JP5187570B2 - Surface coated cutting tool with excellent wear resistance due to hard coating layer - Google Patents
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この発明は、各種の鋼や鋳鉄などの被削材の切削加工を、高い発熱を伴いかつ切刃に対して高負荷が作用する高速重切削条件で行った場合でも、硬質被覆層がチッピングを発生することなく、長期の使用に亘ってすぐれた耐摩耗性を発揮する表面被覆切削工具（以下、被覆工具という）に関するものである。 The present invention enables the hard coating layer to chip even when cutting various work materials such as steel and cast iron under high-speed heavy cutting conditions with high heat generation and high load acting on the cutting edge. The present invention relates to a surface-coated cutting tool (hereinafter referred to as a coated tool) that exhibits excellent wear resistance over a long period of use without being generated.
従来、炭化タングステン（以下、ＷＣで示す）基超硬合金または炭窒化チタン（以下、ＴｉＣＮで示す）基サーメットで構成された基体（以下、これらを総称して工具基体という）の表面に、硬質被覆層として、Ｔｉ化合物層からなる下部層およびα型Ａｌ2Ｏ3層からなる上部層を蒸着形成した被覆工具において、
上部層について、電界放出型走査電子顕微鏡と電子後方散乱回折像装置を用い、表面研磨面の測定範囲内に存在する結晶粒個々に電子線を照射して、六方晶結晶格子からなる結晶粒の構成結晶面のそれぞれの法線が前記表面研磨面の法線と交わる角度を測定し、この測定結果から、隣接する結晶粒の相互の結晶方位関係を算出し、界面を構成する構成原子のそれぞれが前記結晶粒相互間で１つの構成原子を共有する格子点（構成原子共有格子点）の分布を算出し、前記構成原子共有格子点間に構成原子を共有しない格子点がＮ個（但し、Ｎはコランダム型六方最密晶の結晶構造上２以上の偶数となるが、分布頻度の点からＮの上限を２８とした場合、４、８、１４、２４および２６の偶数は存在せず）存在する構成原子共有格子点形態をΣＮ＋１で表した場合に、
個々のΣＮ＋１がΣＮ＋１全体に占める分布割合を示す構成原子共有格子点分布グラフにおいて、Σ３に最高ピークが存在し、かつ前記Σ３のΣＮ＋１全体に占める分布割合が６０〜８０％である構成原子共有格子点分布グラフを示すα型Ａｌ2Ｏ3層で上部層を構成した被覆工具が知られ、この被覆工具が、高速断続切削加工ですぐれた耐チッピング性を発揮することが知られている。
また、前記の被覆工具において、その上部層を、Ｚｒを少量含有するα型（Ａｌ，Ｚｒ）2Ｏ3層（以下、従来ＡｌＺｒＯ層という）で構成した被覆工具（以下、従来被覆工具という）も知られており、そして、この従来被覆工具も、前記同様、高速断続切削加工ですぐれた耐チッピング性を発揮することが知られている。
For the upper layer, using a field emission scanning electron microscope and an electron backscatter diffraction image apparatus, each crystal grain existing within the measurement range of the surface polished surface was irradiated with an electron beam, and a crystal grain composed of a hexagonal crystal lattice was observed. Measure the angle at which each normal of the constituent crystal plane intersects the normal of the surface polished surface, and from this measurement result, calculate the mutual crystal orientation relationship between adjacent crystal grains, and each of the constituent atoms constituting the interface Calculates the distribution of lattice points that share one constituent atom between the crystal grains (constituent atom shared lattice points), and N lattice points that do not share constituent atoms between the constituent atom shared lattice points (however, N is an even number of 2 or more due to the crystal structure of the corundum hexagonal close-packed crystal, but when the upper limit of N is 28 from the point of distribution frequency, the even numbers of 4, 8, 14, 24 and 26 do not exist) ΣN is the configuration of the constituent atomic shared lattice points that exist When expressed in 1,
In the constituent atom shared lattice point distribution graph showing the distribution ratio of each ΣN + 1 in the entire ΣN + 1, the constituent atom shared lattice in which Σ3 has the highest peak and the distribution ratio of the Σ3 in the entire ΣN + 1 is 60 to 80% A coated tool in which an upper layer is formed of an α-type Al 2 O 3 layer showing a point distribution graph is known, and this coated tool is known to exhibit excellent chipping resistance in high-speed intermittent cutting.
Further, in the above-described coated tool, a coated tool (hereinafter referred to as a conventional coated tool) in which the upper layer is composed of an α-type (Al, Zr) 2 O 3 layer containing a small amount of Zr (hereinafter referred to as a conventional AlZrO layer). It is also known that this conventional coated tool exhibits excellent chipping resistance by high-speed interrupted cutting as described above.
近年の切削装置の高性能化はめざましく、一方で切削加工に対する省力化および省エネ化、さらに低コスト化の要求は強く、これに伴い、切削加工はより高速化する傾向になってきているが、上記の従来被覆工具においては、高速連続切削や高速断続切削に用いた場合、上部層がすぐれた高温強度を備え、耐衝撃性にすぐれるため、チッピング等の発生を防止できるという点ですぐれているものの、硬質被覆層の上部層を構成する前記α型Ａｌ2Ｏ3層、前記従来ＡｌＺｒＯ層は、高温強度および表面性状が満足できるものではないため、より高速条件下での重切削加工を行った場合には、チッピングを発生しやすいばかりか、熱塑性変形、偏摩耗をも発生しやすく、これを原因とした耐摩耗性の低下により、比較的短時間で使用寿命に至るのが現状である。 In recent years, the performance of cutting machines has been remarkable. On the other hand, there is a strong demand for labor saving and energy saving and further cost reduction for cutting, and along with this, cutting has become a tendency to increase in speed. The above-mentioned conventional coated tool is excellent in that it can prevent the occurrence of chipping, etc. when it is used for high-speed continuous cutting and high-speed intermittent cutting because the upper layer has excellent high-temperature strength and excellent impact resistance. However, the α-type Al 2 O 3 layer and the conventional AlZrO layer constituting the upper layer of the hard coating layer are not satisfactory in high-temperature strength and surface properties, so that heavy cutting under higher speed conditions is possible. If performed, not only chipping is likely to occur, but also thermoplastic deformation and uneven wear are likely to occur. Due to this decrease in wear resistance, the service life is reached in a relatively short time. Is the current situation.
そこで、本発明者等は、上述のような観点から、特に、より高速条件での切削加工において、硬質被覆層がチッピング、欠損、剥離等を発生することなく、しかも、長期の使用に亘ってすぐれた耐摩耗性を発揮する上部層の構造について研究を行った結果、次のような知見を得た。
（ａ）上記従来被覆工具の従来ＡｌＺｒＯ層からなる上部層は、例えば、通常の化学蒸着装置にて、
第１段階として、
反応ガス組成（容量％）：
ＡｌＣｌ３：２．３〜４％、
ＺｒＣｌ４：０．０２〜０．１３％、
ＣＯ２：１〜５％、
ＨＣｌ：１．５〜３％、
Ｈ2Ｓ：０．０５〜０．２％、
Ｈ2：残り、
反応雰囲気温度：７５０〜９００℃、
反応雰囲気圧力：６〜１０ｋＰａ、
の条件で、下部層であるＴｉ化合物層の表面に、
組成式：（Ａｌ１−ＸＺｒＸ）２Ｏ３、（ただし、原子比で、Ｘ：０．００３〜０．０５）を満足する、好ましくは２０〜２００ｎｍ（０．０２〜０．２μｍ）の平均層厚を有するＡｌ−Ｚｒ複合酸化物核（以下、ＡｌＺｒＯ核という）薄膜を形成し、
引き続いて、加熱雰囲気を圧力：３〜１３ｋＰａの水素雰囲気に変え、かつ加熱雰囲気温度を１１００〜１２００℃に昇温した条件で前記ＡｌＺｒＯ核薄膜に加熱処理を施した状態で、
第２段階として、
反応ガス組成（容量％）：
ＡｌＣｌ３：２．３〜４％、
ＺｒＣｌ４：０．０２〜０．１３％、
ＣＯ２：３〜８％、
ＨＣｌ：１．５〜３％、
Ｈ2Ｓ：０．０５〜０．２％、
Ｈ2：残り、
反応雰囲気温度：１０２０〜１０５０℃、
反応雰囲気圧力：６〜１０ｋＰａ、
の条件で蒸着を行うと、Ａｌ成分との合量に占めるＺｒ成分の含有割合が０．００３〜０．０５（但し、原子比）である組成を有する従来ＡｌＺｒＯ層が形成され、そして、この従来ＡｌＺｒＯ層を電界放出型走査電子顕微鏡で組織観察すると、図２（ａ）に示されるように、層厚方向に垂直な面内で見た場合、微細な多角形状であり、また、図２（ｂ）に示されるように、層厚方向に平行な面内で見た場合、層表面に角錐状の凹凸が存在し、層厚方向にたて長形状（以下、「凹凸多角形たて長形状」という）を有する結晶粒からなる組織構造を有していること。
Therefore, the present inventors, from the above viewpoint, in particular, in the cutting process at higher speed conditions, the hard coating layer does not cause chipping, chipping, peeling, etc., and over a long period of use. As a result of research on the structure of the upper layer that exhibits excellent wear resistance, the following findings were obtained.
