JP6037113B2 - A surface-coated cutting tool that exhibits excellent chipping resistance with a hard coating layer in high-speed intermittent cutting - Google Patents
A surface-coated cutting tool that exhibits excellent chipping resistance with a hard coating layer in high-speed intermittent cutting Download PDFInfo
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- 238000005520 cutting process Methods 0.000 title claims description 67
- 239000011247 coating layer Substances 0.000 title claims description 32
- 239000013078 crystal Substances 0.000 claims description 213
- 239000010410 layer Substances 0.000 claims description 163
- 239000002131 composite material Substances 0.000 claims description 86
- 239000010936 titanium Substances 0.000 claims description 79
- 239000000758 substrate Substances 0.000 claims description 38
- 229910052719 titanium Inorganic materials 0.000 claims description 36
- 229910052782 aluminium Inorganic materials 0.000 claims description 34
- 239000000203 mixture Substances 0.000 claims description 25
- 238000005229 chemical vapour deposition Methods 0.000 claims description 19
- 230000008859 change Effects 0.000 claims description 17
- 238000010894 electron beam technology Methods 0.000 claims description 13
- 238000009826 distribution Methods 0.000 claims description 10
- 230000000737 periodic effect Effects 0.000 claims description 9
- 239000012495 reaction gas Substances 0.000 claims description 9
- 239000011195 cermet Substances 0.000 claims description 7
- 239000011295 pitch Substances 0.000 claims description 5
- 229910052582 BN Inorganic materials 0.000 claims description 4
- PZNSFCLAULLKQX-UHFFFAOYSA-N Boron nitride Chemical compound N#B PZNSFCLAULLKQX-UHFFFAOYSA-N 0.000 claims description 4
- RTAQQCXQSZGOHL-UHFFFAOYSA-N Titanium Chemical compound [Ti] RTAQQCXQSZGOHL-UHFFFAOYSA-N 0.000 claims description 4
- JLTRXTDYQLMHGR-UHFFFAOYSA-N trimethylaluminium Chemical compound C[Al](C)C JLTRXTDYQLMHGR-UHFFFAOYSA-N 0.000 claims description 4
- UONOETXJSWQNOL-UHFFFAOYSA-N tungsten carbide Chemical compound [W+]#[C-] UONOETXJSWQNOL-UHFFFAOYSA-N 0.000 claims description 4
- 238000004519 manufacturing process Methods 0.000 claims description 2
- 239000000843 powder Substances 0.000 description 45
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- 238000007740 vapor deposition Methods 0.000 description 13
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- 239000012298 atmosphere Substances 0.000 description 10
- 238000000034 method Methods 0.000 description 10
- 229910000851 Alloy steel Inorganic materials 0.000 description 9
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- 238000007733 ion plating Methods 0.000 description 7
- 239000000463 material Substances 0.000 description 7
- 238000005240 physical vapour deposition Methods 0.000 description 7
- 239000002994 raw material Substances 0.000 description 7
- 238000005245 sintering Methods 0.000 description 7
- 238000012360 testing method Methods 0.000 description 7
- CSCPPACGZOOCGX-UHFFFAOYSA-N Acetone Chemical compound CC(C)=O CSCPPACGZOOCGX-UHFFFAOYSA-N 0.000 description 6
- 230000015572 biosynthetic process Effects 0.000 description 6
- 239000011248 coating agent Substances 0.000 description 6
- 238000000576 coating method Methods 0.000 description 6
- 230000002159 abnormal effect Effects 0.000 description 5
- ATJFFYVFTNAWJD-UHFFFAOYSA-N Tin Chemical compound [Sn] ATJFFYVFTNAWJD-UHFFFAOYSA-N 0.000 description 4
- 229910052799 carbon Inorganic materials 0.000 description 4
- 238000002156 mixing Methods 0.000 description 4
- 230000008569 process Effects 0.000 description 4
- 229910018072 Al 2 O 3 Inorganic materials 0.000 description 3
- 229910018575 Al—Ti Inorganic materials 0.000 description 3
- 229910001315 Tool steel Inorganic materials 0.000 description 3
- 229910045601 alloy Inorganic materials 0.000 description 3
- 239000000956 alloy Substances 0.000 description 3
- 238000004458 analytical method Methods 0.000 description 3
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- 230000007774 longterm Effects 0.000 description 3
- 150000004767 nitrides Chemical class 0.000 description 3
- 238000012935 Averaging Methods 0.000 description 2
- 229910004349 Ti-Al Inorganic materials 0.000 description 2
- 229910004692 Ti—Al Inorganic materials 0.000 description 2
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- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 description 1
- 229910000975 Carbon steel Inorganic materials 0.000 description 1
- 229910001018 Cast iron Inorganic materials 0.000 description 1
- 229910000881 Cu alloy Inorganic materials 0.000 description 1
- 206010061274 Malocclusion Diseases 0.000 description 1
- 229910000831 Steel Inorganic materials 0.000 description 1
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Classifications
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B23—MACHINE TOOLS; METAL-WORKING NOT OTHERWISE PROVIDED FOR
- B23B—TURNING; BORING
- B23B27/00—Tools for turning or boring machines; Tools of a similar kind in general; Accessories therefor
- B23B27/14—Cutting tools of which the bits or tips or cutting inserts are of special material
- B23B27/148—Composition of the cutting inserts
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- Engineering & Computer Science (AREA)
- Mechanical Engineering (AREA)
- Cutting Tools, Boring Holders, And Turrets (AREA)
- Chemical Vapour Deposition (AREA)
Description
この発明は、合金鋼等の高熱発生を伴うとともに、切刃に対して衝撃的な負荷が作用する高速断続切削加工で、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 is a surface-coated cutting tool that exhibits high chipping resistance with a hard coating layer in high-speed intermittent cutting with high heat generation of alloy steel and the like, and an impact load acting on the cutting edge (hereinafter referred to as “chip coating”). , Referred to as a coated tool).
従来、一般に、炭化タングステン(以下、WCで示す)基超硬合金、炭窒化チタン(以下、TiCNで示す)基サーメットあるいは立方晶窒化ホウ素(以下、cBNで示す)基超高圧焼結体で構成された基体(以下、これらを総称して基体という)の表面に、硬質被覆層として、Ti−Al系の複合窒化物層を物理蒸着法により蒸着形成した被覆工具が知られており、これらは、すぐれた耐摩耗性を発揮することが知られている。
ただ、上記従来のTi−Al系の複合窒化物層を蒸着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, generally composed of tungsten carbide (hereinafter referred to as WC) based cemented carbide, titanium carbonitride (hereinafter referred to as TiCN) based cermet or cubic boron nitride (hereinafter referred to as cBN) based ultra high pressure sintered body There is known a coated tool in which a Ti—Al based composite nitride layer is formed by physical vapor deposition on a surface of a formed substrate (hereinafter collectively referred to as a substrate) as a hard coating layer. It is known that it exhibits excellent wear resistance.
