The measurement range includes a portion where line segments L1 and L3 are drawn.
Further, the average grain size R of the crystal grains is selected by selecting three arbitrary grain boundaries from a plurality of observation fields among grain boundaries of the crystal grains having a NaCl type face-centered cubic structure in which the crystal grains are found. The area of each of the crystal grains present at the ovary boundaries was determined, the diameter of a circle having an area equal to the area was calculated, and the average particle diameter R was obtained.
The above results are shown in Tables 5 and 6.
次に、前記各種の被覆工具Ａ〜Ｃ（ＩＳＯ規格ＳＥＥＮ１２０３ＡＦＳＮ形状）をいずれもカッタ径１２５ｍｍの合金鋼製カッタ先端部に固定治具にてクランプした状態で、本発明被覆工具１〜８、比較被覆工具１〜８について、以下に示す、合金鋼の高速断続切削の一種である乾式高速正面フライス、センターカット切削加工試験を実施し、切刃の逃げ面摩耗幅を測定して、その結果を表７（切削試験１）に示す。
＜切削試験１＞
カッタ径： １２５ｍｍ
被削材： ＪＩＳ・ＳＣＭ４４０ 幅１００ｍｍ、長さ４００ｍｍのブロック材
回転速度： １０１９ ｍｉｎ−１
切削速度： ４００ ｍ／ｍｉｎ
切り込み： ２．０ ｍｍ
一刃送り量：０．３ ｍｍ／刃
切削時間： １８分
（通常の切削速度は、２００ｍ／ｍｉｎ）
Next, all of the various coated tools A to C (ISO standard SEEN1203AFSN shape) were clamped by a fixing jig on the tip of the alloy steel cutter having a cutter diameter of 125 mm, and the coated tools 1 to 8 of the present invention were compared. For the coated tools 1 to 8, the following dry high-speed face milling, which is a type of high-speed intermittent cutting of alloy steel, and a center-cut cutting test were carried out, the flank wear width of the cutting edge was measured, and the result was obtained. It shows in Table 7 (cutting test 1).
<Cutting test 1>
Cutter diameter: 125mm
Work Material: JIS SCM440 Block Material with 100 mm Width and 400 mm Length Rotational Speed: 1019 min -1
Cutting speed: 400 m/min
Notch: 2.0 mm
Single blade feed: 0.3 mm/blade cutting time: 18 minutes (normal cutting speed is 200 m/min)
また、前記各種の被覆工具Ｄ〜Ｆ（ＩＳＯ規格ＣＮＭＧ１２０４１２形状）をいずれも合金鋼製バイトの先端部に固定治具にてネジ止めした状態で、本発明被覆工具９〜１６、比較被覆工具９〜１６について、以下に示す、高炭素鋼の乾式高速断続切削試験を実施し、切刃の逃げ面摩耗幅を測定して、その結果を表８（切削試験２）に示す。
＜切削試験２＞
被削材： ＪＩＳ・Ｓ５５Ｃの長さ方向等間隔４本縦溝入り丸棒
切削速度： ３３０ ｍ／ｍｉｎ
切り込み： ３．０ ｍｍ
一刃送り量：０．３ ｍｍ／刃
切削時間： ６分
（通常の切削速度は、２００ｍ／ｍｉｎ）
Further, all of the various coated tools D to F (ISO standard CNMG120412 shape) are screwed to the tip end of the alloy steel bite with a fixing jig, and coated tools 9 to 16 of the present invention and comparative coated tool 9 The following items were subjected to the dry high speed intermittent cutting test of high carbon steel for Nos. 16 to 16 to measure the flank wear width of the cutting edge, and the results are shown in Table 8 (cutting test 2).
<Cutting test 2>
Work Material: JIS/S55C, 4 lengthwise equally spaced round bars with longitudinal grooves Cutting speed: 330 m/min
Notch: 3.0 mm
Single blade feed: 0.3 mm/Blade cutting time: 6 minutes (normal cutting speed is 200 m/min)
表７、表８に示される結果から、本発明の被覆工具は、ＴｉＡｌＣＮ層の層厚方向において工具基体側端面から工具表面側に向かって、Ａｌの平均含有割合が増加すること、及び、前記線分Ｌ１およびＬ３上において、ＴｉＡｌＣＮ層のＡｌの平均含有割合がＮａＣｌ型の面心立方構造を有する結晶粒における粒界近傍領域と該領域でない領域との間では、前記関係式を満足することから靭性が高く、その結果、高熱発生を伴い、かつ、切れ刃に断続的・衝撃的高負荷が作用する合金鋼や高炭素鋼の高速断続切削加工に用いた場合でも、チッピングの発生もなく、長期の使用にわたって優れた耐摩耗性を発揮する。 From the results shown in Table 7 and Table 8, in the coated tool of the present invention, the average content ratio of Al increases from the tool substrate side end surface to the tool surface side in the layer thickness direction of the TiAlCN layer, and On the line segments L1 and L3, the above relational expression should be satisfied between the grain boundary vicinity region and the region other than the grain boundary region in the crystal grain having an average Al content in the TiAlCN layer of the NaCl type face centered cubic structure. High toughness, resulting in high heat generation, and no chipping even when used for high-speed intermittent cutting of alloy steel or high carbon steel where cutting edge is subjected to intermittent/impact high load Exhibits excellent wear resistance over long-term use.