(A) The upper layer made of the conventional AlZrO layer of the conventional coated tool is, for example, a normal chemical vapor deposition apparatus.
As the first step,
Reaction gas composition (volume%):
AlCl 3 : 2.3 to 4%,
ZrCl 4 : 0.02 to 0.13%,
CO 2: 1~5%,
HCl: 1.5-3%,
H 2 S: 0.05~0.2%,
H 2 : Remaining
Reaction atmosphere temperature: 750 to 900 ° C.
Reaction atmosphere pressure: 6 to 10 kPa,
On the surface of the Ti compound layer as the lower layer under the conditions
Composition formula: (Al 1-X Zr X ) 2 O 3, ( provided that an atomic ratio, X: 0.003 to 0.05) satisfies preferably 20~200nm (0.02~0.2μm) An Al—Zr composite oxide nucleus (hereinafter referred to as AlZrO nucleus) thin film having an average layer thickness of
Subsequently, the heating atmosphere was changed to a hydrogen atmosphere at a pressure of 3 to 13 kPa, and the heating atmosphere temperature was increased to 1100 to 1200 ° C., and the AlZrO core thin film was subjected to a heat treatment.
As the second stage,
Reaction gas composition (volume%):
AlCl 3 : 2.3 to 4%,
ZrCl 4 : 0.02 to 0.13%,
CO 2: 3~8%,
HCl: 1.5-3%,
H 2 S: 0.05~0.2%,
H 2 : Remaining
Reaction atmosphere temperature: 1020 to 1050 ° C.
Reaction atmosphere pressure: 6 to 10 kPa,
When the vapor deposition is performed, a conventional AlZrO layer having a composition in which the content ratio of the Zr component in the total amount of the Al component is 0.003 to 0.05 (however, atomic ratio) is formed. When the structure of a conventional AlZrO layer is observed with a field emission scanning electron microscope, as shown in FIG. 2 (a), it is a fine polygon when viewed in a plane perpendicular to the layer thickness direction. As shown in (b), when viewed in a plane parallel to the layer thickness direction, there are pyramidal irregularities on the surface of the layer, and a long shape in the layer thickness direction (hereinafter referred to as “irregular polygonal length”). It has a structure of crystal grains having a “long shape”.
（ｂ）一方、硬質被覆層の下部層であるＴｉ化合物層上に、通常の化学蒸着装置にて、
まず、第1段階として、
（イ）反応ガス組成（容量％）：
ＡｌＣｌ３： １〜５ ％、
ＣＯ2： ２〜６ ％、
ＨＣｌ： １〜５ ％、
Ｈ２Ｓ： ０．２５〜０．７５ ％、
Ｈ2：残り、
（ロ）反応雰囲気温度； ９６０〜１０１０ ℃、
（ハ）反応雰囲気圧力； ６〜１０ ｋＰａ、
の条件で第1段階の蒸着を行った後、
次に、第2段階として、
（イ）反応ガス組成（容量％）：
ＡｌＣｌ３： ６〜１０ ％、
ＺｒＣｌ４： ０．６〜１．２ ％、
ＣＯ2： ４〜８ ％、
ＨＣｌ： ３〜５ ％、
Ｈ２Ｓ： ０．２５〜０．６ ％、
Ｈ2：残り、
（ロ）反応雰囲気温度； ９２０〜１０００ ℃、
（ハ）反応雰囲気圧力； ６〜１０ ｋＰａ、
の条件で蒸着を行って、２〜１５μｍの平均層厚のＺｒを含有するα型の酸化アルミニウム層（以下、「改質ＡｌＺｒＯ層」という）からなる上部層を形成すると、
この条件で形成された改質ＡｌＺｒＯ層は、該層におけるＡｌ成分との合量に占めるＺｒ成分の含有割合が０．００２〜０．０１（但し、原子比）を満足する組成を有すること。
(B) On the other hand, on the Ti compound layer which is the lower layer of the hard coating layer, with a normal chemical vapor deposition apparatus,
First, as the first step,
(B) Reaction gas composition (volume%):
AlCl 3 : 1 to 5%,
CO 2 : 2-6%,
HCl: 1-5%,
H 2 S: 0.25~0.75%,
H 2 : Remaining
(B) Reaction atmosphere temperature; 960 to 1010 ° C.,
(C) Reaction atmosphere pressure; 6 to 10 kPa,
After performing the first stage deposition under the conditions of
Next, as the second stage,
(B) Reaction gas composition (volume%):
AlCl 3 : 6 to 10%,
ZrCl 4: 0.6~1.2%,
CO 2: 4~8%,
HCl: 3-5%,
H 2 S: 0.25~0.6%,
H 2 : Remaining
(B) Reaction atmosphere temperature; 920 to 1000 ° C.,
(C) Reaction atmosphere pressure; 6 to 10 kPa,
When an upper layer composed of an α-type aluminum oxide layer containing Zr having an average layer thickness of 2 to 15 μm (hereinafter referred to as “modified AlZrO layer”) is formed under the following conditions:
The modified AlZrO layer formed under these conditions has a composition in which the content ratio of the Zr component in the total amount with the Al component in the layer satisfies 0.002 to 0.01 (however, the atomic ratio).
（ｃ）そして、上記改質ＡｌＺｒＯ層を、電界放出型走査電子顕微鏡で組織観察すると、図１（ａ）に示されるように、層厚方向に垂直な面内で見た場合に、大粒径の平板多角形状であり、また、図１（ｂ）に示されるように、層厚方向に平行な面内で見た場合に、層表面はほぼ平坦であり、層厚方向にたて長形状（以下、「平板多角形たて長形状」という）を有する結晶粒からなる組織構造を有すること。
特に、前記改質ＡｌＺｒＯ層の蒸着形成に際して、より限定した蒸着条件（例えば、第1段階における反応ガス中のＨ２Ｓを０．５０〜０．７５容量％、反応雰囲気温度を９８０〜１０００℃とし、さらに、第2段階における反応ガス中のＺｒＣｌ４を０．６〜０．９容量％、Ｈ２Ｓを０．２５〜０．４容量％、反応雰囲気温度を９６０〜９８０℃とした条件）で蒸着を行うと、図１（ｃ）に示されるように、層厚方向に垂直な面内で見た場合に、大粒径の平坦六角形状であり、かつ、層厚方向に平行な面内で見た場合に、図１（ｂ）に示されるのと同様、層表面はほぼ平坦であり、層厚方向にたて長形状を有する結晶粒が、層厚方向に垂直な面内において全体の３５％以上の面積割合を占める組織構造が形成されるようになること。
そして、該改質ＡｌＺｒＯ層について、電界放出型走査電子顕微鏡と電子後方散乱回折像装置を用い、表面研磨面の測定範囲内に存在する結晶粒個々に電子線を照射して、六方晶結晶格子からなる結晶格子面のそれぞれの法線が前記表面研磨面の法線と交わる角度を測定し、
この測定結果から、隣接する結晶格子相互の結晶方位関係を算出し、結晶格子界面を構成する構成原子のそれぞれが前記結晶格子相互間で１つの構成原子を共有する格子点（構成原子共有格子点）の分布を算出し、前記構成原子共有格子点間に構成原子を共有しない格子点がＮ個（但し、Ｎはコランダム型六方最密晶の結晶構造上２以上の偶数となるが、分布頻度の点からＮの上限を２８とした場合、４、８、１４、２４および２６の偶数は存在せず）存在する構成原子共有格子点形態をΣＮ＋１で表した場合に、
図３に示されるように、改質ＡｌＺｒＯ層を構成する平板多角形たて長形状結晶粒の内、面積比率で６０％以上の上記結晶粒の内部は、少なくとも一つ以上の、Σ３で表される構成原子共有格子点形態からなる結晶格子界面（以下、Σ３対応界面という）で分断されていること。
(C) Then, when the microstructure of the modified AlZrO layer is observed with a field emission scanning electron microscope, as shown in FIG. 1 (a), when it is viewed in a plane perpendicular to the layer thickness direction, large grains As shown in FIG. 1B, when viewed in a plane parallel to the layer thickness direction, the layer surface is almost flat and long in the layer thickness direction. It has a textured structure composed of crystal grains having a shape (hereinafter referred to as “flat plate-shaped polygonal long shape”).