However, although the above-mentioned conventional coated tool formed by depositing a Ti-Al composite nitride layer has relatively high wear resistance, it tends to cause abnormal wear such as chipping when used under high-speed intermittent cutting conditions. Therefore, various proposals for improving the hard coating layer have been made.
例えば、特許文献1には、基体の表面に、組成式:(Ti1−XAlX)Nで表した場合に、0.35≦X≦0.60(但し、Xは原子比)を満足するTiとAlの複合窒化物からなる硬質被覆層を物理蒸着法で蒸着形成するとともに、硬質被覆層を、上記(Ti,Al)N層の粒状晶組織と柱状晶組織との交互積層構造として構成することが提案されており、そしてこれによって、高硬度鋼の高速断続切削加工において、硬質被覆層がすぐれた耐チッピング性、耐欠損性、耐剥離性を発揮するとされている。
ただ、この被覆工具は、物理蒸着法により硬質被覆層を蒸着形成するため、Alの含有割合Xを0.6以上にはできず、より一段と切削性能を向上させることが望まれている。
For example, Patent Document 1 satisfies 0.35 ≦ X ≦ 0.60 (where X is an atomic ratio) when expressed on the surface of a substrate by a composition formula: (Ti 1-X Al X ) N. A hard coating layer made of a composite nitride of Ti and Al is deposited by physical vapor deposition, and the hard coating layer is formed as an alternating laminated structure of the granular crystal structure and columnar crystal structure of the (Ti, Al) N layer. It has been proposed that it is constructed, and this makes it possible for the hard coating layer to exhibit excellent chipping resistance, chipping resistance, and peeling resistance in high-speed intermittent cutting of high-hardness steel.
However, since this coated tool deposits a hard coating layer by physical vapor deposition, the Al content ratio X cannot be increased to 0.6 or more, and it is desired to further improve the cutting performance.
このような観点から、化学蒸着法で硬質被覆層を形成することで、Alの含有割合Xを、0.9程度にまで高める技術も提案されている。
例えば、特許文献2には、TiCl4、AlCl3、NH3の混合反応ガス中で、650〜900℃の温度範囲において化学蒸着を行うことにより、Alの含有割合Xの値が0.65〜0.95である(Ti1−XAlX)N層を蒸着形成できることが記載されているが、この文献では、この(Ti1−XAlX)N層の上にさらにAl2O3層を被覆し、これによって断熱効果を高めることを目的とするものであるから、Xの値を0.65〜0.95まで高めた(Ti1−XAlX)N層の形成によって、切削性能へ如何なる影響があるかという点についてまでの開示はない。
From such a viewpoint, a technique for increasing the Al content ratio X to about 0.9 by forming a hard coating layer by chemical vapor deposition has also been proposed.
For example, Patent Document 2 discloses that the value of the Al content ratio X is 0.65 to 0.65 by performing chemical vapor deposition in a temperature range of 650 to 900 ° C. in a mixed reaction gas of TiCl 4 , AlCl 3 , and NH 3. Although it is described that a (Ti 1-X Al X ) N layer of 0.95 can be formed by vapor deposition, in this document, an Al 2 O 3 layer is further formed on the (Ti 1-X Al X ) N layer. Therefore, the cutting performance is improved by forming the (Ti 1-X Al X ) N layer in which the value of X is increased from 0.65 to 0.95. There is no disclosure up to the point of how this will be affected.
また、例えば、特許文献3には、TiCN層、Al2O3層を内層として、その上に、化学蒸着法により、立方晶構造あるいは六方晶構造を含む立方晶構造の(Ti1−XAlX)N層(但し、Xは0.65〜0.9)を外層として被覆するとともに、該外層に100〜1100MPaの圧縮応力を付与することにより、被覆工具の耐熱性と疲労強度を改善することが提案されている。 Further, for example, in Patent Document 3, a TiCN layer and an Al 2 O 3 layer are used as an inner layer, and a cubic structure (Ti 1-X Al) including a cubic structure or a hexagonal structure is formed thereon by chemical vapor deposition. X ) N layer (where X is 0.65 to 0.9) is coated as an outer layer, and compressive stress of 100 to 1100 MPa is applied to the outer layer, thereby improving the heat resistance and fatigue strength of the coated tool. It has been proposed.
近年の切削加工における省力化および省エネ化の要求は強く、これに伴い、切削加工は一段と高速化、高効率化の傾向にあり、被覆工具には、より一層、耐チッピング性、耐欠損性、耐剥離性等の耐異常損傷性が求められるとともに、長期の使用に亘ってのすぐれた耐摩耗性が求められている。
しかし、上記特許文献1に記載される被覆工具は、(Ti1−XAlX)N層からなる硬質被覆層が物理蒸着法で蒸着形成され、硬質被覆層中のAl含有量Xを高めることができないため、例えば、合金鋼の高速断続切削に供した場合には、耐チッピング性が十分であるとは言えない。
一方、上記特許文献2に記載される化学蒸着法で蒸着形成した(Ti1−XAlX)N層については、Al含有量Xを高めることができ、また、立方晶構造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はすぐれた硬質被覆層が得られるものの、基体との密着強度は十分でなく、また、靭性に劣る。
さらに、上記特許文献3に記載される被覆工具は、所定の硬さを有し耐摩耗性にはすぐれるものの、靭性に劣ることから、合金鋼の高速断続切削加工等に供した場合には、チッピング、欠損、剥離等の異常損傷が発生しやすく、満足できる切削性能を発揮するとは言えない。
本発明は、合金鋼の高速断続切削等の高速断続切削加工に供した場合であっても、すぐれた靭性を備え、長期の使用に亘ってすぐれた耐チッピング性、耐摩耗性を発揮する被覆工具を提供することを目的とするものである。
In recent years, there has been a strong demand for energy saving and energy saving in cutting, and along with this, cutting tends to be faster and more efficient, and the coated tool has even more chipping resistance, chipping resistance, Abnormal damage resistance such as peel resistance is required, and excellent wear resistance over long-term use is required.
However, in the coated tool described in Patent Document 1, a hard coating layer made of a (Ti 1-X Al X ) N layer is deposited by physical vapor deposition to increase the Al content X in the hard coating layer. Therefore, for example, when it is subjected to high-speed intermittent cutting of alloy steel, it cannot be said that the chipping resistance is sufficient.