これに対して、ＴｉＡｌＣＮ層において、上記本発明の特徴を一つでも有していない比較被覆工具は、合金鋼や高炭素鋼の高速断続切削加工において、チッピング等の異常損傷の発生、あるいは、摩耗進行により、短時間で寿命に至ることが明らかである。 On the other hand, in the TiAlCN layer, the comparative coated tool which does not have any one of the features of the present invention causes abnormal damage such as chipping in high speed interrupted cutting of alloy steel or high carbon steel, or It is clear that the progress of wear leads to a short life.
なお、前記実施例では設けていないが、Ｔｉの炭化物層、窒化物層、炭窒化物層、炭酸化物層および炭窒酸化物層のうちの１層または２層以上からなり、０．１〜２０．０μｍの合計平均層厚を有するＴｉ化合物層を含む下部層、および／または、少なくとも酸化アルミニウム層を含む１．０〜２５．０μｍの合計平均層厚を有する上部層を設けてもよい。 Although not provided in the above-mentioned embodiment, it is composed of one or more layers of a Ti carbide layer, a nitride layer, a carbonitride layer, a carbon oxide layer and a carbonitride oxide layer. A lower layer comprising a Ti compound layer having a total average layer thickness of 20.0 μm and/or an upper layer having a total average layer thickness of 1.0 to 25.0 μm including at least an aluminum oxide layer may be provided.
前述のように、本発明の被覆工具は、合金鋼や高炭素鋼の高速断続切削加工ばかりでなく、各種の被削材の被覆工具として用いることができ、しかも、長期の使用にわたって優れた切削性能を発揮するものであるから、切削装置の高性能化並びに切削加工の省力化および省エネ化、さらに低コスト化に十分に満足する対応が可能である。 As described above, the coated tool of the present invention can be used not only for high-speed intermittent cutting of alloy steel and high carbon steel, but also as a coated tool for various work materials, and is excellent in cutting over long-term use. Since it exerts its performance, it is possible to fully satisfy the requirements for high performance of cutting equipment, labor saving and energy saving of cutting, and cost reduction.
Claims (2)
（ａ）前記硬質被覆層は、平均層厚１．０〜２０．０μｍのＴｉとＡｌの複合窒化物層または複合炭窒化物層を少なくとも含み、
（ｂ）前記複合窒化物層または複合炭窒化物層は、ＮａＣｌ型の面心立方構造を有する複合窒化物または複合炭窒化物の結晶粒の占める割合が８０面積％以上であり、
（ｃ）前記複合窒化物層または複合炭窒化物層について該層の縦断面を観察した場合に、前記複合窒化物層または複合炭窒化物層内の前記ＮａＣｌ型の面心立方構造を有する結晶粒は、平均粒子幅Ｗが０．１０〜２．００μｍ、平均アスペクト比Ａが２．０〜１０．０であり、
（ｄ）前記複合窒化物層または複合炭窒化物層は、
組成式：（Ｔｉ１−ＸＡｌＸ）（ＣＹＮ１−Ｙ）
で表した場合、０．５μｍの間隔で該層を層厚方向に複数の区間に分割したとき、各区間におけるＡｌのＴｉとＡｌの合量に占める平均含有割合Ｘａｖｇが０．６０≦Ｘａｖｇ≦０．９５を満足し、また、該層全体におけるＣのＣとＮの合量に占める平均含有割合Ｙａｖｇが０．０００≦Ｙａｖｇ≦０．００５を満足し、（但し、Ｘａｖｇ、Ｙａｖｇはいずれも原子比）
（ｅ）前記複合窒化物層または複合炭窒化物層において、前記Ａｌの平均含有割合Ｘａｖｇが該層の層厚方向において工具表面に向かって増加し、
（ｆ）前記複合窒化物層または複合炭窒化物層において、前記ＮａＣｌ型の面心立方構造を有する隣り合う２つの結晶粒の粒界から粒内に１０ｎｍ入り込んだ曲線ｍに囲まれた範囲を領域α、該曲線ｍと粒界に囲まれた範囲を領域βとし、前記工具基体表面に平行に複数の前記隣り合う結晶粒の粒界を貫通する線分を、前記層の厚さを６等分する間隔で５本引いたとき、層厚方向で最も工具基体側端面に近い線分Ｌ１および中央に位置する線分Ｌ３上のいずれにおいても、
関係式：Ｘαａｖｇ≦０．９０のときＸαａｖｇ＋０．１０≦Ｘβａｖｇ≦１．００、０．９０＜ＸαａｖｇのときＸαａｖｇ＋０．０５≦Ｘβａｖｇ≦１．００（ただし、Ｘαａｖｇ及びＸβａｖｇはそれぞれ前記領域αおよび前記領域βにおけるＡｌのＴｉとＡｌの合量に占める含有割合の平均値）
を満足する、
ことを特徴とする表面被覆切削工具。 On the surface of the tool base, in a surface-coated cutting tool provided with a hard coating layer,
(A) The hard coating layer includes at least a composite nitride layer or a composite carbonitride layer of Ti and Al having an average layer thickness of 1.0 to 20.0 μm,
(B) In the composite nitride layer or the composite carbonitride layer, the ratio of the crystal grains of the composite nitride or the composite carbonitride having the NaCl-type face-centered cubic structure is 80 area% or more,
(C) A crystal having the NaCl-type face-centered cubic structure in the composite nitride layer or the composite carbonitride layer, when the longitudinal section of the composite nitride layer or the composite carbonitride layer is observed. The particles have an average particle width W of 0.10 to 2.00 μm and an average aspect ratio A of 2.0 to 10.0,
(D) The composite nitride layer or the composite carbonitride layer is
Compositional formula: (Ti 1-X Al X )(C Y N 1-Y )