In particular, when the modified AlZrO layer is formed by vapor deposition, more limited vapor deposition conditions (for example, H 2 S in the reaction gas in the first stage is 0.50 to 0.75 vol%, and the reaction atmosphere temperature is 980 to 1000 ° C. And ZrCl 4 in the reaction gas in the second stage is 0.6 to 0.9% by volume, H 2 S is 0.25 to 0.4% by volume, and the reaction atmosphere temperature is 960 to 980 ° C. 1), as shown in FIG. 1C, when viewed in a plane perpendicular to the layer thickness direction, it has a flat hexagonal shape with a large grain size and is parallel to the layer thickness direction. When viewed in-plane, as shown in FIG. 1B, the layer surface is substantially flat, and crystal grains having a long shape in the layer thickness direction are in-plane perpendicular to the layer thickness direction. In order to form a tissue structure occupying an area ratio of 35% or more of the whole.
Then, the modified AlZrO layer is irradiated with an electron beam on each crystal grain existing within the measurement range of the surface polished surface using a field emission scanning electron microscope and an electron backscatter diffraction image apparatus, and a hexagonal crystal lattice Measure the angle at which each normal of the crystal lattice plane consisting of intersects with the normal of the surface polished surface,
From this measurement result, the crystal orientation relationship between adjacent crystal lattices is calculated, and each of the constituent atoms constituting the crystal lattice interface shares one constituent atom between the crystal lattices (constituent atom shared lattice point). ) And the number of lattice points that do not share constituent atoms between the constituent atomic shared lattice points (where N is an even number of 2 or more on the crystal structure of the corundum hexagonal close-packed crystal, but the distribution frequency) In the case where the upper limit of N is 28 from this point, even numbers of 4, 8, 14, 24 and 26 do not exist)
As shown in FIG. 3, at least one of the above-described crystal grains having an area ratio of 60% or more among the flat plate-shaped long crystal grains constituting the modified AlZrO layer is represented by Σ3. It is divided at the crystal lattice interface (hereinafter referred to as Σ3-compatible interface) composed of the constituent atomic shared lattice point form.
（ｄ）上記（ｂ）の第１段階および第２段階の化学蒸着条件（以下、本発明条件という）で蒸着形成された改質ＡｌＺｒＯ層からなる上部層は、その表面の結晶面が、該層の層厚方向に垂直な面内における結晶面（例えば、（０００１））と同配向を有するため、（層厚方向に平行な面内で見た場合、）層表面はほぼ平坦な平板状に形成され、その表面性状の故にすぐれた耐チッピング性を示し、さらに、平板多角形たて長形状の結晶粒内部のΣ３対応界面の存在によって結晶粒内強度が高められるため、従来被覆工具の従来ＡｌＺｒＯ層に比して、一段とすぐれた高温硬さ、高温強度、表面性状を具備し、その結果として、本発明の改質ＡｌＺｒＯ層は、高い発熱を伴うとともに切刃部に高負荷が作用する高速重切削加工においても、チッピング、欠損、剥離等を発生することもなく、すぐれた耐摩耗性を長期に亘って発揮すること。 (D) The upper layer composed of the modified AlZrO layer formed by vapor deposition under the chemical vapor deposition conditions of the first stage and the second stage of the above (b) (hereinafter referred to as the present invention conditions) has a crystal plane on the surface, Since it has the same orientation as a crystal plane (for example, (0001)) in a plane perpendicular to the layer thickness direction, the layer surface is almost flat (when viewed in a plane parallel to the layer thickness direction). In addition, it exhibits excellent chipping resistance due to its surface properties, and furthermore, the presence of the Σ3 corresponding interface inside the plate-shaped polygonal long-shaped crystal grains enhances the intra-grain strength. Compared to the conventional AlZrO layer, it has superior high-temperature hardness, high-temperature strength, and surface properties. As a result, the modified AlZrO layer of the present invention is accompanied by high heat generation and high load on the cutting edge. Even in high-speed heavy cutting, Ring, defect, without generating a peeling, to exert over the superior wear resistance to long term.
この発明は、上記の知見に基づいてなされたものであって、
「（１） 炭化タングステン基超硬合金または炭窒化チタン基サーメットで構成された工具基体の表面に、
（ａ）下部層が、３〜２０μｍの全体平均層厚を有する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層以上からなるＴｉ化合物層、
（ｂ）上部層が、２〜１５μｍの平均層厚を有し、かつ、α型の結晶構造を有しＺｒを含有する酸化アルミニウム層、
上記（ａ）、（ｂ）からなる硬質被覆層を蒸着形成した表面被覆切削工具において、
上記上部層を、電界放出型走査電子顕微鏡で組織観察した場合に、層厚方向に垂直な面内で平板多角形状、また、層厚方向に平行な面内で層厚方向にたて長形状を有する結晶粒からなる組織構造を有し、さらに、
該上部層について、電界放出型走査電子顕微鏡と電子後方散乱回折像装置を用い、表面研磨面の測定範囲内に存在する結晶粒個々に電子線を照射して、六方晶結晶格子からなる結晶格子面のそれぞれの法線が前記表面研磨面の法線と交わる角度を測定し、
この測定結果から、隣接する結晶格子相互の結晶方位関係を算出し、結晶格子界面を構成する構成原子のそれぞれが前記結晶格子相互間で１つの構成原子を共有する格子点（構成原子共有格子点）の分布を算出し、前記構成原子共有格子点間に構成原子を共有しない格子点がＮ個（但し、Ｎはコランダム型六方最密晶の結晶構造上２以上の偶数となるが、分布頻度の点からＮの上限を２８とした場合、４、８、１４、２４および２６の偶数は存在せず）存在する構成原子共有格子点形態をΣＮ＋１で表した場合に、
上記上部層を構成する結晶粒の内、面積比率で６０％以上の結晶粒の内部は、少なくとも一つ以上の、Σ３で表される構成原子共有格子点形態からなる結晶格子界面により分断されていることを特徴とする表面被覆切削工具（被覆工具）。
（２） 前記上部層（ｂ）を電界放出型走査電子顕微鏡で組織観察した場合に、層厚方向に垂直な面内で平坦六角形状、また、層厚方向に平行な面内で層厚方向にたて長形状を有する結晶粒が、層厚方向に垂直な面内において全体の３５％以上の面積割合を占める前記（１）に記載の表面被覆切削工具（被覆工具）。」
に特徴を有するものである。
This invention has been made based on the above findings,
“(1) On the surface of a tool base made of tungsten carbide-based cemented carbide or titanium carbonitride-based cermet,
(A) The lower layer is one or more of Ti carbide layer, nitride layer, carbonitride layer, carbonate layer, and carbonitride oxide layer having an overall average layer thickness of 3 to 20 μm. A Ti compound layer comprising:
(B) The upper layer has an average layer thickness of 2 to 15 μm, and has an α-type crystal structure and contains Zr,
In the surface-coated cutting tool in which the hard coating layer composed of the above (a) and (b) is formed by vapor deposition,
When the upper layer is observed with a field emission scanning electron microscope, the polygonal shape is flat in a plane perpendicular to the layer thickness direction, and is long in the layer thickness direction in a plane parallel to the layer thickness direction. Having a texture structure composed of crystal grains having,
A crystal lattice comprising a hexagonal crystal lattice is formed on the upper layer by using a field emission scanning electron microscope and an electron backscatter diffraction image apparatus to irradiate each crystal grain existing within the measurement range of the surface polished surface with an electron beam. Measure the angle at which each normal of the surface intersects the normal of the surface polished surface,
From this measurement result, the crystal orientation relationship between adjacent crystal lattices is calculated, and each of the constituent atoms constituting the crystal lattice interface shares one constituent atom between the crystal lattices (constituent atom shared lattice point). ) And the number of lattice points that do not share constituent atoms between the constituent atomic shared lattice points (where N is an even number of 2 or more on the crystal structure of the corundum hexagonal close-packed crystal, but the distribution frequency) In the case where the upper limit of N is 28 from this point, even numbers of 4, 8, 14, 24 and 26 do not exist)
Among the crystal grains constituting the upper layer, the interior of the crystal grains having an area ratio of 60% or more is divided by at least one crystal lattice interface composed of a constituent atomic shared lattice point represented by Σ3. A surface-coated cutting tool (coated tool).
(2) When the upper layer (b) is observed with a field emission scanning electron microscope, a flat hexagonal shape is formed in a plane perpendicular to the layer thickness direction, and a layer thickness direction in a plane parallel to the layer thickness direction. The surface-coated cutting tool (coated tool) according to (1), wherein the crystal grains having a long shape occupy an area ratio of 35% or more of the whole in a plane perpendicular to the layer thickness direction. "
It has the characteristics.