On the other hand, for the (Ti 1-X Al X ) N layer formed by chemical vapor deposition described in Patent Document 2, the Al content X can be increased and a cubic structure can be formed. Therefore, although a hard coating layer having a predetermined hardness and excellent wear resistance can be obtained, the adhesion strength with the substrate is not sufficient, and the toughness is inferior.
Furthermore, although the coated tool described in Patent Document 3 has a predetermined hardness and excellent wear resistance, it is inferior in toughness, so when it is used for high-speed intermittent cutting of alloy steel, etc. In addition, abnormal damage such as chipping, chipping and peeling is likely to occur, and it cannot be said that satisfactory cutting performance is exhibited.
The present invention is a coating that has excellent toughness and excellent chipping resistance and wear resistance over a long period of use even when subjected to high-speed intermittent cutting such as high-speed intermittent cutting of alloy steel. The purpose is to provide a tool.
本発明者等は、上述の観点から、少なくともTiとAlの複合炭窒化物(以下、「(Ti,Al)(C,N)」あるいは「(Ti1−XAlX)(CYN1−Y)」で示すことがある)を含む硬質被覆層を化学蒸着で蒸着形成した被覆工具の耐チッピング性、耐摩耗性の改善をはかるべく、鋭意研究を重ねた結果、次のような知見を得た。 From the above viewpoint, the present inventors have at least a composite carbonitride of Ti and Al (hereinafter referred to as “(Ti, Al) (C, N)” or “(Ti 1-X Al X ) (C Y N 1 ). As a result of earnest research to improve the chipping resistance and wear resistance of a coated tool formed by chemical vapor deposition of a hard coating layer including -Y ))), the following findings Got.
炭化タングステン基超硬合金(以下、「WC基超硬合金」で示す)、炭窒化チタン基サーメット(以下、「TiCN基サーメット」で示す)、または立方晶窒化ホウ素基超高圧焼結体(以下、「cBN基超高圧焼結体」で示す)のいずれかで構成された基体の表面に、
例えば、トリメチルアルミニウム(Al(CH3)3)を反応ガス成分として含有する化学蒸着法により、複合炭窒化物層として、立方晶結晶相と六方晶結晶相との所定の面積割合の混合組織からなる(Ti1−XAlX)(CYN1−Y)層を蒸着形成することができるとともに、基体表面の法線方向に対する該複合炭窒化物層の六方晶結晶相の結晶粒の(0001)面の法線の傾斜角度数分布割合を40%以上とすることができ、これにより、複合炭窒化物層は、高い耐摩耗性を保ちつつ靭性が向上し、長期の使用に亘って、すぐれた耐チッピング性、耐摩耗性を示すことを見出したのである。
Tungsten carbide-based cemented carbide (hereinafter referred to as “WC-based cemented carbide”), titanium carbonitride-based cermet (hereinafter referred to as “TiCN-based cermet”), or cubic boron nitride-based ultrahigh pressure sintered body (hereinafter referred to as “TiCN-based cemented carbide”) On the surface of the substrate composed of any one of “cBN-based ultra-high pressure sintered body”
For example, by a chemical vapor deposition method containing trimethylaluminum (Al (CH 3 ) 3 ) as a reaction gas component, as a composite carbonitride layer, from a mixed structure of a predetermined area ratio of a cubic crystal phase and a hexagonal crystal phase (Ti 1-X Al X ) (C Y N 1-Y ) layer can be formed by vapor deposition, and the hexagonal crystal phase of the composite carbonitride layer with respect to the normal direction of the substrate surface ( The inclination angle number distribution ratio of the normal line of the (0001) plane can be made 40% or more, whereby the composite carbonitride layer has improved toughness while maintaining high wear resistance, and can be used over a long period of use. They have found that they have excellent chipping resistance and wear resistance.
また、本発明者等は、上記立方晶結晶相と六方晶結晶相との混合組織からなる(Ti1−XAlX)(CYN1−Y)層において、各結晶相の結晶粒について測定した粒子幅およびアスペクト比から求めた各結晶相の結晶粒の平均粒子幅、平均アスペクト比を所定の数値範囲に規制することにより、複合炭窒化物層の靭性を維持しつつ、より一段と、複合炭窒化物層の耐摩耗性を向上させ得ることを見出したのである。 In addition, the present inventors, in the (Ti 1-X Al X ) (C Y N 1-Y ) layer composed of a mixed structure of the cubic crystal phase and the hexagonal crystal phase, By controlling the average grain width of each crystal phase obtained from the measured grain width and aspect ratio, the average aspect ratio to a predetermined numerical range, while maintaining the toughness of the composite carbonitride layer, It has been found that the wear resistance of the composite carbonitride layer can be improved.
さらに、本発明者等は、上記複合炭窒化物層の立方晶結晶相の結晶粒の立方晶構造を有する結晶内に(Ti1−XAlX)(CYN1−Y)のTiとAlの周期的な濃度変化が存在し、周期的に変化するXの極大値と極小値及び、周期を所定の数値範囲に規制することにより、複合炭窒化物層の硬さを向上させ、より一段と、複合炭窒化物層の耐摩耗性を向上させ得ることを見出したのである。 Furthermore, the inventors of the present invention have included the Ti of (Ti 1-X Al X ) (C Y N 1-Y ) in the crystal having the cubic crystal structure of the cubic crystal phase of the composite carbonitride layer. There is a periodic concentration change of Al, and by periodically limiting the maximum and minimum values of X and the period to a predetermined numerical range, the hardness of the composite carbonitride layer is improved, and more It has been found that the wear resistance of the composite carbonitride layer can be further improved.
したがって、上記のような複合炭窒化物層を備えた被覆工具を、例えば、合金鋼の高速断続切削等に用いた場合には、チッピング、欠損、剥離等の発生が抑えられるとともに、長期の使用にわたってすぐれた耐摩耗性を発揮することができるのである。 Therefore, when the coated tool provided with the composite carbonitride layer as described above is used for, for example, high-speed intermittent cutting of alloy steel, the occurrence of chipping, chipping, peeling, etc. is suppressed, and long-term use It is possible to exhibit excellent wear resistance.
