JP4529638B2 - Cutting tool made of surface-coated cemented carbide that provides excellent chipping resistance with a hard coating layer in high-speed heavy cutting - Google Patents
Cutting tool made of surface-coated cemented carbide that provides excellent chipping resistance with a hard coating layer in high-speed heavy cutting Download PDFInfo
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この発明は、特に各種の鋼や鋳鉄などの高速重切削加工で、硬質被覆層がすぐれた耐チッピング性を発揮する表面被覆超硬合金製切削工具（以下、被覆超硬工具という）に関するものである。 The present invention relates to a surface-coated cemented carbide cutting tool (hereinafter referred to as a coated cemented carbide tool) that exhibits excellent chipping resistance with a hard coating layer, particularly in high-speed heavy cutting of various steels and cast iron. is there.
従来、一般に、被覆超硬工具として、炭化タングステン（以下、ＷＣで示す）基超硬合金で構成された工具基体の表面に、いずれも化学蒸着形成した状態で、
（ａ）下部層として、いずれも粒状結晶組織を有するＴｉの炭化物（以下、ＴｉＣで示す）層、窒化物（以下、同じくＴｉＮで示す）層、炭窒化物（以下、ＴｉＣＮで示す）層、炭酸化物（以下、ＴｉＣＯで示す）層、および炭窒酸化物（以下、ＴｉＣＮＯで示す）層のうちの１層または２層以上からなり、かつ３〜２０μｍの全体平均層厚を有するＴｉ化合物層、
（ｂ）上部層として、α型の結晶構造および粒状結晶組織を有し、かつ１〜２０μｍの平均層厚を有する酸化アルミニウム層（以下、従来α型Ａｌ2Ｏ3層という示す）、
以上の下部層および上部層で構成された硬質被覆層を蒸着形成してなる、被覆超硬工具が知られており、この被覆超硬工具が、例えば各種の鋼や鋳鉄などの連続切削加工や断続切削加工に用いられてことも良く知られるところである。
Conventionally, generally, as a coated carbide tool, on the surface of a tool base made of tungsten carbide (hereinafter referred to as WC) -based cemented carbide, both are formed by chemical vapor deposition.
(A) As a lower layer, Ti carbide (hereinafter referred to as TiC) layer, nitride (hereinafter also referred to as TiN) layer, carbonitride (hereinafter referred to as TiCN) layer each having a granular crystal structure, Ti compound layer composed of one or more of a carbon oxide (hereinafter referred to as TiCO) layer and a carbonitride oxide (hereinafter referred to as TiCNO) layer and having an overall average layer thickness of 3 to 20 μm ,
(B) As an upper layer, an aluminum oxide layer having an α-type crystal structure and a granular crystal structure and an average layer thickness of 1 to 20 μm (hereinafter referred to as a conventional α-type Al 2 O 3 layer),
A coated carbide tool formed by vapor-depositing a hard coating layer composed of the above lower layer and upper layer is known, and this coated carbide tool can be used for continuous cutting such as various types of steel and cast iron. It is also well known that it is used for intermittent cutting.
また、一般に、上記の被覆超硬工具の硬質被覆層を構成するＴｉ化合物層のうちのＴｉＣＮ層として、層自身の強靭化を目的として、通常の化学蒸着装置にて、反応ガスとして有機炭窒化物を含む混合ガスを使用し、７００〜９５０℃の中温温度域で蒸着形成して縦長成長結晶組織をもつようにしたＴｉＣＮ層（以下、ｌ−ＴｉＣＮ層で示す）も知られている。
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、切削加工は一段と高速化の傾向にあるほか、高切り込みや高送りなどの重切削加工条件での切削加工を余儀なくされる状況にあるが、上記の従来被覆超硬工具においては、これを鋼や鋳鉄などの通常の条件での切削加工に用いた場合には問題はないが、特にこれを切削条件の厳しい高速重切削加工、すなわち高温加熱下で切刃部にきわめて高い荷重のかかる高速重切削加工に用いた場合、硬質被覆層を構成する従来α型Ａｌ2Ｏ3層は、高い高温硬さおよびすぐれた耐熱性を備えるものの、十分な高温強度を具備するものでないために、前記従来α型Ａｌ2Ｏ3層が原因で硬質被覆層にはチッピング（微小欠け）が発生し易くなり、この結果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 equipment has been remarkable. On the other hand, there is a strong demand for labor saving and energy saving and further cost reduction for cutting work. Although it is inevitable to perform cutting under heavy cutting conditions such as high feed, the above conventional coated carbide tools are used for cutting under normal conditions such as steel and cast iron. There is no problem, but especially when this is used for high-speed heavy cutting with severe cutting conditions, that is, high-speed heavy cutting with a very high load on the cutting edge under high temperature heating, the conventional α type that constitutes a hard coating layer Although the Al 2 O 3 layer has high high-temperature hardness and excellent heat resistance, it does not have sufficient high-temperature strength, so the conventional α-type Al 2 O 3 layer is used to chip the hard coating layer. (Fine Only) are easily generated, the reach this result relatively short time service life at present.