When the layer is divided into a plurality of sections in the layer thickness direction at intervals of 0.5 μm, the average content ratio X avg of Al in Ti and Al in each section is 0.60≦X. avg ≤ 0.95, and the average content Y avg of C in the total amount of C and N in the entire layer satisfies 0.000 ≤ Y avg ≤ 0.005 (provided that X avg , Y avg are all atomic ratios)
(E) In the composite nitride layer or the composite carbonitride layer, the average content ratio X avg of Al increases toward the tool surface in the layer thickness direction of the layer,
(F) In the composite nitride layer or the composite carbonitride layer, a range surrounded by a curve m in which 10 nm is inserted into the grain from the grain boundary of two adjacent crystal grains having the NaCl-type face-centered cubic structure A region α, a region surrounded by the curve m and the grain boundary is defined as a region β, and a line segment penetrating the grain boundaries of the plurality of adjacent crystal grains in parallel to the tool base surface has a layer thickness of 6 When five lines are drawn at equal intervals, both on the line segment L1 closest to the tool base side end face and the line segment L3 located at the center in the layer thickness direction,
Relationship: Xα avg Xα avg + 0.10 ≦ when ≦ 0.90 Xβ avg ≦ 1.00,0.90 <When Xα avg Xα avg + 0.05 ≦ Xβ avg ≦ 1.00 ( provided that, X [alpha avg and Xβ avg is the average value of the content ratio of Al in the total amount of Ti and Al in the regions α and β, respectively.
Satisfy,
A surface-coated cutting tool characterized in that
Individual crystals having the NaCl-type face-centered cubic structure in the composite nitride layer or the composite carbonitride layer when the longitudinal section of the composite nitride layer or the composite carbonitride layer is observed. The area ratio of the crystal grains having a wurtzite structure existing in the grain boundaries of the grains is 5.0 area% or less, and the average grain size R of the crystal grains is 0.50 μm or less. Item 1. The surface-coated cutting tool according to Item 1.
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| JP2015163423A (en) * | 2014-01-31 | 2015-09-10 | 三菱マテリアル株式会社 | Surface coated cutting tool whose hard coating layer exerts excellent chipping resistance in high-speed intermittent cutting work |
| JP2016030319A (en) * | 2014-07-30 | 2016-03-07 | 三菱マテリアル株式会社 | Surface coated cutting tool having hard coating layer exhibiting superior chipping resistance |
| JP2016049573A (en) * | 2014-08-28 | 2016-04-11 | 三菱マテリアル株式会社 | Surface-coated cutting tool allowing hard coating layer to exhibit superior chipping resistance |
| JP2018522748A (en) * | 2015-07-27 | 2018-08-16 | ヴァルター アーゲー | Tool with TiAlN coating |
| JP2018144115A (en) * | 2017-03-01 | 2018-09-20 | 三菱マテリアル株式会社 | Surface-coated cutting tool having hard coating layer excellent in chipping resistance and peeling resistance |
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| JP2015163423A (en) * | 2014-01-31 | 2015-09-10 | 三菱マテリアル株式会社 | Surface coated cutting tool whose hard coating layer exerts excellent chipping resistance in high-speed intermittent cutting work |
| JP2016030319A (en) * | 2014-07-30 | 2016-03-07 | 三菱マテリアル株式会社 | Surface coated cutting tool having hard coating layer exhibiting superior chipping resistance |
| JP2016049573A (en) * | 2014-08-28 | 2016-04-11 | 三菱マテリアル株式会社 | Surface-coated cutting tool allowing hard coating layer to exhibit superior chipping resistance |
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