以下に、この発明の被覆工具の硬質被覆層の構成層について、より詳細に説明する。
（ａ）下部層（Ｔｉ化合物層）
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層以上からなるＴｉ化合物層は、硬質被覆層の下部層として存在し、自身の具備するすぐれた高温強度によって硬質被覆層の高温強度向上に寄与するほか、工具基体と改質ＡｌＺｒＯ層のいずれにも強固に密着し、よって硬質被覆層の工具基体に対する接合強度を向上させる作用を有するが、その平均層厚が３μｍ未満では、前記作用を十分に発揮させることができず、一方その平均層厚が２０μｍを越えると、特に高熱発生を伴う高速切削では熱塑性変形を起し易くなり、これが偏摩耗の原因となることから、その平均層厚を３〜２０μｍと定めた。
Below, the constituent layer of the hard coating layer of the coated tool of this invention is demonstrated in detail.
(A) Lower layer (Ti compound layer)
Ti compound layer composed of one or more of Ti carbide layer, nitride layer, carbonitride layer, carbonate layer, and carbonitride layer exists as a lower layer of the hard coating layer, In addition to contributing to improving the high temperature strength of the hard coating layer due to its excellent high temperature strength, it firmly adheres to both the tool substrate and the modified AlZrO layer, thereby improving the bonding strength of the hard coating layer to the tool substrate. However, if the average layer thickness is less than 3 μm, the above-mentioned effect cannot be sufficiently exerted. On the other hand, if the average layer thickness exceeds 20 μm, thermoplastic deformation occurs particularly in high-speed cutting with high heat generation. Since this becomes easy and causes uneven wear, the average layer thickness was determined to be 3 to 20 μm.
（ｂ）上部層（改質ＡｌＺｒＯ層）
下部層の上に化学蒸着された改質ＡｌＺｒＯ層からなる上部層は、その構成成分であるＡｌ成分が、層の高温硬さおよび耐熱性を向上させ、また、層中に微量（Ａｌとの合量に占める割合で、Ｚｒ／（Ａｌ＋Ｚｒ）が０．００２〜０．０１（但し、原子比））含有されたＺｒ成分が、改質ＡｌＺｒＯ層の結晶粒界強度を向上させ、高温強度の向上に寄与するが、Ｚｒ成分の含有割合が０．００２未満では、上記作用を期待することはできず、一方、Ｚｒ成分の含有割合が０．０１を超えた場合には、層中にＺｒＯ２粒子が析出することによって粒界強度が低下するため、Ａｌ成分との合量に占めるＺｒ成分の含有割合（Ｚｒ／（Ａｌ＋Ｚｒ）の比の値）は０．００２〜０．０１（但し、原子比）であることが望ましい。
(B) Upper layer (modified AlZrO layer)
In the upper layer composed of the modified AlZrO layer chemically vapor-deposited on the lower layer, the constituent Al component improves the high-temperature hardness and heat resistance of the layer, and there is a slight amount (with Al) in the layer. Zr component containing Zr / (Al + Zr) of 0.002 to 0.01 (however, atomic ratio) in the ratio to the total amount improves the grain boundary strength of the modified AlZrO layer, Although it contributes to improvement, if the content ratio of the Zr component is less than 0.002, the above effect cannot be expected. On the other hand, if the content ratio of the Zr component exceeds 0.01, ZrO is contained in the layer. Since the grain boundary strength decreases due to precipitation of two particles, the content ratio of the Zr component in the total amount with the Al component (value of the ratio of Zr / (Al + Zr)) is 0.002 to 0.01 (however, (Atomic ratio) is desirable.
そして、上記改質ＡｌＺｒＯ層は、蒸着時の反応ガス組成、反応雰囲気温度および反応雰囲気圧力の各化学蒸着条件を、例えば、以下のとおり調整することによって蒸着形成することができる。
即ち、まず、
（イ）反応ガス組成（容量％）：
ＡｌＣｌ３： １〜５ ％、
ＣＯ2： ２〜６ ％、
ＨＣｌ： １〜５ ％、
Ｈ２Ｓ： ０．２５〜０．７５ ％、
Ｈ2：残り、
（ロ）反応雰囲気温度； ９６０〜１０１０ ℃、
（ハ）反応雰囲気圧力； ６〜１０ ｋＰａ、
の条件で第1段階の蒸着を約１時間行った後、
次に、
（イ）反応ガス組成（容量％）：
ＡｌＣｌ３： ６〜１０ ％、
ＺｒＣｌ４： ０．６〜１．２ ％、
ＣＯ2： ４〜８ ％、
ＨＣｌ： ３〜５ ％、
Ｈ２Ｓ： ０．２５〜０．６ ％、
Ｈ2：残り、
（ロ）反応雰囲気温度； ９２０〜１０００ ℃、
（ハ）反応雰囲気圧力； ６〜１０ ｋＰａ、
の条件で第2段階の蒸着を行うことによって、２〜１５μｍの平均層厚の蒸着層を成膜すると、Ｚｒ／（Ａｌ＋Ｚｒ）の比の値が原子比で０．００２〜０．０１である改質ＡｌＺｒＯ層を形成することができる。
And the said modified AlZrO layer can be vapor-deposited by adjusting each chemical vapor deposition conditions, such as the reaction gas composition at the time of vapor deposition, reaction atmospheric temperature, and reaction atmospheric pressure, as follows.
First of all,
(B) Reaction gas composition (volume%):
AlCl 3 : 1 to 5%,
CO 2 : 2-6%,
HCl: 1-5%,
H 2 S: 0.25~0.75%,
H 2 : Remaining
(B) Reaction atmosphere temperature; 960 to 1010 ° C.,
(C) Reaction atmosphere pressure; 6 to 10 kPa,
After performing the first stage deposition for about 1 hour under the conditions of
next,
(B) Reaction gas composition (volume%):
AlCl 3 : 6 to 10%,
ZrCl 4: 0.6~1.2%,
CO 2: 4~8%,
HCl: 3-5%,
H 2 S: 0.25~0.6%,
H 2 : Remaining
(B) Reaction atmosphere temperature; 920 to 1000 ° C.,
(C) Reaction atmosphere pressure; 6 to 10 kPa,
When a vapor deposition layer having an average layer thickness of 2 to 15 μm is formed by performing the second stage vapor deposition under the above conditions, the value of the ratio of Zr / (Al + Zr) is 0.002 to 0.01 in atomic ratio. A modified AlZrO layer can be formed.
そして、上記改質ＡｌＺｒＯ層について、電界放出型走査電子顕微鏡で組織観察すると、図１（ａ）に示されるように、層厚方向に垂直な面内で見た場合に、結晶粒径の大きい平板多角形状であり、また、図１（ｂ）に示されるように、層厚方向に平行な面内で見た場合に、層表面はほぼ平坦であって、しかも、層厚方向にたて長形状を有する結晶粒（平板多角形たて長形状結晶粒）からなる組織構造が形成され、改質ＡｌＺｒＯ層のこの層表面の平坦性により、表面に凹凸が存在する従来ＡｌＺｒＯ層に比して、耐チッピング性が一段と向上する。
特に、前記改質ＡｌＺｒＯ層の蒸着において、より限定した条件（例えば、第1段階における反応ガス中のＨ２Ｓを０．５０〜０．７５容量％、反応雰囲気温度を９８０〜１０００℃とし、さらに、第2段階における反応ガス中のＺｒＣｌ４を０．６〜０．９容量％、Ｈ２Ｓを０．２５〜０．４容量％、反応雰囲気温度を９６０〜９８０℃とした条件）で蒸着を行うと、図１（ｃ）に示されるように、層厚方向に垂直な面内で見た場合に、大粒径の平坦六角形状であり、かつ、層厚方向に平行な面内で見た場合に、図１（ｂ）に示されるのと同様、層表面はほぼ平坦であり、層厚方向にたて長形状を有する結晶粒が、層厚方向に垂直な面内において全体の３５％以上の面積割合を占める組織構造が形成される。
なお、従来ＡｌＺｒＯ層では、その表面の結晶面が、該層の層厚方向に垂直な面内における結晶面（例えば、（０００１））と異なった配向（例えば、（１−１０２）を有するため、（層厚方向に平行な面内で見た場合、）図２（ｂ）に示されるように、層表面に角錐状の凹凸が存在し、これが故に、耐チッピング性の劣るものとなっている。
さらに、改質ＡｌＺｒＯ層について、電界放出型走査電子顕微鏡と電子後方散乱回折像装置を用い、表面研磨面の測定範囲内に存在する結晶粒個々に電子線を照射して、六方晶結晶格子からなる結晶格子面のそれぞれの法線が前記表面研磨面の法線と交わる角度を測定し、
この測定結果から、隣接する結晶格子相互の結晶方位関係を算出し、結晶格子界面を構成する構成原子のそれぞれが前記結晶格子相互間で１つの構成原子を共有する格子点（構成原子共有格子点）の分布を算出し、前記構成原子共有格子点間に構成原子を共有しない格子点がＮ個（但し、Ｎはコランダム型六方最密晶の結晶構造上２以上の偶数となるが、分布頻度の点からＮの上限を２８とした場合、４、８、１４、２４および２６の偶数は存在せず）存在する構成原子共有格子点形態をΣＮ＋１で表すと、
図３に示すように、改質ＡｌＺｒＯ層を構成する上記平板多角形（平坦六角形を含む）たて長形状結晶粒の内、面積比率で６０％以上の結晶粒の内部は、少なくとも一つ以上の、Σ３対応界面で分断されていることがわかる。
そして、改質ＡｌＺｒＯ層の平板多角形（平坦六角形を含む）たて長形状結晶粒の内部に、上記のΣ３対応界面が存在することによって、結晶粒内強度の向上が図られ、その結果として、高速重切削加工時に改質ＡｌＺｒＯ層中にクラックが発生することが抑えられ、また、仮にクラックが発生したとしても、クラックの成長・伝播が妨げられ、耐チッピング性、耐欠損性、耐剥離性の向上が図られる。
When the microstructure of the modified AlZrO layer is observed with a field emission scanning electron microscope, the crystal grain size is large when viewed in a plane perpendicular to the layer thickness direction as shown in FIG. As shown in FIG. 1B, the surface of the layer is substantially flat when viewed in a plane parallel to the layer thickness direction, as shown in FIG. Compared to the conventional AlZrO layer, which has a textured structure composed of crystal grains with long shapes (flat polygonal long and flat crystal grains), and due to the flatness of the surface of the modified AlZrO layer. Therefore, chipping resistance is further improved.