そこで、本発明者等は、上述のような観点から、高速重切削加工で硬質被覆層がすぐれた耐チッピング性を発揮する被覆超硬工具を開発すべく研究を行った結果、
（ａ）上記の従来被覆超硬工具の硬質被覆層を構成するＴｉ化合物層のうち、特に工具基体表面に対する密着接合性のすぐれたＴｉＮ層とＴｉＣＮ層、さらに強靭性を有するｌ−ＴｉＣＮ層を特定すると共に、上記従来α型Ａｌ2Ｏ3層の形成に先だって、まず、前記ｌ−ＴｉＣＮ層の表面に、通常の条件で、０．１〜１μｍの平均層厚でＴｉＣＮ層を形成し、これに、窒化雰囲気処理、望ましくは圧力：２０〜４０ｋＰａの窒素雰囲気中、９５０〜１１００℃の温度に、１０〜６０分間保持の条件で窒化雰囲気処理を施し、さらに引き続いて酸化雰囲気処理、望ましくはガス組成が、容量％で、ＣＯ２：５〜１０％，ＣＯ：５〜１０％，Ｈ２：残りからなる、圧力：５〜１０ｋＰａの酸化雰囲気中、９５０〜１１００℃の温度に、３〜１０分間保持の条件で酸化雰囲気処理を施して、これを履歴核ＴｉＣＮ層とし、ついで、前記履歴核ＴｉＣＮ層の上に、通常の条件、すなわち従来α型Ａｌ2Ｏ3層の形成条件と同じ条件でα型Ａｌ2Ｏ3層を形成すると、形成時の前記α型Ａｌ2Ｏ3層は、前記履歴核ＴｉＣＮ層の結晶配列に著しく影響を受け、これを十分に履歴するようになり、しかもこの結果形成されたα型Ａｌ2Ｏ3層（以下、履歴α型Ａｌ2Ｏ3層という）は、α型Ａｌ2Ｏ3層自身が具備するすぐれた高温硬さおよび耐熱性を損なうことなく、上記の従来α型Ａｌ2Ｏ3層に比して、一段とすぐれた高温強度を具備するようになるので、硬質被覆層が上記のＴｉＮ層およびＴｉＣＮ層のいずれか、またはこれら両層の積層からなる密着接合層、前記ｌ−ＴｉＣＮ層の強靭層、および前記履歴α型Ａｌ2Ｏ3層の強化硬質層からなる被覆超硬工具は、前記硬質被覆層が前記強靭層と強化硬質層の共存作用で、すぐれた高温強度を有するようになることから、特に高温加熱下で切刃部にきわめて高い荷重のかかる高速重切削加工でも、前記硬質被覆層がすぐれた耐チッピング性を発揮し、長期に亘ってすぐれた耐摩耗性を示すようになること。
Therefore, the present inventors, from the above viewpoint, as a result of conducting research to develop a coated carbide tool that exhibits excellent chipping resistance with a hard coating layer in high-speed heavy cutting,
(A) Among the Ti compound layers constituting the hard coating layer of the above-mentioned conventional coated carbide tool, a TiN layer and a TiCN layer excellent in tight adhesion particularly to the surface of the tool substrate, and further a 1-TiCN layer having toughness Prior to the formation of the conventional α-type Al 2 O 3 layer, a TiCN layer is first formed on the surface of the l-TiCN layer with an average layer thickness of 0.1 to 1 μm under normal conditions. This is subjected to a nitriding atmosphere treatment, preferably a pressure: 20 to 40 kPa in a nitrogen atmosphere at a temperature of 950 to 1100 ° C. under a condition of holding for 10 to 60 minutes, followed by an oxidizing atmosphere treatment, preferably gas composition, by volume%, CO 2: 5~10%, CO: 5~10%, H 2: consisting of the remaining pressure: in an oxidizing atmosphere of 5～10KPa, to a temperature of from 950 to 1100 ° C.,. 3 to 10 Oxidation atmosphere treatment is performed under the condition of holding for a minute to make this a history nucleus TiCN layer, and then on the history nucleus TiCN layer, the normal conditions, that is, the same conditions as the formation conditions of the conventional α-type Al 2 O 3 layer When the α-type Al 2 O 3 layer is formed by the above method, the α-type Al 2 O 3 layer at the time of formation is significantly affected by the crystal arrangement of the hysteresis nucleus TiCN layer, and this history is sufficiently recorded. The resulting α-type Al 2 O 3 layer (hereinafter referred to as the history α-type Al 2 O 3 layer) does not impair the excellent high-temperature hardness and heat resistance of the α-type Al 2 O 3 layer itself. As compared with the conventional α-type Al 2 O 3 layer, the hard coating layer is one of the TiN layer and the TiCN layer, or a laminate of these two layers. An adhesive bonding layer comprising: a tough layer of the l-TiCN layer; Coated cemented carbide tool consisting of reinforced rigid layer of the preliminary the history α-type Al 2 O 3 layer with coexistence effect of the hard layer is the tough layer with the reinforcing hard layer, since it will have excellent high-temperature strength In particular, the hard coating layer exhibits excellent chipping resistance even during high-speed heavy cutting where a very high load is applied to the cutting edge part under high temperature heating, and it will show excellent wear resistance over a long period of time. .
（ｂ）上記（ａ）の履歴α型Ａｌ2Ｏ3層および従来α型Ａｌ2Ｏ3層について、電界放出型走査電子顕微鏡を用い、図１（ａ），（ｂ）に概略説明図で示される通り、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Ａｌ2Ｏ3結晶粒個々に電子線を照射して、前記表面研磨面の法線に対して、前記結晶粒の結晶面である（０００１）面の法線がなす傾斜角を測定し、前記測定傾斜角のうち、０〜４５度の範囲内にある測定傾斜角を０．２５度のピッチ毎に区分すると共に、各区分内に存在する度数を集計してなる傾斜角度数分布グラフを作成した場合、前記従来α型Ａｌ2Ｏ3層は、図３に例示される通り、（０００１）面の測定傾斜角の分布が０〜４５度の範囲内で不偏的な傾斜角度数分布グラフを示すのに対して、前記履歴α型Ａｌ2Ｏ3層は、図２に例示される通り、傾斜角区分の特定位置に少なくとも２つのシャープなピークが現れ、このシャープなピークは、グラフ横軸の傾斜角区分に現れる位置および高さが上記履歴核ＴｉＣＮ層の形成に際しての窒化雰囲気処理条件および酸化雰囲気処理条件によって変化すること。 (B) The history α-type Al 2 O 3 layer and the conventional α-type Al 2 O 3 layer of (a) are schematically illustrated in FIGS. 1A and 1B using a field emission scanning electron microscope. as shown, by irradiating an electron beam to the Al 2 O 3 crystal grains each having a hexagonal crystal lattice present within the measuring range of the surface polishing plane, with respect to the normal of the surface polishing plane, the crystal grains The inclination angle formed by the normal line of the (0001) plane which is the crystal plane is measured, and among the measurement inclination angles, the measurement inclination angles within the range of 0 to 45 degrees are classified for each pitch of 0.25 degrees. In the case of creating an inclination angle number distribution graph obtained by counting the frequencies existing in each section, the conventional α-type Al 2 O 3 layer has a measured inclination angle on the (0001) plane as illustrated in FIG. In contrast to the distribution of the inclination angle number distribution graph in the range of 0 to 45 degrees, the history α type In the Al 2 O 3 layer, as illustrated in FIG. 2, at least two sharp peaks appear at specific positions in the tilt angle section, and these sharp peaks are positions and heights that appear in the tilt angle section on the horizontal axis of the graph. Varies depending on the nitriding atmosphere processing conditions and the oxidizing atmosphere processing conditions in forming the history nucleus TiCN layer.