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、
「(1) 炭化タングステン基超硬合金、炭窒化チタン基サーメット、または立方晶窒化ホウ素基超高圧焼結体のいずれかで構成された基体の表面に、硬質被覆層が被覆された表面被覆切削工具であって、
(a)上記硬質被覆層は、平均層厚1〜20μmのTiとAlの複合炭窒化物層を少なくとも含み、その平均組成を、
組成式:(Ti1−XAlX)(CYN1−Y)
で表した場合、Al含有割合XおよびC含有割合Y(但し、X、Yは何れも原子比)は、それぞれ、0.60≦X≦0.95、0.0005≦Y≦0.005を満足し、
(b)上記複合炭窒化物層は、電子線後方散乱回折装置を用いて個々の結晶粒の結晶構造を、上記TiとAlの複合炭窒化物層の縦断面方向から解析した場合、立方晶結晶格子の電子線後方散乱回折像が観察される立方晶結晶相と六方晶結晶格子の電子線後方散乱回折像が観察される六方晶結晶相との混合組織からなり、かつ、立方晶結晶相と六方晶結晶相との合計に占める六方晶結晶相の面積割合は10〜50面積%であり、
(c)基体表面の法線方向に対する上記複合炭窒化物層の六方晶結晶相の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、該測定傾斜角のうち、基体表面の法線方向に対して0〜90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して各区分内に存在する度数を集計した場合、2〜12度の範囲内の傾斜角区分に最高ピークが存在するとともに、該2〜12度の傾斜角区分に存在する度数の合計は、傾斜角度数分布における度数全体の40%以上であることを特徴とする表面被覆切削工具。
(2) 上記複合炭窒化物層の立方晶結晶相の結晶粒の平均粒子幅ωcが0.3μm以下であり、平均アスペクト比αcが2未満であり、また、
上記複合炭窒化物層の六方晶結晶相の結晶粒の平均粒子幅ωhが0.1〜2μmであり、平均アスペクト比αhが2以上、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。
(3) 上記複合炭窒化物層の立方晶結晶相の結晶粒の立方晶構造を有する結晶内に(Ti1−XAlX)(CYN1−Y)のTiとAlの周期的な濃度変化が存在し、周期的に変化するXの極大値と極小値の差が0.05〜0.25、望ましくは0.10〜0.20であり、その周期が3〜30nmであることを特徴とする前記(1)または(2)に記載の表面被覆切削工具。
(4) 上記複合炭窒化物層は、少なくとも、トリメチルアルミニウムを反応ガス成分として含有する化学蒸着法により蒸着形成することを特徴とする前記(1)から(3)のいずれかに記載の表面被覆切削工具の製造方法。」
に特徴を有するものである。
なお、本発明における硬質被覆層は、前述のような複合炭窒化物層をその本質的構成とするが、さらに、従来より知られている下部層や上部層などと併用することにより、一層すぐれた特性を創出することができる。
This invention was made based on the above research results,
“(1) Surface-coated cutting in which a hard coating layer is coated on the surface of a substrate composed of any of tungsten carbide-based cemented carbide, titanium carbonitride-based cermet, or cubic boron nitride-based ultrahigh-pressure sintered body A tool,
(A) the hard coating layer comprises at least a complex carbonitride layer of Ti and Al flat HitoshisoAtsu 1 to 20 [mu] m, the average composition,
Formula: (Ti 1-X Al X ) (C Y N 1-Y)
In this case, the Al content ratio X and the C content ratio Y (where X and Y are atomic ratios) satisfy 0.60 ≦ X ≦ 0.95 and 0.0005 ≦ Y ≦ 0.005, respectively. Satisfied,
(B) When the composite carbonitride layer is analyzed from the longitudinal cross-sectional direction of the composite carbonitride layer of Ti and Al using an electron beam backscattering diffractometer, the crystal structure of each crystal grain is cubic. It consists of a mixed structure of a cubic crystal phase in which an electron beam backscatter diffraction image of the crystal lattice is observed and a hexagonal crystal phase in which an electron beam backscatter diffraction image of the hexagonal crystal lattice is observed, and the cubic crystal phase The area ratio of the hexagonal crystal phase to the total of the hexagonal crystal phase is 10 to 50 area%,
(C) measuring an inclination angle formed by a normal line of a (0001) plane which is a crystal plane of a crystal grain of a hexagonal crystal phase of the composite carbonitride layer with respect to a normal direction of the substrate surface; When the measured inclination angles within the range of 0 to 90 degrees with respect to the normal direction of the substrate surface are divided into pitches of 0.25 degrees and the frequencies existing in each section are tabulated, 2 to 12 degrees The maximum peak exists in the inclination angle section within the range of 2 to 12, and the sum of the frequencies existing in the inclination angle section of 2 to 12 degrees is 40% or more of the entire frequency in the inclination angle frequency distribution. Surface coated cutting tool.
(2) The average grain width ω c of the cubic crystal phase grains of the composite carbonitride layer is 0.3 μm or less, the average aspect ratio α c is less than 2,
In the above (1), the average grain width ω h of the hexagonal crystal phase crystal grains of the composite carbonitride layer is 0.1 to 2 μm, and the average aspect ratio α h is 2 or more. The surface-coated cutting tool described.
(3) The periodicity of Ti and Al in (Ti 1-X Al X ) (C Y N 1-Y ) in a crystal having a cubic crystal structure of cubic crystal phase of the composite carbonitride layer. There is a change in concentration, and the difference between the maximum value and the minimum value of X that changes periodically is 0.05 to 0.25, preferably 0.10 to 0.20, and the period is 3 to 30 nm. The surface-coated cutting tool according to (1) or (2), characterized in that
(4) the composite carbonitride layer is at least, the surface coating according to any one of, which comprises vapor deposited by chemical vapor deposition containing trimethyl aluminum as a reaction gas component from (1) (3) Cutting tool manufacturing method . "
It has the characteristics.
Note that the hard coating layer in the present invention has the above-described composite carbonitride layer as its essential structure, but is further improved by using it together with conventionally known lower layers and upper layers. New characteristics can be created.
つぎに、この発明の被覆工具の硬質被覆層について、より具体的に説明する。 Next, the hard coating layer of the coated tool of the present invention will be described more specifically.