In particular, in the deposition of the modified AlZrO layer, more limited conditions (for example, H 2 S in the reaction gas in the first stage is 0.50 to 0.75 vol%, the reaction atmosphere temperature is 980 to 1000 ° C., Further, the ZrCl 4 in the reaction gas in the second stage is 0.6 to 0.9% by volume, H 2 S is 0.25 to 0.4% by volume, and the reaction atmosphere temperature is 960 to 980 ° C. When vapor deposition is performed, as shown in FIG. 1 (c), when viewed in a plane perpendicular to the layer thickness direction, it is a flat hexagonal shape with a large grain size and in a plane parallel to the layer thickness direction. As shown in FIG. 1B, the layer surface is substantially flat as shown in FIG. 1 (b), and the crystal grains having a long shape in the layer thickness direction are entirely within a plane perpendicular to the layer thickness direction. A tissue structure occupying an area ratio of 35% or more is formed.
In the conventional AlZrO layer, the crystal plane of the surface has an orientation (for example, (1-102)) different from the crystal plane (for example, (0001)) in a plane perpendicular to the layer thickness direction of the layer. (When viewed in a plane parallel to the layer thickness direction) As shown in FIG. 2 (b), pyramidal irregularities exist on the surface of the layer, and therefore chipping resistance is poor. Yes.
Further, for the modified AlZrO layer, using a field emission scanning electron microscope and an electron backscatter diffraction image apparatus, each crystal grain existing in the measurement range of the surface polished surface was irradiated with an electron beam, and the hexagonal crystal lattice was used. Measuring the angle at which each normal of the crystal lattice plane intersects the normal of the surface polished surface,
From this measurement result, the crystal orientation relationship between adjacent crystal lattices is calculated, and each of the constituent atoms constituting the crystal lattice interface shares one constituent atom between the crystal lattices (constituent atom shared lattice point). ) And the number of lattice points that do not share constituent atoms between the constituent atomic shared lattice points (where N is an even number of 2 or more on the crystal structure of the corundum hexagonal close-packed crystal, but the distribution frequency) When the upper limit of N is 28 from this point, the even number of 4, 8, 14, 24 and 26 does not exist.)
As shown in FIG. 3, at least one of the above-mentioned flat plate polygons (including flat hexagonal) long crystal grains constituting the modified AlZrO layer has an area ratio of 60% or more. It turns out that it is divided by the above Σ3 interface.
Further, the presence of the above-mentioned Σ3-corresponding interface inside the long polygonal crystal grains (including flat hexagonal) of the modified AlZrO layer improves the strength within the grains, and as a result As described above, the generation of cracks in the modified AlZrO layer during high-speed heavy cutting is suppressed, and even if cracks occur, the growth and propagation of cracks is hindered, and chipping resistance, chipping resistance, The peelability is improved.
したがって、平板多角形（平坦六角形を含む）たて長形状結晶粒の内部にΣ３対応界面が存在し、表面平坦な表面性状を備えた改質ＡｌＺｒＯ層からなる本発明の上部層は、各種鋼や鋳鉄等の高い発熱を伴い切刃部に対して高負荷が作用する高速重切削加工においても、チッピング、欠損、剥離等を発生することなく、すぐれた耐摩耗性を長期に亘って発揮する。
ただ、改質ＡｌＺｒＯ層からなる上部層の層厚が２μｍ未満では、上記上部層のすぐれた特性を十分に発揮することができず、一方、上部層の層厚が１５μｍを超えると偏摩耗の原因となる熱塑性変形が発生しやすくなり、また、チッピングも発生しやすくなることから、上部層の平均層厚を２〜１５μｍと定めた。
Therefore, the upper layer of the present invention comprising a modified AlZrO layer having a Σ3-compatible interface in the plane polygonal (including flat hexagonal) long-shaped crystal grains and having a flat surface property Even in high-speed heavy cutting where high load is applied to the cutting edge with high heat generation such as steel and cast iron, excellent wear resistance is demonstrated over a long period of time without causing chipping, chipping or peeling. To do.
However, if the thickness of the upper layer made of the modified AlZrO layer is less than 2 μm, the excellent characteristics of the upper layer cannot be fully exhibited, while if the thickness of the upper layer exceeds 15 μm, uneven wear is not achieved. The causative thermoplastic deformation is likely to occur, and chipping is also likely to occur. Therefore, the average layer thickness of the upper layer is set to 2 to 15 μm.
なお、硬質被覆層の上部層が従来ＡｌＺｒＯ層からなる従来被覆工具について、電界放出型走査電子顕微鏡、電子後方散乱回折像装置を用い、上部層の結晶粒の組織構造および構成原子共有格子点形態を調べたところ、結晶粒の組織構造については、図２（ａ）、（ｂ）に示されるような角錐状の凹凸を有し、多角形たて長形状の結晶粒からなる組織構造を有しているため、改質ＡｌＺｒＯ層に比して、耐摩耗性は不十分であった。
また、結晶粒の構成原子共有格子点形態については、従来ＡｌＺｒＯ層を構成する凹凸多角形たて長形状結晶粒の内部にΣ３対応界面が存在する結晶粒の面積比率は、４０％以下と少なく、結晶粒内強度の向上は図られていなかった。
したがって、硬質被覆層の上部層が従来ＡｌＺｒＯ層で構成された従来被覆工具は、高い発熱を伴うとともに切刃部に高負荷が作用する高速重切削加工において、チッピング、欠損、剥離等の発生を防止することはできず、さらに、耐摩耗性も満足できるものではなかった。
In addition, for a conventional coated tool in which the upper layer of the hard coating layer is a conventional AlZrO layer, a field emission scanning electron microscope and an electron backscatter diffraction image apparatus were used, and the crystal structure and constituent atomic shared lattice point form of the upper layer As a result, the crystal grain structure has a pyramid-like unevenness as shown in FIGS. 2 (a) and 2 (b), and has a structure composed of polygonal long crystal grains. Therefore, the wear resistance was insufficient as compared with the modified AlZrO layer.
In addition, regarding the constituent atomic shared lattice point form of the crystal grains, the area ratio of the crystal grains in which the Σ3-corresponding interface exists inside the concave and convex polygonal long crystal grains constituting the conventional AlZrO layer is as low as 40% or less. No improvement in the strength within the crystal grains was achieved.
Therefore, the conventional coated tool in which the upper layer of the hard coating layer is composed of the conventional AlZrO layer does not cause chipping, chipping, peeling, etc. in high-speed heavy cutting with high heat generation and high load acting on the cutting edge. It was not possible to prevent this, and furthermore, the wear resistance was not satisfactory.
上記のとおり、この発明の被覆工具は、上部層を構成する改質ＡｌＺｒＯ層について、表面平坦性を備えた平板多角形（平坦六角形を含む）たて長形状の結晶粒からなる組織構造とし、さらに、上記結晶粒の内部にΣ３対応界面を形成し、結晶粒内強度を強化したことにより、凹凸多角形たて長形状の結晶粒からなり、結晶粒内にΣ３対応界面の少ない従来ＡｌＺｒＯ層を上部層とする従来被覆工具に比して、従来ＡｌＺｒＯ層のもつ高温硬さ、耐熱性に加えて、一段とすぐれた高温強度と一段とすぐれた耐摩耗性を兼備し、その結果、各種の鋼や鋳鉄などを、高い発熱を伴うとともに切刃部に対して高負荷が作用する高速重切削条件下で切削加工した場合にも、硬質被覆層がすぐれた耐チッピング性、耐欠損性、耐剥離性とすぐれた耐摩耗性を発揮し、使用寿命の一層の延命化が可能となる。 As described above, the coated tool of the present invention has a textured structure composed of flat polygons (including flat hexagons) and long crystal grains having surface flatness with respect to the modified AlZrO layer constituting the upper layer. Furthermore, by forming a Σ3-compatible interface inside the crystal grains and strengthening the strength within the crystal grains, the conventional AlZrO is composed of uneven polygonal and long-shaped crystal grains and has few Σ3-compatible interfaces in the crystal grains. Compared with the conventional coated tool with the upper layer as the upper layer, in addition to the high temperature hardness and heat resistance of the conventional AlZrO layer, it has both higher temperature strength and higher wear resistance. Even when steel or cast iron is machined under high-speed heavy cutting conditions with high heat generation and high load acting on the cutting edge, chipping resistance, chipping resistance, Peelability and excellent wear resistance The service life can be further extended.