（ｃ）上記履歴核ＴｉＣＮ層の形成に際して、窒化雰囲気処理および酸化雰囲気処理を上記の通りの条件で行うと、前記履歴α型Ａｌ2Ｏ3層の傾斜角度数分布グラフで、１番高いピークが傾斜角区分の７〜１５度の範囲内に、ついで２番目に高いピークが０〜７度の範囲内に現れ、かつ、傾斜角度数分布グラフにおける度数全体に占める割合で、前記７〜１５度の範囲内に存在する度数の合計が３５〜５０％、前記０〜７度の範囲内に存在する度数の合計が２５〜４０％、である傾斜角度数分布グラフを示すようになり、したがって、上記の条件で窒化雰囲気処理および酸化雰囲気処理のいずれかを行わなかったり、前記処理の条件が上記の条件から外れたりすると、傾斜角度数分布グラフにおいて、ピークが現れる傾斜角区分および前記傾斜角区分に占める度数割合が前記した範囲から外れるようになり、この場合は高温強度に所望の向上効果が得られないこと。
以上（ａ）〜（ｃ）に示される研究結果を得たのである。
(C) When the history nucleus TiCN layer is formed, if the nitriding atmosphere treatment and the oxidation atmosphere treatment are performed under the conditions as described above, the highest peak in the gradient angle distribution graph of the history α-type Al 2 O 3 layer In the range of 7 to 15 degrees of the tilt angle section, and then the second highest peak appears in the range of 0 to 7 degrees, and the ratio of the total frequency in the tilt angle number distribution graph is 7 to 15 The inclination angle frequency distribution graph in which the total of the frequencies existing in the range of degrees is 35 to 50% and the total of the frequencies existing in the range of 0 to 7 degrees is 25 to 40%, and therefore If either the nitriding atmosphere treatment or the oxidizing atmosphere treatment is not performed under the above conditions, or if the treatment conditions deviate from the above conditions, the slope angle distribution graph in which the peak appears in the slope angle distribution graph and the slope The frequency ratio occupying the beveled section is out of the above-mentioned range, and in this case, the desired improvement effect on the high-temperature strength cannot be obtained.
The research results shown in (a) to (c) above were obtained.
この発明は、上記の研究結果に基づいてなされたものであって、ＷＣ基超硬合金で構成された工具基体の表面に、いずれも化学蒸着形成した状態で、
（ａ）第１層として、ＴｉＮ層およびＴｉＣＮ層のうちのいずれか、またはこれら両層の積層からなり、かつ０．１〜１μｍの平均層厚を有する密着接合層、
（ｂ）第２層として、ｌ−ＴｉＣＮ層からなり、かつ３〜１５μｍの平均層厚を有する強靭層、
（ｃ）第３層として、電界放出型走査電子顕微鏡を用い、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、前記表面研磨面の法線に対して、前記結晶粒の結晶面である（０００１）面の法線がなす傾斜角を測定し、前記測定傾斜角のうち、０〜４５度の範囲内にある測定傾斜角を０．２５度のピッチ毎に区分すると共に、各区分内に存在する度数を集計してなる傾斜角度数分布グラフにおいて、少なくとも７〜１５度の範囲内の傾斜角区分および０〜７度の範囲内の傾斜角区分にピークが存在すると共に、傾斜角度数分布グラフにおける度数全体に占める割合で、前記７〜１５度の範囲内に存在する度数の合計が３５〜５０％、前記０〜７度の範囲内に存在する度数の合計が２５〜４０％、である傾斜角度数分布グラフを示す履歴α型Ａｌ2Ｏ3層からなり、かつ３〜１５μｍの平均層厚を有する強化硬質層、
以上第１層〜第３層で構成された硬質被覆層を蒸着形成してなる、高速重切削加工で硬質被覆層がすぐれた耐チッピング性を発揮する被覆超硬工具に特徴を有するものである。
This invention was made based on the above research results, and in a state where both are formed by chemical vapor deposition on the surface of a tool base made of a WC-based cemented carbide.
(A) As a first layer, a TiJ layer and a TiCN layer, or a close contact bonding layer having an average layer thickness of 0.1 to 1 μm, comprising a laminate of both layers,
(B) As a second layer, a tough layer comprising an l-TiCN layer and having an average layer thickness of 3 to 15 μm,
(C) Using a field emission scanning electron microscope as the third layer, irradiating each crystal grain having a hexagonal crystal lattice existing within the measurement range of the surface polished surface with an electron beam, The inclination angle formed by the normal line of the (0001) plane, which is the crystal plane of the crystal grain, is measured with respect to the line, and the measured inclination angle within the range of 0 to 45 degrees is set to 0. In an inclination angle distribution graph obtained by dividing the pitch every 25 degrees and counting the frequencies existing in each section, the inclination angle section in the range of at least 7 to 15 degrees and the range of 0 to 7 degrees A peak is present in the tilt angle section, and the ratio of the total frequency in the range of 7 to 15 degrees is 35 to 50% in the ratio of the entire frequency in the tilt angle distribution graph, and the range of 0 to 7 degrees. The total frequency present in the range is 25-40% Consists historical α type the Al 2 O 3 layer that shows an oblique angle frequency distribution graph, and reinforcing hard layer having an average layer thickness of 3 to 15 [mu] m,
As described above, it is characterized by a coated carbide tool that exhibits excellent chipping resistance by high-speed heavy cutting, which is formed by vapor-depositing a hard coating layer composed of the first to third layers. .