硬質被覆層を構成するTiとAlの複合炭窒化物((Ti1−XAlX)(CYN1−Y))層の平均組成:
上記(Ti1−XAlX)(CYN1−Y)層において、Alの含有割合X(原子比)の値が0.60未満になると、複合炭窒化物層の組織中における六方晶結晶相の面積割合の減少により、耐クレータ摩耗性が低下し、チッピング、欠損等の異常損傷を発生しやすくなり、一方、X(原子比)の値が0.95を超えると、相対的なTi含有割合の減少により、複合炭窒化物層の組織中における立方晶結晶相の面積割合の減少により、硬さが低下するとともに耐逃げ面摩耗性が低下することから、X(原子比)の値は、0.60以上0.95以下とすることが必要である。
また、上記(Ti1−XAlX)(CYN1−Y)層において、C成分には層の潤滑性を向上させ、一方、N成分には層の高温強度を向上させる作用があるが、C成分の含有割合Y(原子比)が0.0005未満となると高い潤滑性が得られなくなり、一方、Y(原子比)が0.005を超えると、高温強度が低下してくることから、Y(原子比)の値は、0.0005以上0.005以下と定めた。
なお、上記(Ti1−XAlX)(CYN1−Y)層は、その平均層厚が1μm未満では、長期の使用に亘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20μmを越えると、高熱発生を伴う高速断続切削で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、その合計平均層厚は1〜20μmと定めた。
Average composition of Ti and Al composite carbonitride ((Ti 1-X Al X ) (C Y N 1-Y )) layer constituting the hard coating layer:
In the above (Ti 1-X Al X ) (C Y N 1-Y ) layer, when the Al content ratio X (atomic ratio) is less than 0.60, hexagonal crystals in the structure of the composite carbonitride layer Due to the decrease in the area ratio of the crystal phase, crater wear resistance is reduced, and abnormal damage such as chipping and defects is likely to occur. On the other hand, if the value of X (atomic ratio) exceeds 0.95, Due to the decrease in the Ti content ratio, the decrease in the area ratio of the cubic crystal phase in the structure of the composite carbonitride layer decreases the hardness and flank wear resistance, so X (atomic ratio) The value needs to be 0.60 or more and 0.95 or less.
Further, in the (Ti 1-X Al X ) (C Y N 1-Y ) layer, the C component improves the lubricity of the layer, while the N component has an effect of improving the high temperature strength of the layer. However, when the content ratio Y (atomic ratio) of the C component is less than 0.0005, high lubricity cannot be obtained. On the other hand, when the Y (atomic ratio) exceeds 0.005, the high-temperature strength decreases. Therefore, the value of Y (atomic ratio) was determined to be 0.0005 or more and 0.005 or less.
In addition, the (Ti 1-X Al X ) (C Y N 1-Y ) layer has an average layer thickness of less than 1 μm, and cannot sufficiently ensure wear resistance over a long period of use. On the other hand, when the average layer thickness exceeds 20 μm, it becomes easy to cause thermoplastic deformation by high-speed intermittent cutting with high heat generation, and this causes uneven wear. Therefore, the total average layer thickness is set to 1 to 20 μm. .
この発明では、上記平均組成を有する(Ti1−XAlX)(CYN1−Y)層からなる複合炭窒化物層において、層全体にわたって単一相組織にするのではなく、六方晶結晶相と立方晶結晶相の混合組織として形成する。
即ち、複合炭窒化物層の断面について、電子線後方散乱回折装置を用いてその結晶構造を解析した場合、立方晶結晶格子の電子線後方散乱回折像が観察される立方晶結晶相と六方晶結晶格子の電子線後方散乱回折像が観察される六方晶結晶相との混合組織からなり、かつ、立方晶結晶相と六方晶結晶相との合計に占める六方晶結晶相の面積割合は10〜50面積%である。
上記の混合組織からなる複合炭窒化物層において、六方晶結晶相の面積割合が50面積%を超えると硬さが低下し、特に、耐逃げ面摩耗性が低下する。
一方、六方晶結晶相の面積割合が10面積%未満となった場合には、耐クレータ摩耗性が低下し、切れ刃が異常損傷を起こしやすくなり、その結果として、工具寿命が短命となる。
したがって、立方晶結晶相と六方晶結晶相との混合組織からなる複合炭窒化物層中における六方晶結晶相の占める面積割合は10〜50面積%とする。
In the present invention, in the composite carbonitride layer composed of the (Ti 1-X Al X ) (C Y N 1-Y ) layer having the above average composition, a hexagonal crystal is used instead of a single phase structure throughout the layer. It forms as a mixed structure of crystal phase and cubic crystal phase.
That is, when the crystal structure of the composite carbonitride layer is analyzed using an electron backscattering diffractometer, the cubic crystal phase and hexagonal crystal in which the electron backscattering diffraction image of the cubic crystal lattice is observed. It consists of a mixed structure with the hexagonal crystal phase in which the electron backscatter diffraction image of the crystal lattice is observed, and the area ratio of the hexagonal crystal phase to the total of the cubic crystal phase and the hexagonal crystal phase is 10 to 10 50 area%.
In the composite carbonitride layer composed of the above mixed structure, when the area ratio of the hexagonal crystal phase exceeds 50 area%, the hardness decreases, and in particular, the flank wear resistance decreases.
On the other hand, when the area ratio of the hexagonal crystal phase is less than 10 area%, the crater wear resistance is lowered, and the cutting edge is liable to be damaged abnormally. As a result, the tool life is shortened.
Therefore, the area ratio of the hexagonal crystal phase in the composite carbonitride layer composed of the mixed structure of the cubic crystal phase and the hexagonal crystal phase is 10 to 50 area%.
また、この発明では、複合炭窒化物層の耐クレータ摩耗性を更に高めるために、複合炭窒化物層中で六方晶結晶相を構成する結晶粒について、電界放出型走査電子顕微鏡と電子線後方散乱回折装置を用いて基体表面の法線方向に対する六方晶結晶相の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、該測定傾斜角のうち、基体表面の法線方向に対して0〜90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して各区分内に存在する度数を集計した場合、2〜12度の範囲内の傾斜角区分に最高ピークが存在するとともに、該2〜12度の傾斜角区分に存在する度数の合計は、傾斜角度数分布における度数全体の40%以上を占めるようにすることが必要である。 Further, in the present invention, in order to further enhance the crater wear resistance of the composite carbonitride layer, the field emission scanning electron microscope and the back of the electron beam are used for the crystal grains constituting the hexagonal crystal phase in the composite carbonitride layer. Using a scattering diffractometer, the inclination angle formed by the normal of the (0001) plane, which is the crystal plane of the crystal grain of the hexagonal crystal phase, with respect to the normal direction of the substrate surface is measured. When the measurement inclination angle within the range of 0 to 90 degrees with respect to the normal direction is divided into pitches of 0.25 degrees and the frequencies existing in each section are tabulated, the range of 2 to 12 degrees is included. It is necessary that the highest peak exists in the inclination angle section, and the total of the frequencies existing in the inclination angle section of 2 to 12 degrees occupies 40% or more of the entire frequencies in the inclination angle distribution.