つぎに、この発明の被覆工具を実施例により具体的に説明する。 Next, the coated tool of the present invention will be specifically described with reference to examples.
原料粉末として、いずれも２〜４μｍの平均粒径を有するＷＣ粉末、ＴｉＣ粉末、ＺｒＣ粉末、ＶＣ粉末、ＴａＣ粉末、ＮｂＣ粉末、Ｃｒ3Ｃ2粉末、ＴｉＮ粉末、ＴａＮ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、この圧粉体を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、切刃部にＲ：０．０７ｍｍのホーニング加工を施すことによりＩＳＯ・ＣＮＭＧ１２０４０８ＭＡに規定するスローアウエイチップ形状をもったＷＣ基超硬合金製の工具基体Ａ〜Ｅをそれぞれ製造した。 WC powder, TiC powder, ZrC powder, VC powder, TaC powder, NbC powder, Cr 3 C 2 powder, TiN powder, TaN powder, and Co powder all having an average particle diameter of 2 to 4 μm are prepared as raw material powders. These raw material powders were blended into the composition shown in Table 1, added with wax, ball milled in acetone for 24 hours, dried under reduced pressure, and pressed into a green compact with a predetermined shape at a pressure of 98 MPa. The green compact was vacuum sintered at a predetermined temperature in the range of 1370 to 1470 ° C. for 1 hour in a vacuum of 5 Pa. After sintering, the cutting edge portion was R: 0.07 mm honing By processing, tool bases A to E made of a WC-based cemented carbide having a throwaway tip shape defined in ISO · CNMG120408MA were produced.
また、原料粉末として、いずれも０．５〜２μｍの平均粒径を有するＴｉＣＮ（質量比でＴｉＣ／ＴｉＮ＝５０／５０）粉末、Ｍｏ2Ｃ粉末、ＺｒＣ粉末、ＮｂＣ粉末、ＴａＣ粉末、ＷＣ粉末、Ｃｏ粉末、およびＮｉ粉末を用意し、これら原料粉末を、表２に示される配合組成に配合し、ボールミルで２４時間湿式混合し、乾燥した後、９８ＭＰａの圧力で圧粉体にプレス成形し、この圧粉体を１．３ｋＰａの窒素雰囲気中、温度：１５４０℃に１時間保持の条件で焼結し、焼結後、切刃部分にＲ：０．０７ｍｍのホーニング加工を施すことによりＩＳＯ規格・ＣＮＭＧ１２０４０８ＭＡのチップ形状をもったＴｉＣＮ基サーメット製の工具基体ａ〜ｅを形成した。 In addition, as raw material powders, TiCN (mass ratio TiC / TiN = 50/50) powder, Mo 2 C powder, ZrC powder, NbC powder, TaC powder, WC powder, all having an average particle diameter of 0.5 to 2 μm. Co powder and Ni powder are prepared, and these raw material powders are blended in the blending composition shown in Table 2, wet mixed by a ball mill for 24 hours, dried, and pressed into a compact at a pressure of 98 MPa. The green compact was sintered in a nitrogen atmosphere of 1.3 kPa at a temperature of 1540 ° C. for 1 hour, and after the sintering, the cutting edge portion was subjected to a honing process of R: 0.07 mm. Tool bases a to e made of TiCN base cermet having a standard / CNMG120408MA chip shape were formed.
ついで、これらの工具基体Ａ〜Ｅおよび工具基体ａ〜ｅのそれぞれを、通常の化学蒸着装置に装入し、まず、表３（表３中のｌ−ＴｉＣＮは特開平６−８０１０号公報に記載される縦長成長結晶組織をもつＴｉＣＮ層の形成条件を示すものであり、これ以外は通常の粒状結晶組織の形成条件を示すものである）に示される条件にて、表６に示される組み合わせおよび目標層厚でＴｉ化合物層を硬質被覆層の下部層として蒸着形成した。
次に、表４に示される蒸着条件により、同じく表６に示される目標層厚の改質ＡｌＺｒＯ層を硬質被覆層の上部層として蒸着形成することにより本発明被覆工具１〜１５をそれぞれ製造した。
Next, each of the tool bases A to E and the tool bases a to e was charged into a normal chemical vapor deposition apparatus. First, Table 3 (l-TiCN in Table 3 is disclosed in JP-A-6-8010). The combinations shown in Table 6 under the conditions shown in Table 6 are the conditions for forming the TiCN layer having the vertically elongated crystal structure described, and other conditions for forming the normal granular crystal structure. And Ti compound layer was vapor-deposited as a lower layer of a hard coating layer with target layer thickness.
Next, according to the deposition conditions shown in Table 4, the coated tools 1 to 15 of the present invention were manufactured by vapor-depositing a modified AlZrO layer having the target layer thickness shown in Table 6 as the upper layer of the hard coating layer. .
また、比較の目的で、本発明被覆工具１〜１５と同条件で下部層を蒸着形成した後、硬質被覆層の上部層として、表５に示される条件で、表７に示される組み合わせおよび目標層厚で従来ＡｌＺｒＯ層を形成することにより従来被覆工具１〜１５をそれぞれ製造した。 For the purpose of comparison, after the lower layer is formed by vapor deposition under the same conditions as the coated tools 1 to 15 of the present invention, the combinations and targets shown in Table 7 are used as the upper layer of the hard coating layer under the conditions shown in Table 5. Conventional coated tools 1-15 were produced by forming conventional AlZrO layers with layer thicknesses, respectively.
ついで、上記の本発明被覆工具１〜１５および従来被覆工具１〜１５の硬質被覆層の上部層を構成する改質ＡｌＺｒＯ層および従来ＡｌＺｒＯ層について、電界放出型走査電子顕微鏡、電子後方散乱回折像装置を用いて、結晶粒組織構造および構成原子共有格子点形態を調査した。
すなわち、まず、上記の本発明被覆工具１〜１５の改質ＡｌＺｒＯ層および従来被覆工具１〜１５の従来ＡｌＺｒＯ層について、電界放出型走査電子顕微鏡を用いて観察したところ、本発明被覆工具では、図１（ａ）、（ｂ）で代表的に示される平板多角形（平坦六角形を含む）状かつたて長形状の大きな粒径の結晶粒組織構造が観察された（なお、図１（ａ）は、層厚方向に垂直な面内で見た本発明被覆工具１〜１０の組織構造模式図、また、図１（ｃ）は、層厚方向に垂直な面内で見た本発明被覆工具１１〜１５の、平坦六角形状かつたて長形状の大きな粒径の結晶粒組織構造模式図）。
一方、従来被覆工具では、図２（ａ）、（ｂ）で代表的に示されるように、多角形状かつたて長形状の結晶粒組織が観察されたが、各結晶粒の粒径は本発明のものに比して小さく、かつ、図２（ｂ）からも明らかなように、層表面には角錐状の凹凸が形成されていた（なお、図２（ａ）、（ｂ）は、従来被覆工具１〜１５の組織構造模式図）。
Next, with respect to the modified AlZrO layer and the conventional AlZrO layer constituting the upper layer of the hard coating layer of the present invention coated tools 1 to 15 and the conventional coated tools 1 to 15, a field emission scanning electron microscope, an electron backscatter diffraction image Using the apparatus, the grain structure and the constituent atomic shared lattice point morphology were investigated.
That is, first, when the modified AlZrO layer of the present invention coated tool 1-15 and the conventional AlZrO layer of the conventional coated tool 1-15 were observed using a field emission scanning electron microscope, 1 (a) and 1 (b), a flat plate polygon (including a flat hexagon) and a long and long crystal grain structure with a large grain size were observed (see FIG. 1 ( a) is a schematic diagram of the structure of the coated tools 1 to 10 of the present invention viewed in a plane perpendicular to the layer thickness direction, and FIG. 1 (c) is the present invention viewed in a plane perpendicular to the layer thickness direction. The flat hexagonal shape and long shape crystal grain structure schematic diagram of the coated tools 11 to 15 ).
On the other hand, in the conventional coated tool, a polygonal and elongated crystal grain structure was observed as representatively shown in FIGS. 2 (a) and 2 (b). As shown in FIG. 2 (b), which is smaller than that of the invention, pyramidal irregularities were formed on the surface of the layer (note that FIGS. 2 (a) and (b) Structure structure schematic diagram of conventional coated tools 1-15 ).