つぎに、この発明の被覆超硬工具の硬質被覆層の構成層について、上記の通りに数値限定した理由を以下に説明する。
（ａ）ＴｉＮ層およびＴｉＣＮ層（密着接合層）
ＴｉＮ層およびＴｉＣＮ層は、強靭層であるｌ−ＴｉＣＮ層は勿論のこと、特に工具基体との密着接合性にすぐれ、これによって硬質被覆層の工具基体に対する密着接合性が向上したものになるが、その平均層厚が０．１μｍ未満では、所望のすぐれた密着接合性を確保することができず、一方所望の密着接合性は１μｍまでの平均層厚で十分確保することができることから、その平均層厚を０．１〜１μｍと定めた。
Next, the reason why the constituent layers of the hard coating layer of the coated carbide tool of the present invention are numerically limited as described above will be described below.
(A) TiN layer and TiCN layer (adhesion bonding layer)
The TiN layer and the TiCN layer are excellent in the tight bondability to the tool substrate, not to mention the l-TiCN layer, which is a tough layer, and this improves the tight bondability of the hard coating layer to the tool substrate. If the average layer thickness is less than 0.1 μm, it is impossible to ensure the desired excellent adhesive bondability, while the desired adhesive bondability can be sufficiently ensured with an average layer thickness of up to 1 μm. The average layer thickness was determined to be 0.1-1 μm.
（ｂ）ｌ−ＴｉＣＮ層（強靭層）
ｌ−ＴｉＣＮ層は、上記の通り縦長成長結晶組織を有し、これによってすぐれた強靭性を具備するようになることから、高速重切削加工での熱的機械的衝撃に対してすぐれた耐チッピング性を発揮するが、その平均層厚が３μｍ未満では、所望のすぐれた耐チッピング性を確保することができず、一方その平均層厚が１５μｍを越えると、高熱発生を伴なう高速重切削加工では、切刃部に偏摩耗の原因となる熱塑性変形が発生し易くなることから、その平均層厚を３〜１５μｍと定めた。
(B) l-TiCN layer (tough layer)
Since the l-TiCN layer has a vertically grown crystal structure as described above and thereby has excellent toughness, it has excellent chipping resistance against thermal mechanical shock in high-speed heavy cutting. However, if the average layer thickness is less than 3 μm, the desired excellent chipping resistance cannot be ensured. On the other hand, if the average layer thickness exceeds 15 μm, high-speed heavy cutting with high heat generation occurs. In processing, since the thermoplastic deformation that causes uneven wear tends to occur in the cutting edge portion, the average layer thickness is set to 3 to 15 μm.
（ｃ）履歴α型Ａｌ2Ｏ3層（強化硬質層）
履歴α型Ａｌ2Ｏ3層は、傾斜角度数分布グラフで、１番高いピークが傾斜角区分の７〜１５度、そして２番目に高いピークが０〜７度のそれぞれの範囲内に現れ、かつ傾斜角度数分布グラフにおける度数全体に占める割合で、前記７〜１５度の範囲内に存在する度数の合計が３５〜５０％、前記０〜７度の範囲内に存在する度数の合計が２５〜４０％、である傾斜角度数分布グラフを示し、この結果すぐれた高温強度を具備し、耐チッピング性の向上が図られるようになるものであり、さらにＡｌ2Ｏ3層自身のもつすぐれた高温硬さと耐熱性によって、硬質被覆層の耐摩耗性向上に寄与するが、その平均層厚が３μｍ未満では、硬質被覆層に十分な耐摩耗性を付与することができず、一方その平均層厚が１５μｍを越えて厚くなりすぎると、高速重切削加工ではチッピングが発生し易くなることから、その平均層厚を３〜１５μｍと定めた。
(C) Hysteresis α-type Al 2 O 3 layer (reinforced hard layer)
The history α-type Al 2 O 3 layer is an inclination angle number distribution graph, in which the highest peak appears in the range of 7 to 15 degrees of the inclination angle section, and the second highest peak in the range of 0 to 7 degrees, In addition, the ratio of the frequencies existing in the range of 7 to 15 degrees is 35 to 50% and the total number of frequencies existing in the range of 0 to 7 degrees is 25 as a ratio of the entire frequencies in the inclination angle frequency distribution graph. An inclination angle number distribution graph of ˜40% is shown, and as a result, it has excellent high-temperature strength, and can improve chipping resistance, and the Al 2 O 3 layer itself is tangled. High temperature hardness and heat resistance contribute to improving the wear resistance of the hard coating layer. However, if the average layer thickness is less than 3 μm, sufficient wear resistance cannot be imparted to the hard coating layer. If the thickness exceeds 15 μm and becomes too thick, Since high-speed heavy cutting tends to cause chipping, the average layer thickness is determined to be 3 to 15 μm.