また、基体表面の法線方向に対する、上記六方晶結晶相の結晶粒の結晶面である(0001)面の法線がなす傾斜角が2〜12度の傾斜角区分に存在する度数が、傾斜角度数分布における度数全体の40%未満である場合には、すぐれた耐クレータ摩耗性を期待できないので、前記2〜12度の傾斜角区分に存在する度数割合は40%以上とすることが必要である。 In addition, the frequency existing in the tilt angle section with the tilt angle of 2 to 12 degrees formed by the normal line of the (0001) plane which is the crystal plane of the crystal grains of the hexagonal crystal phase with respect to the normal direction of the substrate surface is tilted. When the angle distribution is less than 40% of the entire frequency, excellent crater wear resistance cannot be expected. Therefore, the frequency ratio existing in the inclination angle section of 2 to 12 degrees needs to be 40% or more. It is.
さらに、この発明では、複合炭窒化物層中の立方晶結晶相と六方晶結晶相を構成するそれぞれの結晶粒について、平均粒子幅と平均アスペクト比を所定の数値範囲に定めることが好ましく、これによって、複合炭窒化物層の更なる硬さの向上と耐クレータ摩耗性の向上を期待することができる。 Further, in the present invention, it is preferable that the average grain width and the average aspect ratio are determined within a predetermined numerical range for each crystal grain constituting the cubic crystal phase and the hexagonal crystal phase in the composite carbonitride layer. Thus, it is possible to expect further improvement in hardness and crater wear resistance of the composite carbonitride layer.
さらに、この発明では、上記複合炭窒化物層の立方晶結晶相の結晶粒の立方晶構造を有する結晶内に(Ti1−XAlX)(CYN1−Y)のTiとAlの周期的な濃度変化が存在し、周期的に変化するXの極大値と極小値及び、周期を所定の数値範囲に定めることが好ましく、これによって、複合炭窒化物層の更なる硬さの向上と耐逃げ面摩耗性の向上を期待することができる。 Further, in the present invention, the Ti and Al of (Ti 1-X Al X ) (C Y N 1-Y ) are contained in a crystal having a cubic crystal structure of the cubic crystal phase of the composite carbonitride layer. It is preferable that the periodic maximum concentration and minimum value and the period of X change periodically, and the period be set to a predetermined numerical range, thereby further improving the hardness of the composite carbonitride layer. And improvement of flank wear resistance can be expected.
具体的には以下のとおりである。
まず、複合炭窒化物層中の立方晶結晶相を構成する結晶粒について述べる。
基体表面と平行な方向の上記結晶粒の粒子幅をWc、また、基体表面に垂直な方向の上記結晶粒の粒子長さをLcとし、該WcとLcとの比Lc/Wcを各結晶粒のアスペクト比Acとし、さらに、個々の結晶粒について求めたアスペクト比Acの平均値を平均アスペクト比αc、個々の結晶粒について求めた粒子幅Wcの平均値を平均粒子幅ωcとした場合、平均アスペクト比αcを2未満、また、平均粒子幅ωcを0.3μm以下とすることによって、立方晶結晶相をより高硬度のものとすることができる。
次に、複合炭窒化物層中の六方晶結晶相を構成する結晶粒について述べる。
前記立方晶結晶相を構成する結晶粒についての場合と同様に、複合炭窒化物層中の六方晶結晶相の各結晶粒について、基体表面と平行な方向の粒子幅をWh、また、基体表面に垂直な方向の粒子長さをLhとし、該WhとLhとの比Lh/Whを各結晶粒のアスペクト比Ahとし、さらに、個々の結晶粒について求めたアスペクト比Ahの平均値を平均アスペクト比αh、個々の結晶粒について求めた粒子幅Whの平均値を平均粒子幅ωhとした場合、平均アスペクト比αhを2以上、また、平均粒子幅ωhを0.1〜2μmとすることによって、六方晶結晶相の耐クレータ摩耗性を向上させることができる。
したがって、この発明では、複合炭窒化物層中の立方晶結晶相を構成する結晶粒の平均アスペクト比αcを2未満、また、平均粒子幅ωcを0.3μm以下とし、また、六方晶結晶相を構成する結晶粒の平均アスペクト比αhを2以上、また、平均粒子幅ωhを0.1〜2μmとすることが好ましく、そしてこれによって、複合炭窒化物層の硬さの向上と耐クレータ摩耗性の向上を図ることができる。
Specifically, it is as follows.
First, the crystal grains constituting the cubic crystal phase in the composite carbonitride layer will be described.
The particle width of the substrate surface in a direction parallel to the grain W c, also the crystal grains of the grain length in the direction perpendicular to the substrate surface and L c, the ratio between the W c and L c L c / the W c and the aspect ratio a c of the crystal grains, further, the average value of the individual average aspect ratio the mean value of the aspect ratio a c determined for grains alpha c, the particle width W c obtained for each grain Is the average grain width ω c , the average aspect ratio α c is less than 2 and the average grain width ω c is 0.3 μm or less, so that the cubic crystal phase has a higher hardness. it can.
Next, the crystal grains constituting the hexagonal crystal phase in the composite carbonitride layer will be described.
As in the case of the crystal grains constituting the cubic crystal phase, for each crystal grain of the hexagonal crystal phase in the composite carbonitride layer, the grain width in the direction parallel to the substrate surface is set to W h , and L h perpendicular direction of the particle length to the surface, the ratio L h / W h of the W h and L h is the aspect ratio a h of each crystal grain, further, the aspect ratio determined for individual grain When the average value of A h is the average aspect ratio α h and the average value of the particle width W h obtained for each crystal grain is the average particle width ω h , the average aspect ratio α h is 2 or more, and the average particle width By setting ω h to 0.1 to 2 μm, the crater wear resistance of the hexagonal crystal phase can be improved.
Therefore, in the present invention, the average aspect ratio α c of the crystal grains constituting the cubic crystal phase in the composite carbonitride layer is less than 2, the average grain width ω c is 0.3 μm or less, and the hexagonal crystal The average aspect ratio α h of the crystal grains constituting the crystal phase is preferably 2 or more, and the average particle width ω h is preferably 0.1 to 2 μm, thereby improving the hardness of the composite carbonitride layer And crater wear resistance can be improved.