つぎに、上記の本発明被覆工具１〜１５の改質ＡｌＺｒＯ層および従来被覆工具１〜１５の従来ＡｌＺｒＯ層について、それぞれの層を構成する結晶粒の内部にΣ３対応界面が存在する結晶粒の面積割合を測定した。
まず、上記の本発明被覆工具１〜１５の改質ＡｌＺｒＯ層について、その表面を研磨面とした状態で、電界放出型走査電子顕微鏡の鏡筒内にセットし、前記表面研磨面に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、それぞれの前記表面研磨面の測定範囲内に存在する六方晶結晶格子を有する結晶粒個々に電子線を照射して、電子後方散乱回折像装置を用い、３０×５０μｍの領域を０．１μｍ／ｓｔｅｐの間隔で、前記結晶粒の各結晶格子面のそれぞれの法線が前記表面研磨面の法線と交わる角度を測定し、この測定結果から、隣接する結晶格子相互の結晶方位関係を算出し、結晶格子界面を構成する構成原子のそれぞれが前記結晶格子相互間で１つの構成原子を共有する格子点（構成原子共有格子点）の分布を算出し、前記構成原子共有格子点間に構成原子を共有しない格子点がＮ個（但し、Ｎはコランダム型六方最密晶の結晶構造上２以上の偶数となるが、分布頻度の点からＮの上限を２８とした場合、４、８、１４、２４および２６の偶数は存在せず）存在する構成原子共有格子点形態をΣＮ＋１で表した場合に、改質ＡｌＺｒＯ層の測定範囲内に存在する全結晶粒のうちで、結晶粒の内部に、少なくとも一つ以上のΣ３対応界面が存在する結晶粒の面積比率を求め、その値を表６に示した。
次に、従来被覆工具１〜１５の従来ＡｌＺｒＯ層についても、本発明被覆工具の場合と同様な方法により、従来ＡｌＺｒＯ層の測定範囲内に存在する全結晶粒のうちで、結晶粒の内部に、少なくとも一つ以上のΣ３対応界面が存在する結晶粒の面積比率を求め、その値を表７に示した。
Next, with respect to the modified AlZrO layer of the present invention-coated tools 1 to 15 and the conventional AlZrO layer of the conventional coated tools 1 to 15, the crystal grains having a Σ3-corresponding interface exist inside the crystal grains constituting the respective layers. The area ratio was measured.
First, the modified AlZrO layers of the above-described coated tools 1 to 15 of the present invention are set in a lens barrel of a field emission scanning electron microscope in a state where the surface is a polished surface, and the surface polished surface is set to 70 degrees. Electron backscattering is performed by irradiating an electron beam with an electron beam with an acceleration voltage of 15 kV at an incident angle with an irradiation current of 1 nA on each crystal grain having a hexagonal crystal lattice existing within the measurement range of each surface polished surface. Using a diffractive image apparatus, a 30 × 50 μm region is measured at an interval of 0.1 μm / step, and an angle at which each normal line of each crystal lattice plane of the crystal grain intersects with a normal line of the polished surface is measured. From the measurement results, the crystal orientation relationship between adjacent crystal lattices is calculated, and each constituent atom constituting the crystal lattice interface shares one constituent atom between the crystal lattices (constituent atom shared lattice point) Calculate the distribution of The number of lattice points that do not share constituent atoms between the constituent atomic shared lattice points is N (however, N is an even number of 2 or more on the crystal structure of the corundum hexagonal close-packed crystal. (When the upper limit is 28, there is no even number of 4, 8, 14, 24, and 26) When the existing configuration of the shared atom point is represented by ΣN + 1, it exists within the measurement range of the modified AlZrO layer. Among all the crystal grains, the area ratio of the crystal grains in which at least one Σ3-corresponding interface exists inside the crystal grains was determined, and the values are shown in Table 6.
Next, with respect to the conventional AlZrO layers of the conventional coated tools 1 to 15, by the same method as in the case of the coated tool of the present invention, among all the crystal grains existing within the measurement range of the conventional AlZrO layer, The area ratio of crystal grains in which at least one Σ3-corresponding interface exists was determined, and the values are shown in Table 7.
表６、７に示される通り、本発明被覆工具の改質ＡｌＺｒＯ層において、Σ３対応界面が存在する結晶粒の面積比率は、６０％以上であるのに対して、従来被覆工具の従来ＡｌＺｒＯ層において、Σ３対応界面が存在する結晶粒の面積比率は、４０％以下であって、結晶粒の内部にΣ３対応界面が存在する率は非常に小さいことがわかる。 As shown in Tables 6 and 7, in the modified AlZrO layer of the coated tool of the present invention, the area ratio of the crystal grains where the Σ3-corresponding interface exists is 60% or more, whereas the conventional AlZrO layer of the conventional coated tool , The area ratio of the crystal grains where the Σ3-corresponding interface is present is 40% or less, and it can be seen that the rate at which the Σ3-corresponding interface exists inside the crystal grain is very small.
さらに、本発明被覆工具１〜１５および従来被覆工具１〜１５の硬質被覆層の構成層の厚さを、走査型電子顕微鏡を用いて測定（縦断面測定）したところ、いずれも目標層厚と実質的に同じ平均層厚（５点測定の平均値）を示した。
また、本発明被覆工具１１〜１５の改質ＡｌＺｒＯ層については、電界放出型走査電子顕微鏡を用いて、層厚方向に垂直な面内に存在する、大粒径の平坦六角形状の結晶粒の面積割合を求め、この値を表６に示した。
なお、本発明で言う「大粒径の平坦六角形状」の結晶粒とは、「電界放出型走査電子顕微鏡により観察される層厚方向に垂直な面内に存在する粒子の直径を計測し、１０粒子の平均値が３〜８μｍであり、頂点の角度が１００〜１４０°である頂角を６個有する多角形状である。」
と定義する。
Furthermore, when the thicknesses of the constituent layers of the hard coating layers of the present coated tools 1 to 15 and the conventional coated tools 1 to 15 were measured using a scanning electron microscope (longitudinal cross section measurement), both of the target layer thicknesses and The substantially same average layer thickness (average value of 5-point measurement) was shown.
In addition, for the modified AlZrO layers of the coated tools 11 to 15 of the present invention, using a field emission scanning electron microscope, a large hexagonal crystal grain having a large grain size that exists in a plane perpendicular to the layer thickness direction is used. The area ratio was determined and this value is shown in Table 6.
In addition, the crystal grain of the “large hexagonal flat hexagonal shape” referred to in the present invention is “the diameter of particles existing in a plane perpendicular to the layer thickness direction observed by a field emission scanning electron microscope, It is a polygonal shape having 6 apex angles with an average value of 10 particles of 3 to 8 μm and an apex angle of 100 to 140 °. ”
It is defined as
つぎに、上記の本発明被覆工具１〜１５および従来被覆工具１〜１５の各種の被覆工具について、いずれも工具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、
[切削条件Ａ]
被削材：ＪＩＳ・Ｓ４５Ｃの丸棒、
切削速度： ４５０ ｍ／ｍｉｎ、
切り込み： ２．５ ｍｍ、
送り： ０．７ ｍｍ／ｒｅｖ、
切削時間： ８ 分、
の条件での炭素鋼の乾式高速高送り切削試験（通常の切削速度および送り量は、それぞれ、２５０ｍ／ｍｉｎ、０．３ｍｍ／ｒｅｖ）、
[切削条件Ｂ]
被削材：ＪＩＳ・ＳＣＭ４４０の丸棒、
切削速度： ３２０ ｍ／ｍｉｎ、
切り込み： ２．２ ｍｍ、
送り： ０．３ ｍｍ／ｒｅｖ、
切削時間： ５ 分、
の条件でのクロムモリブデン合金鋼の乾式高速高切込み切削試験（通常の切削速度および切込み量は、それぞれ、２５０ｍ／ｍｉｎ、１．５ｍｍ）、
[切削条件Ｃ]
被削材：ＪＩＳ・ＦＣ３００の丸棒、
切削速度： ５４５ ｍ／ｍｉｎ、
切り込み： ５．６ ｍｍ、
送り： ０．６ ｍｍ／ｒｅｖ、
切削時間： ５ 分、
の条件での鋳鉄の湿式高速高切込み切削試験（通常の切削速度および切込み量は、それぞれ、３５０ｍ／ｍｉｎ、２．５ｍｍ）、
を行い、いずれの切削試験でも切刃の逃げ面摩耗幅を測定した。この測定結果を表８に示した。
Next, for the various coated tools of the present invention coated tools 1-15 and the conventional coated tools 1-15, all of them are screwed to the tip of the tool steel tool with a fixing jig,
[Cutting conditions A]
Work material: JIS / S45C round bar,
Cutting speed: 450 m / min,
Cutting depth: 2.5 mm,
Feed: 0.7 mm / rev,
Cutting time: 8 minutes,
Carbon steel dry high-speed high-feed cutting test under normal conditions (normal cutting speed and feed amount are 250 m / min and 0.3 mm / rev, respectively)
[Cutting conditions B]
Work material: JIS / SCM440 round bar,
Cutting speed: 320 m / min,
Cutting depth: 2.2 mm,
Feed: 0.3 mm / rev,
Cutting time: 5 minutes,
Dry high-speed high-cut cutting test of chrome-molybdenum alloy steel under the conditions (normal cutting speed and cutting depth are 250 m / min and 1.5 mm, respectively)
[Cutting conditions C]
Work material: JIS / FC300 round bar,
Cutting speed: 545 m / min,
Incision: 5.6 mm,
Feed: 0.6 mm / rev,
Cutting time: 5 minutes,
Wet high-speed high-cutting cutting test of cast iron under the conditions (normal cutting speed and cutting depth are 350 m / min and 2.5 mm, respectively)
In each cutting test, the flank wear width of the cutting edge was measured. The measurement results are shown in Table 8.