この発明の被覆超硬工具は、上記の従来被覆超硬工具の硬質被覆層を構成するＴｉ化合物層を密着接合性にすぐれたＴｉＮ層およびＴｉＣＮ層と、強靭性を有するｌ−ＴｉＣＮ層に特定し、かつ同α型Ａｌ2Ｏ3層を上記のすぐれた高温強度を有する履歴α型Ａｌ2Ｏ3層で構成することにより、特に高温加熱下で切刃部にきわめて高い荷重のかかる鋼や鋳鉄などの高速重切削加工でも、チッピング発生なく、長期に亘ってすぐれた耐摩耗性を発揮するようにしたものである。 In the coated carbide tool of the present invention, the Ti compound layer constituting the hard coating layer of the above-described conventional coated carbide tool is specified as a TiN layer and a TiCN layer excellent in tight bonding and a tough l-TiCN layer. In addition, the α-type Al 2 O 3 layer is composed of the above-mentioned hysteretic α-type Al 2 O 3 layer having excellent high-temperature strength. Even in high-speed heavy cutting such as cast iron, chipping does not occur and excellent wear resistance is exhibited over a long period of time.
つぎに、この発明の被覆超硬工具を実施例により具体的に説明する。 Next, the coated carbide tool of the present invention will be specifically described with reference to examples.
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、ＶＣ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・ＣＮＭＧ１２０４０８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〜Ｆをそれぞれ製造した。 As raw material powders, WC powder, TiC powder, ZrC powder, VC powder, TaC powder, NbC powder, Cr 3 C 2 powder, TiN powder, and Co powder each having an average particle diameter of 1 to 3 μm are prepared. The raw material powder is blended in the blending composition shown in Table 1, added with wax, ball mill mixed in acetone for 24 hours, dried under reduced pressure, and press-molded into a green compact of a predetermined shape at a pressure of 98 MPa. The green compact is vacuum-sintered in a vacuum of 5 Pa at a predetermined temperature within a range of 1370 to 1470 ° C. for 1 hour. After sintering, the cutting edge is subjected to a honing process of R: 0.07 mm. Thus, tool bases A to F made of a WC-based cemented carbide having a throwaway tip shape specified in ISO · CNMG120408 were manufactured.
つぎに、これらの工具基体Ａ〜Ｆのそれぞれの表面に、通常の化学蒸着装置を用い、表２に示される条件にて（表２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を有する構成層の形成条件を示すものである。）、硬質被覆層の密着接合層（ＴｉＮ層、ＴｉＣＮ層）および強靭層（ｌ−ＴｉＣＮ層）を表３に示される目標層厚で蒸着形成し、ついで、まず、ＴｉＣＮ層を表２に示される条件で、かつ表３に示される目標層厚で蒸着形成した後、これに、
（ａ）圧力：２５ｋＰａの窒素雰囲気中、１０００℃の温度に、１０〜６０分間保持の条件での窒化雰囲気処理を施し、
（ｂ）引き続いてガス組成が、容量％で、ＣＯ２：７％，ＣＯ：７％，Ｈ２：残りからなる、圧力：７ｋＰａの酸化雰囲気中、１０００℃の温度に、３〜１０分間保持の条件での酸化雰囲気処理を施して、
履歴核ＴｉＣＮ層とし、この状態で同じく表２に示される従来α型Ａｌ2Ｏ3層の形成条件と同じ条件で、同じく表３に示される目標層厚でα型Ａｌ2Ｏ3層を蒸着形成して、これを履歴α型Ａｌ2Ｏ3層（強化硬質層）とすることにより本発明被覆超硬工具１〜６をそれぞれ製造した。
Next, a normal chemical vapor deposition apparatus is used on each surface of these tool bases A to F under the conditions shown in Table 2 (l-TiCN in Table 2 is described in JP-A-6-8010). The conditions for forming a TiCN layer having a vertically elongated crystal structure are shown, and the other conditions are the conditions for forming a constituent layer having a normal granular crystal structure.), An adhesive bonding layer of a hard coating layer ( TiN layer, TiCN layer) and tough layer (1-TiCN layer) are formed by vapor deposition at the target layer thickness shown in Table 3, and then the TiCN layer is first formed under the conditions shown in Table 2 and shown in Table 3. After vapor deposition with the target layer thickness,
(A) Pressure: In a nitrogen atmosphere of 25 kPa, a nitriding atmosphere treatment is performed at a temperature of 1000 ° C. for 10 to 60 minutes.
(B) Subsequently, the gas composition is in volume%, CO 2 : 7%, CO: 7%, H 2 : remaining, pressure: held in an oxidizing atmosphere of 7 kPa at a temperature of 1000 ° C. for 3 to 10 minutes. Applying an oxidizing atmosphere treatment under the conditions of
A history nucleus TiCN layer, also under the same conditions as the conditions for forming the conventional α type the Al 2 O 3 layer as shown in Table 2, similarly deposited α-type in the target layer thickness the Al 2 O 3 layer shown in Table 3 in this condition Formed and made into a history α-type Al 2 O 3 layer (reinforced hard layer), the coated carbide tools 1 to 6 of the present invention were manufactured.
また、比較の目的で、表３に示される通り、履歴核ＴｉＣＮ層の形成を行わない以外は同一の条件で密着接合層（ＴｉＮ層、ＴｉＣＮ層）、強靭層（ｌ−ＴｉＣＮ層）、および硬質層（従来α型Ａｌ2Ｏ3層）を形成することにより比較被覆超硬工具１〜６をそれぞれ製造した。 For the purpose of comparison, as shown in Table 3, an adhesion bonding layer (TiN layer, TiCN layer), a tough layer (1-TiCN layer), and a tough layer under the same conditions except that the history nucleus TiCN layer is not formed, and Comparative coated carbide tools 1 to 6 were produced by forming a hard layer (conventional α-type Al 2 O 3 layer), respectively.