さらに、立方晶構造を有する結晶を組成式:(Ti1−xAlx)(CyN1−y)で表した場合、TiとAlの周期的な濃度変化が存在するとき、結晶粒に歪みが生じ、硬さが向上する。しかしながら、TiとAlの濃度変化の大きさの指標である前記組成式におけるXの極大値と極小値の差が0.05より小さいと前述した結晶粒の歪みが小さく十分な硬さの向上が見込めない。一方、Xの極大値と極小値の差が0.25を超えると結晶粒の歪みが大きくなり過ぎ、格子欠陥が大きくなり、硬さが低下する。また、濃度変化の周期が3nm未満では靭性が低下し、30nmを超えると硬さの向上効果が見込めない。そこで、立方晶構造を有する結晶内に存在するTiとAlの濃度変化は、周期的に変化するXの極大値と極小値の差を0.05〜0.25、望ましくは0.10〜0.20とし、その周期を3〜30nmとすることが好ましく、そしてこれによって、複合炭窒化物層の硬さの向上と耐逃げ面摩耗性の向上を図ることができる。 Further, when a crystal having a cubic structure is expressed by a composition formula: (Ti 1-x Al x ) (C y N 1-y ), when there is a periodic concentration change of Ti and Al, Distortion occurs and hardness is improved. However, if the difference between the maximum value and the minimum value of X in the composition formula, which is an index of the change in the concentration of Ti and Al, is smaller than 0.05, the distortion of the crystal grains described above is small and sufficient hardness is improved. I can't expect. On the other hand, if the difference between the maximum value and the minimum value of X exceeds 0.25, the distortion of crystal grains becomes too large, lattice defects become large, and the hardness decreases. Further, if the period of concentration change is less than 3 nm, the toughness decreases, and if it exceeds 30 nm, the effect of improving hardness cannot be expected. Therefore, the change in the concentration of Ti and Al present in the crystal having a cubic structure is 0.05 to 0.25, preferably 0.10 to 0, in which the difference between the maximum value and the minimum value of X that changes periodically is 0.05 to 0.25. 20 and the period is preferably 3 to 30 nm, and this can improve the hardness and flank wear resistance of the composite carbonitride layer.
この発明の(Ti1−XAlX)(CYN1−Y)層は、例えば、次に述べる条件の化学蒸着法によって蒸着形成することができる。
反応ガス組成(容量%):
TiCl4 2.0〜3.0%、Al(CH3)3 3.0〜5.0%、
AlCl3 3.0〜5.0%、NH3 2.0〜5.0%、
N2 6.0〜10.0%、C2H40〜1.0%、
残りH2、
反応雰囲気温度: 700〜900 ℃、
反応雰囲気圧力: 2〜5 kPa、
上記条件の化学蒸着法によって、平均組成が、0.60≦X≦0.95、0.0005≦Y≦0.005(但し、X、Yは何れも原子比)を満足し、
組成式:(Ti1−XAlX)(CYN1−Y)
で表されるTiとAlの複合炭窒化物層が蒸着形成される。
なお、複合炭窒化物層中の立方晶結晶相と六方晶結晶相の面積割合は、特に、NH3の含有量によって影響され、例えば、他の条件を一定(反応ガス組成(容量%):TiCl4 3.0%、Al(CH3)3 4.0%、AlCl3 5.0%、N28.0%、C2H4 1%、 残りH2、反応雰囲気温度:900℃、反応雰囲気圧力: 4kPa)とし、NH3の含有量のみを変化させた場合、NH3の含有量が、下限の2.0%である場合には、六方晶結晶相の面積割合は33%、また、上限の5.0%である場合には、六方晶結晶相の面積割合は10%となる。
The (Ti 1-X Al X ) (C Y N 1-Y ) layer of the present invention can be deposited by, for example, chemical vapor deposition under the following conditions.
Reaction gas composition (volume%):
TiCl 4 2.0-3.0%, Al (CH 3 ) 3 3.0-5.0%,
AlCl 3 3.0~5.0%, NH 3 2.0~5.0 %,
N 2 6.0~10.0%, C 2 H 4 0~1.0%,
Remaining H 2 ,
Reaction atmosphere temperature: 700 to 900 ° C.
Reaction atmosphere pressure: 2 to 5 kPa,
By chemical vapor deposition under the above conditions, the average composition satisfies 0.60 ≦ X ≦ 0.95 and 0.0005 ≦ Y ≦ 0.005 (where X and Y are atomic ratios),
Formula: (Ti 1-X Al X ) (C Y N 1-Y)
A composite carbonitride layer of Ti and Al represented by is formed by vapor deposition.
In addition, the area ratio of the cubic crystal phase and the hexagonal crystal phase in the composite carbonitride layer is particularly affected by the content of NH 3 , for example, other conditions are constant (reaction gas composition (volume%): TiCl 4 3.0%, Al (CH 3 ) 3 4.0%, AlCl 3 5.0%, N 2 8.0%, C 2 H 4 1%, remaining H 2 , reaction atmosphere temperature: 900 ° C. When the reaction atmosphere pressure is 4 kPa) and only the NH 3 content is changed, when the NH 3 content is 2.0% of the lower limit, the area ratio of the hexagonal crystal phase is 33%, When the upper limit is 5.0%, the area ratio of the hexagonal crystal phase is 10%.
さらに、前記成膜工程の際に、反応を一時停止し、TiCl4:2.0〜5.0%、H2:残、反応雰囲気圧力:3.0kPa、反応雰囲気温度:800〜900℃の条件からなる、TiCl4エッチング工程を所定回数挟むことにより、複合炭窒化物層の立方晶結晶相の結晶粒の立方晶構造を有する結晶内に(Ti1−XAlX)(CYN1−Y)のTiとAlの周期的な濃度変化が存在するTiとAlの複合炭窒化物層が蒸着形成される。
前述のようなTiCl4エッチング工程を成膜工程中に挟むことにより、立方晶TiAlCNが選択的にエッチングされ、結晶粒内にTiとAlの局所的な組成差が形成され、それが、安定化するために原子の再配列が起こり、組成の周期的な変化が生じ、その結果、硬さが向上することを見出した。
Further, during the film forming step, the reaction was temporarily stopped, and TiCl 4 : 2.0 to 5.0%, H 2 : remaining, reaction atmosphere pressure: 3.0 kPa, reaction atmosphere temperature: 800 to 900 ° C. By sandwiching a TiCl 4 etching step consisting of conditions for a predetermined number of times, (Ti 1-X Al X ) (C Y N 1 ) in the crystal having a cubic crystal structure of the cubic crystal phase of the composite carbonitride layer. A composite carbonitride layer of Ti and Al in which a periodic concentration change of Ti and Al of -Y ) is present is formed by vapor deposition.
By sandwiching the TiCl 4 etching process as described above in the film forming process, the cubic TiAlCN is selectively etched, and a local compositional difference between Ti and Al is formed in the crystal grains, which is stabilized. Therefore, it was found that the rearrangement of atoms occurred and the composition changed periodically, and as a result, the hardness was improved.