表６〜８に示される結果から、この発明の被覆工具は、上部層を構成するＺｒを含有する酸化アルミニウム層（改質ＡｌＺｒＯ層）が、平板多角形（平坦六角形）たて長形状の結晶粒の組織構造として構成し、さらに、結晶粒の内部に少なくとも一つ以上のΣ３対応界面が存在する結晶粒の面積比率が高いことにより、従来被覆工具の従来ＡｌＺｒＯ層のもつ高温硬さ、高温強度、耐熱性に加えて、一段とすぐれた表面平坦性と一段とすぐれた高温強度を兼備し、その結果、各種の鋼や鋳鉄などを、高い発熱を伴い切刃部に高負荷が作用する高速重切削条件の切削加工で用いた場合にも、硬質被覆層がすぐれた耐チッピング性、耐欠損性、耐剥離性と一段とすぐれた耐摩耗性を発揮し、使用寿命の一層の延命化を可能とするものであるのに対して、硬質被覆層の上部層として従来ＡｌＺｒＯ層が蒸着形成された従来被覆工具１〜１５においては、高速重切削条件下では、高温強度が不十分であるとともに摩耗が促進されやすく、その結果、比較的短時間で使用寿命に至ることが明らかである。 From the results shown in Tables 6 to 8, in the coated tool of the present invention, the aluminum oxide layer (modified AlZrO layer) containing Zr constituting the upper layer is a flat plate polygon (flat hexagonal) vertically long shape. The high-temperature hardness of the conventional AlZrO layer of the conventional coated tool is configured as a structure structure of crystal grains, and further, the area ratio of the crystal grains in which at least one Σ3-compatible interface exists inside the crystal grains is high, In addition to high-temperature strength and heat resistance, it has excellent surface flatness and excellent high-temperature strength. As a result, various types of steel, cast iron, etc. have high heat generation and a high load acts on the cutting edge. Even when used in heavy cutting conditions, the hard coating layer exhibits excellent chipping resistance, chipping resistance, and peeling resistance, as well as excellent wear resistance, further extending the service life. Vs. In the conventional coated tools 1 to 15 in which the conventional AlZrO layer is vapor-deposited as the upper layer of the hard coating layer, under high speed heavy cutting conditions, the high temperature strength is insufficient and the wear tends to be promoted. It is clear that the service life is reached in a relatively short time.
上述のように、この発明の被覆工具は、各種の鋼や鋳鉄などの通常の条件での切削加工は勿論のこと、特に高い発熱を伴うとともに切刃部に対して高負荷が作用する高速重切削加工でも硬質被覆層がすぐれた耐チッピング性、耐欠損性、耐剥離性と一段とすぐれた耐摩耗性を示し、長期に亘ってすぐ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満足に対応できるものである。 As described above, the coated tool of the present invention is not only used for cutting under normal conditions such as various types of steel and cast iron, but also has a particularly high speed with high heat generation and high load acting on the cutting edge. Even in cutting, the hard coating layer exhibits excellent chipping resistance, chipping resistance, peeling resistance and excellent wear resistance, and exhibits excellent cutting performance over a long period of time. It can fully satisfy the performance, labor saving and energy saving of cutting, and cost reduction.
Claims (2)
（ａ）下部層が、３〜２０μｍの全体平均層厚を有する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層以上からなるＴｉ化合物層、
（ｂ）上部層が、２〜１５μｍの平均層厚を有し、かつ、α型の結晶構造を有しＺｒを含有する酸化アルミニウム層、
上記（ａ）、（ｂ）からなる硬質被覆層を蒸着形成した表面被覆切削工具において、
上記上部層を、電界放出型走査電子顕微鏡で組織観察した場合に、層厚方向に垂直な面内で平板多角形状、また、層厚方向に平行な面内で層厚方向にたて長形状を有する結晶粒からなる組織構造を有し、さらに、
該上部層について、電界放出型走査電子顕微鏡と電子後方散乱回折像装置を用い、表面研磨面の測定範囲内に存在する結晶粒個々に電子線を照射して、六方晶結晶格子からなる結晶格子面のそれぞれの法線が前記表面研磨面の法線と交わる角度を測定し、
この測定結果から、隣接する結晶格子相互の結晶方位関係を算出し、結晶格子界面を構成する構成原子のそれぞれが前記結晶格子相互間で１つの構成原子を共有する格子点（構成原子共有格子点）の分布を算出し、前記構成原子共有格子点間に構成原子を共有しない格子点がＮ個（但し、Ｎはコランダム型六方最密晶の結晶構造上２以上の偶数となるが、分布頻度の点からＮの上限を２８とした場合、４、８、１４、２４および２６の偶数は存在せず）存在する構成原子共有格子点形態をΣＮ＋１で表した場合に、
上記上部層を構成する結晶粒の内、面積比率で６０％以上の結晶粒の内部は、少なくとも一つ以上の、Σ３で表される構成原子共有格子点形態からなる結晶格子界面により分断されていることを特徴とする表面被覆切削工具。 On the surface of the tool base composed of tungsten carbide based cemented carbide or titanium carbonitride based cermet,
(A) The lower layer is one or more of Ti carbide layer, nitride layer, carbonitride layer, carbonate layer, and carbonitride oxide layer having an overall average layer thickness of 3 to 20 μm. A Ti compound layer comprising:
(B) The upper layer has an average layer thickness of 2 to 15 μm, and has an α-type crystal structure and contains Zr,
In the surface-coated cutting tool in which the hard coating layer composed of the above (a) and (b) is formed by vapor deposition,
When the upper layer is observed with a field emission scanning electron microscope, the polygonal shape is flat in a plane perpendicular to the layer thickness direction, and is long in the layer thickness direction in a plane parallel to the layer thickness direction. Having a texture structure composed of crystal grains having,
A crystal lattice comprising a hexagonal crystal lattice is formed on the upper layer by using a field emission scanning electron microscope and an electron backscatter diffraction image apparatus to irradiate each crystal grain existing within the measurement range of the surface polished surface with an electron beam. Measure the angle at which each normal of the surface intersects the normal of the surface polished surface,
From this measurement result, the crystal orientation relationship between adjacent crystal lattices is calculated, and each of the constituent atoms constituting the crystal lattice interface shares one constituent atom between the crystal lattices (constituent atom shared lattice point). ) And the number of lattice points that do not share constituent atoms between the constituent atomic shared lattice points (where N is an even number of 2 or more on the crystal structure of the corundum hexagonal close-packed crystal, but the distribution frequency) In the case where the upper limit of N is 28 from this point, even numbers of 4, 8, 14, 24 and 26 do not exist)
Among the crystal grains constituting the upper layer, the interior of the crystal grains having an area ratio of 60% or more is divided by at least one crystal lattice interface composed of a constituent atomic shared lattice point represented by Σ3. A surface-coated cutting tool characterized by comprising:
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| EP08172909A EP2085500B1 (en) | 2007-12-28 | 2008-12-24 | Surface-coated cutting tool with hard coating layer having excellent abrasion resistance |
| ES08172909T ES2402166T3 (en) | 2007-12-28 | 2008-12-24 | Hard surface coated tool with hard coating layer that has excellent abrasion resistance |
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| JP5594570B2 (en) * | 2010-01-27 | 2014-09-24 | 三菱マテリアル株式会社 | Surface coated cutting tool with excellent chipping resistance due to hard coating layer |
| JP5594572B2 (en) * | 2010-01-27 | 2014-09-24 | 三菱マテリアル株式会社 | Surface-coated cutting tool with excellent peel resistance, chipping resistance, and wear resistance with excellent hard coating layer |
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| JP5594574B2 (en) * | 2010-02-16 | 2014-09-24 | 三菱マテリアル株式会社 | Surface-coated cutting tool with excellent peeling resistance and wear resistance due to its hard coating layer |
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