ついで、上記の本発明被覆超硬工具と比較被覆超硬工具の硬質被覆層を構成する履歴α型Ａｌ2Ｏ3層および従来α型Ａｌ2Ｏ3層について、電界放出型走査電子顕微鏡を用いて、傾斜角度数分布グラフをそれぞれ作成した。
すなわち、上記傾斜角度数分布グラフは、上記の履歴α型Ａｌ2Ｏ3層および従来α型Ａｌ2Ｏ3層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、前記表面研磨面の測定範囲内に存在する立方晶結晶格子を有する結晶粒個々に照射して、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、前記表面研磨面の法線に対して、前記結晶粒の結晶面である（０００１）面の法線がなす傾斜角を測定し、この測定結果に基づいて、前記測定傾斜角のうち、０〜４５度の範囲内にある測定傾斜角を０．２５度のピッチ毎に区分すると共に、各区分内に存在する度数を集計することにより作成した。
Next, a field emission scanning electron microscope was used for the hysteresis α-type Al 2 O 3 layer and the conventional α-type Al 2 O 3 layer constituting the hard coating layer of the above-described coated carbide tool of the present invention and the comparative coated carbide tool. Thus, an inclination angle number distribution graph was created.
That is, the inclination angle number distribution graph is shown in the column of the field emission scanning electron microscope with the surfaces of the hysteresis α-type Al 2 O 3 layer and the conventional α-type Al 2 O 3 layer as the polished surface. Set and irradiate the polished surface with an electron beam with an acceleration voltage of 15 kV at an incident angle of 70 degrees with an irradiation current of 1 nA on each crystal grain having a cubic crystal lattice existing within the measurement range of the polished surface. Then, using an electron backscatter diffraction image apparatus, a region of 30 × 50 μm is spaced at a spacing of 0.1 μm / step, and the (0001) plane of the crystal plane of the crystal grain with respect to the normal line of the polished surface The inclination angle formed by the normal is measured, and based on the measurement result, the measurement inclination angle within the range of 0 to 45 degrees is divided into the 0.25 degree pitches among the measurement inclination angles. Created by counting the frequencies existing in the category.
この結果得られた履歴α型Ａｌ2Ｏ3層の傾斜角度数分布グラフにおいて、（０００１）面が１番高いピークを示す傾斜角区分および２番目に高いピークを示す傾斜角区分をそれぞれ表４に示した。表４に示される結果から、１番高いピークが７〜１５度の範囲内の傾斜角区分、そして２番目に高いピークが０〜７度の範囲内の傾斜角区分に存在することが確認された。
また、上記の従来α型Ａｌ2Ｏ3層の傾斜角度数分布グラフでは、表４に示される通りピークが存在しないことが確認された。
さらに、表４には、上記の履歴α型Ａｌ2Ｏ3層および従来α型Ａｌ2Ｏ3層の傾斜角度数分布グラフにおいて、７〜１５度の範囲内の傾斜角区分および０〜７度の範囲内の傾斜角区分に存在する傾斜角度数の傾斜角度数分布グラフ全体の傾斜角度数に占める割合をそれぞれ示した。
In the inclination angle number distribution graph of the hysteresis α-type Al 2 O 3 layer obtained as a result, the inclination angle section showing the highest peak on the (0001) plane and the inclination angle section showing the second highest peak are shown in Table 4 respectively. It was shown to. From the results shown in Table 4, it is confirmed that the highest peak exists in the tilt angle section in the range of 7 to 15 degrees, and the second highest peak exists in the tilt angle section in the range of 0 to 7 degrees. It was.
Further, in the inclination angle number distribution graph of the conventional α-type Al 2 O 3 layer, it was confirmed that no peak exists as shown in Table 4.
Further, in Table 4, in the inclination angle number distribution graph of the above-mentioned hysteresis α-type Al 2 O 3 layer and the conventional α-type Al 2 O 3 layer, the inclination angle division within the range of 7 to 15 degrees and 0 to 7 degrees The ratio of the number of tilt angles existing in the tilt angle section within the range of the tilt angle number distribution graph to the entire tilt angle number distribution graph is shown.
上記の各種の傾斜角度数分布グラフにおいて、表４に示される通り、本発明被覆超硬工具の履歴α型Ａｌ2Ｏ3層は、いずれも（０００１）面の測定傾斜角の分布が少なくとも７〜１５度および０〜７度の範囲内の傾斜角区分にピークが現れ、かつ７〜１５度および０〜７度の範囲内の傾斜角区分内に存在する傾斜角度数の割合が、それぞれ３５〜５０％および２５〜４０％である傾斜角度数分布グラフを示すのに対して、比較被覆超硬工具の従来α型Ａｌ2Ｏ3層は、いずれも（０００１）面の測定傾斜角の分布が０〜４５度の範囲内で不偏的で、ピークが存在せず、７〜１５度および０〜７度の範囲内の傾斜角区分内に存在する傾斜角度数の割合もいずれの場合も２０％以下である傾斜角度数分布グラフを示すものであった。
なお、図２は、本発明被覆超硬工具２の履歴α型Ａｌ2Ｏ3層の傾斜角度数分布グラフ、図３は、比較被覆超硬工具２の従来α型Ａｌ2Ｏ3層の傾斜角度数分布グラフをそれぞれ示すものである。
In the above-mentioned various inclination angle number distribution graphs, as shown in Table 4, the hysteresis α-type Al 2 O 3 layer of the coated carbide tool of the present invention has a measured inclination angle distribution of at least 7 on the (0001) plane. A peak appears in the inclination angle sections in the range of -15 degrees and 0-7 degrees, and the ratio of the number of inclination angles existing in the inclination angle sections in the range of 7-15 degrees and 0-7 degrees is 35 respectively. While the inclination angle number distribution graphs of -50% and 25-40% are shown, the conventional α-type Al 2 O 3 layer of the comparative coated carbide tool has a distribution of measured inclination angles on the (0001) plane. Is unbiased in the range of 0 to 45 degrees, no peak is present, and the ratio of the number of tilt angles present in the tilt angle sections in the range of 7 to 15 degrees and 0 to 7 degrees is 20 in each case. % Inclination angle number distribution graph that is less than or equal to%.
2 is an inclination angle number distribution graph of the history α-type Al 2 O 3 layer of the coated carbide tool 2 of the present invention, and FIG. 3 is a gradient of the conventional α-type Al 2 O 3 layer of the comparative coated carbide tool 2. An angle number distribution graph is shown respectively.
さらに、上記の本発明被覆超硬工具１〜６および比較被覆超硬工具１〜６について、これ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。 Furthermore, about the said invention coated carbide tools 1-6 and comparative coated carbide tools 1-6, the thickness of the constituent layer of the hard coating layer is measured using a scanning electron microscope (longitudinal section measurement). As a result, all showed an average layer thickness (average value of five-point measurement) substantially the same as the target layer thickness.
つぎに、上記の各種の被覆超硬工具を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、本発明被覆超硬工具１〜６および比較被覆超硬工具１〜６について、
被削材：ＪＩＳ・ＳＣＭ４３５の丸棒、
切削速度：４００ｍ／ｍｉｎ、
切り込み：２．５ｍｍ、
送り：０．２ｍｍ／ｒｅｖ、
切削時間：５分、
の条件（切削条件Ａ）での合金鋼の乾式高速高切り込み切削試験（通常の切削速度および切り込みは２５０ｍ／ｍｉｎおよび１．５ｍｍ）、
被削材：ＪＩＳ・Ｓ３５Ｃの丸棒、
切削速度：４５０ｍ／ｍｉｎ、
切り込み：１．０ｍｍ、
送り：０．５ｍｍ／ｒｅｖ、
切削時間：５分、
の条件（切削条件Ｂ）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は３００ｍ／ｍｉｎおよび０．３ｍｍ／ｒｅｖ）、
被削材：ＪＩＳ・ＦＣＤ５００の丸棒、
切削速度：３００ｍ／ｍｉｎ、
切り込み：２．８ｍｍ、
送り：０．３ｍｍ／ｒｅｖ、
切削時間：５分、
の条件（切削条件Ｃ）でのダクタイル鋳鉄の乾式高速高切り込切削試験（通常の切削速度および切り込みは１８０ｍ／ｍｉｎおよび１．５ｍｍ）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９に示した。
Next, the coated carbide tools 1 to 6 of the present invention and the comparative coated carbide tools 1 to 6 are compared with the above-mentioned various coated carbide tools screwed to the tip of the tool steel tool with a fixing jig. For 6,
Work material: JIS / SCM435 round bar,
Cutting speed: 400 m / min,
Incision: 2.5mm,
Feed: 0.2mm / rev,
Cutting time: 5 minutes
Dry high-speed high-cutting test of alloy steel under the following conditions (cutting condition A) (normal cutting speed and cutting are 250 m / min and 1.5 mm),
Work material: JIS / S35C round bar,
Cutting speed: 450 m / min,
Cutting depth: 1.0 mm,
Feed: 0.5mm / rev,
Cutting time: 5 minutes
Dry high-speed high-feed cutting test of carbon steel under the following conditions (cutting condition B) (normal cutting speed and feed are 300 m / min and 0.3 mm / rev),
Work material: JIS / FCD500 round bar,
Cutting speed: 300 m / min,
Cutting depth: 2.8 mm,
Feed: 0.3mm / rev,
Cutting time: 5 minutes
The dry high-speed, high-cut cutting test (normal cutting speed and cutting is 180 m / min and 1.5 mm) of ductile cast iron under the above conditions (cutting condition C). Was measured. The measurement results are shown in Table 9.
表３〜５に示される結果から、本発明被覆超硬工具１〜６は、いずれも硬質被覆層が、（０００１）面の傾斜角が７〜１５度および０〜７度の範囲内の傾斜角区分に１番高いピークと２番目に高いピークが現れ、かつ、前記７〜１５度および０〜７度の傾斜角区分範囲内に存在する度数の合計割合がそれぞれ３５〜５０％および２５〜４０％を占める傾斜角度数分布グラフを示す履歴α型Ａｌ2Ｏ3層で構成され、高温加熱下で高い荷重のかかる鋼や鋳鉄の高速重切削加工でも、前記履歴α型Ａｌ2Ｏ3層がすぐれた高温強度を有し、すぐれた耐チッピング性を発揮することから、切刃部にチッピングの発生なく、すぐれた耐摩耗性を発揮するのに対して、硬質被覆層が、（０００１）面の測定傾斜角の分布が０〜４５度の範囲内で不偏的で、ピークが存在しない傾斜角度数分布グラフを示す従来α型Ａｌ2Ｏ3層で構成された比較被覆超硬工具１〜６においては、いずれも高速重切削加工では特に前記従来α型Ａｌ2Ｏ3層の高温強度が不十分であるために、切刃部にチッピングが発生し、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 3 to 5, each of the coated carbide tools 1 to 6 of the present invention has a hard coating layer having a (0001) plane inclination angle of 7 to 15 degrees and an inclination in the range of 0 to 7 degrees. The highest peak and the second highest peak appear in the corner section, and the total ratio of the frequencies existing in the tilt angle section ranges of 7 to 15 degrees and 0 to 7 degrees is 35 to 50% and 25 to 25%, respectively. It consists of historical α type the Al 2 O 3 layer showing the inclination angle frequency distribution graph which accounts for 40%, even at high heavy cutting of steel and cast iron consuming high loads in a high-temperature heating, the history α type the Al 2 O 3 layer Because it has excellent high-temperature strength and excellent chipping resistance, it exhibits excellent wear resistance without chipping at the cutting edge, whereas the hard coating layer is (0001) The distribution of the measured tilt angle of the surface is unbiased within the range of 0 to 45 degrees, In comparison coated carbide tool 6 which is constituted by a conventional α type the Al 2 O 3 layer showing the inclination angle frequency distribution graph over click is not present, conventional one in particular at high speed heavy cutting the α-type Al 2 O Since the high temperature strength of the three layers is insufficient, it is clear that chipping occurs at the cutting edge and the service life is reached in a relatively short time.
上述のように、この発明の被覆超硬工具は、各種鋼や鋳鉄などの通常の条件での切削加工は勿論のこと、特に硬質被覆層を構成するα型Ａｌ2Ｏ3層に高温強度が要求される高速重切削加工でもすぐれた耐チッピング性を示し、長期に亘ってすぐれた耐摩耗性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 carbide tool of the present invention has high-temperature strength in the α-type Al 2 O 3 layer constituting the hard coating layer as well as cutting under normal conditions such as various steels and cast iron. It exhibits excellent chipping resistance even in the required high-speed heavy cutting, and exhibits excellent wear resistance over a long period of time. It can cope with cost reduction sufficiently satisfactorily.
Claims (1)
（ａ）第１層として、粒状結晶組織を有する窒化チタン層および炭窒化チタン層のうちのいずれか、またはこれら両層の積層からなり、かつ０．１〜１μｍの平均層厚を有する密着接合層、
（ｂ）第２層として、縦長成長結晶組織を有する炭窒化チタン層からなり、かつ３〜１５μｍの平均層厚を有する強靭層、
（ｃ）第３層として、α型の結晶構造および粒状結晶組織を有すると共に、電界放出型走査電子顕微鏡を用い、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、前記表面研磨面の法線に対して、前記結晶粒の結晶面である（０００１）面の法線がなす傾斜角を測定し、前記測定傾斜角のうち、０〜４５度の範囲内にある測定傾斜角を０．２５度のピッチ毎に区分すると共に、各区分内に存在する度数を集計してなる傾斜角度数分布グラフにおいて、少なくとも７〜１５度の範囲内の傾斜角区分および０〜７度の範囲内の傾斜角区分にピークが存在すると共に、傾斜角度数分布グラフにおける度数全体に占める割合で、前記７〜１５度の範囲内に存在する度数の合計が３５〜５０％、前記０〜７度の範囲内に存在する度数の合計が２５〜４０％、である傾斜角度数分布グラフを示す履歴酸化アルミニウム層からなり、かつ３〜１５μｍの平均層厚を有する強化硬質層、
以上第１層〜第３層で構成された硬質被覆層を蒸着形成したこと、を特徴とする高速重切削加工で硬質被覆層がすぐれた耐チッピング性を発揮する表面被覆超硬合金製切削工具。 On the surface of the tool base composed of tungsten carbide base cemented carbide, both are formed by chemical vapor deposition,
(A) Adhesive bonding consisting of a titanium nitride layer and a titanium carbonitride layer having a granular crystal structure as a first layer, or a laminate of both layers, and having an average layer thickness of 0.1 to 1 μm layer,
(B) a tough layer comprising a titanium carbonitride layer having a vertically grown crystal structure as the second layer and having an average layer thickness of 3 to 15 μm,
(C) As the third layer, each crystal grain having an α-type crystal structure and a granular crystal structure and having a hexagonal crystal lattice existing within the measurement range of the surface polished surface using a field emission scanning electron microscope Irradiated with an electron beam, the inclination angle formed by the normal line of the (0001) plane that is the crystal plane of the crystal grain is measured with respect to the normal line of the surface polished surface. In the inclination angle number distribution graph obtained by dividing the measured inclination angle within the range of 45 degrees into every 0.25 degree pitch and totaling the frequencies existing in each division, at least within the range of 7 to 15 degrees In addition, there is a peak in the tilt angle section and the tilt angle section in the range of 0 to 7 degrees, and the total of the frequencies existing in the range of 7 to 15 degrees as a percentage of the entire frequency in the tilt angle frequency distribution graph Is 35-50%, said 0-7 degrees The total of the frequencies present in 囲内 consists history aluminum oxide layer exhibiting a tilt angle frequency distribution graph 25 to 40%, and reinforcing hard layer having an average layer thickness of 3 to 15 [mu] m,
A surface-coated cemented carbide cutting tool that exhibits excellent chipping resistance in high-speed heavy cutting, characterized in that the hard coating layer composed of the first to third layers is formed by vapor deposition. .
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| JP2006305687A (en) * | 2005-04-28 | 2006-11-09 | Mitsubishi Materials Corp | SURFACE-COATED CERMET CUTTING TOOL WITH alpha-TYPE ALUMINUM OXIDE THICK LAYER EXERTING EXCELLENT CHIPPING RESISTANCE |
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| Publication number | Priority date | Publication date | Assignee | Title |
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| JP2000144427A (en) * | 1998-11-05 | 2000-05-26 | Hitachi Metals Ltd | Aluminum oxide coated tool |
| JP2004188577A (en) * | 2002-06-28 | 2004-07-08 | Mitsubishi Materials Corp | Cutting tool of surface-coated cermet with hard coating layer having excellent thermal shock resistance |
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| Publication number | Priority date | Publication date | Assignee | Title |
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| JP2000144427A (en) * | 1998-11-05 | 2000-05-26 | Hitachi Metals Ltd | Aluminum oxide coated tool |
| JP2004188577A (en) * | 2002-06-28 | 2004-07-08 | Mitsubishi Materials Corp | Cutting tool of surface-coated cermet with hard coating layer having excellent thermal shock resistance |
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| Publication number | Priority date | Publication date | Assignee | Title |
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| JP2006305687A (en) * | 2005-04-28 | 2006-11-09 | Mitsubishi Materials Corp | SURFACE-COATED CERMET CUTTING TOOL WITH alpha-TYPE ALUMINUM OXIDE THICK LAYER EXERTING EXCELLENT CHIPPING RESISTANCE |
| JP4666211B2 (en) * | 2005-04-28 | 2011-04-06 | 三菱マテリアル株式会社 | Surface-coated cermet cutting tool with excellent chipping resistance thanks to thick α-type aluminum oxide layer |
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