上記の化学蒸着法によって形成された複合炭窒化物層は、電子線後方散乱回折装置を用いて個々の結晶粒の結晶構造を、上記TiとAlの複合炭窒化物層の縦断面方向から解析した場合、立方晶結晶格子の電子線後方散乱回折像が観察される立方晶結晶相と六方晶結晶格子の電子線後方散乱回折像が観察される六方晶結晶相との混合組織からなり、かつ、複合炭窒化物層の縦断面方向の測定領域内において、電子線後方散乱回折像が観察された立方晶結晶相と六方晶結晶相との合計に占める六方晶結晶相の面積割合は10〜50面積%である。
さらに、上記混合組織中の六方晶結晶相の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、該測定傾斜角のうち、基体表面の法線方向に対して0〜90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して各区分内に存在する度数を集計した場合、2〜12度の範囲内の傾斜角区分に最高ピークが存在するとともに、該2〜12度の傾斜角区分に存在する度数の合計は、傾斜角度数分布における度数全体の40%以上である傾斜角度数分布形態が形成される。
The composite carbonitride layer formed by the above chemical vapor deposition method analyzes the crystal structure of each crystal grain from the longitudinal cross-sectional direction of the above composite carbonitride layer of Ti and Al using an electron beam backscattering diffractometer. A cubic crystal phase in which the electron beam backscatter diffraction image of the cubic crystal lattice is observed and a hexagonal crystal phase in which the electron beam backscatter diffraction image of the hexagonal crystal lattice is observed, and In the measurement region in the longitudinal section direction of the composite carbonitride layer, the area ratio of the hexagonal crystal phase to the total of the cubic crystal phase and the hexagonal crystal phase in which the electron backscatter diffraction image was observed is 10 to 10. 50 area%.
Further, the inclination angle formed by the normal line of the (0001) plane which is the crystal plane of the hexagonal crystal phase in the mixed structure is measured, and the measured inclination angle with respect to the normal direction of the substrate surface. When the measured inclination angle within the range of 0 to 90 degrees is divided into pitches of 0.25 degrees and the frequencies existing in each division are tabulated, the highest peak in the inclination angle classification within the range of 2 to 12 degrees , And the sum of the frequencies existing in the tilt angle section of 2 to 12 degrees forms a tilt angle number distribution form that is 40% or more of the entire frequencies in the tilt angle frequency distribution.
また、前記化学蒸着条件において、さらに蒸着条件を限定した蒸着を行うことによって、複合炭窒化物層中の立方晶結晶相を構成する結晶粒の平均アスペクト比αcが2未満、また、平均粒子幅ωcが0.3μm以下であり、また、六方晶結晶相を構成する結晶粒の平均アスペクト比αhが2以上、また、平均粒子幅ωhが0.1〜2μmとなる立方晶結晶相と六方晶結晶相との混合組織が形成される。
ここで、更に限定した蒸着条件とは、例えば、以下のとおりである。
反応ガス組成(容量%):
TiCl4 2.0〜2.5%、Al(CH3)3 3.0〜4.0%、
AlCl3 3.0〜4.0%、NH3 2.0〜5.0%、
N2 6.0〜10.0%、C2H4 0〜1.0%、残りH2、
反応雰囲気温度: 800〜900℃、
反応雰囲気圧力: 2〜3kPa、
Moreover, in the chemical vapor deposition conditions, by performing vapor deposition with further limited vapor deposition conditions, the average aspect ratio α c of the crystal grains constituting the cubic crystal phase in the composite carbonitride layer is less than 2, and the average particles Cubic crystals having a width ω c of 0.3 μm or less, a crystal grain constituting the hexagonal crystal phase having an average aspect ratio α h of 2 or more, and an average grain width ω h of 0.1 to 2 μm A mixed structure of phase and hexagonal crystal phase is formed.
Here, the more limited deposition conditions are, for example, as follows.
Reaction gas composition (volume%):
TiCl 4 2.0-2.5%, Al (CH 3 ) 3 3.0-4.0%,
AlCl 3 3.0~4.0%, NH 3 2.0~5.0 %,
N 2 6.0-10.0%, C 2 H 4 0-1.0%, remaining H 2 ,
Reaction atmosphere temperature: 800-900 ° C
Reaction atmosphere pressure: 2-3 kPa,
本発明の被覆工具は、複合炭窒化物層として、例えば、トリメチルアルミニウム(Al(CH3)3)を反応ガス成分として含有する化学蒸着法により、10〜50面積%の六方晶結晶相を含む立方晶結晶相と六方晶結晶相との混合組織からなる(Ti1−XAlX)(CYN1−Y)層を被覆形成し、さらに、該複合炭窒化物層中の六方晶結晶相の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た場合、基体表面の法線方向に対して2〜12度の範囲内の傾斜角区分に最高ピークが存在するとともに、該2〜12度の傾斜角区分に存在する度数の合計は、傾斜角度数分布における度数全体の40%以上を占めるような傾斜角度数分布形態を示すことから、複合炭窒化物層は、高い耐摩耗性を保ちつつ靭性が向上し、その結果、合金鋼の高速断続切削等の高速断続切削加工に用いた場合でも、長期の使用に亘って、すぐれた耐チッピング性、耐摩耗性を発揮するのである。 The coated tool of the present invention includes a hexagonal crystal phase of 10 to 50 area% as a composite carbonitride layer, for example, by chemical vapor deposition containing trimethylaluminum (Al (CH 3 ) 3 ) as a reaction gas component. A (Ti 1-X Al X ) (C Y N 1-Y ) layer composed of a mixed structure of a cubic crystal phase and a hexagonal crystal phase is formed to cover the hexagonal crystal in the composite carbonitride layer. When the inclination angle formed by the normal of the (0001) plane, which is the crystal plane of the phase crystal grain, is measured, the highest peak exists in the inclination angle section within the range of 2 to 12 degrees with respect to the normal direction of the substrate surface. In addition, since the sum of the frequencies existing in the tilt angle section of 2 to 12 degrees shows a tilt angle number distribution form that occupies 40% or more of the entire frequency in the tilt angle frequency distribution, the composite carbonitride layer Improves toughness while maintaining high wear resistance As a result, even when using a high-speed intermittent cutting work of high-speed interrupted cutting, etc. of alloy steel, over a long period of use, excellent chipping resistance is to exert wear resistance.
さらに、本発明では、上記蒸着をより限定した条件で行うことによって、立方晶結晶相と六方晶結晶相との混合組織からなる(Ti1−XAlX)(CYN1−Y)層において、各結晶相の結晶粒の平均粒子幅、平均アスペクト比を所定の数値範囲に定めた場合には、複合炭窒化物層の靭性を維持しつつ、より一段と、複合炭窒化物層の耐摩耗性向上を図ることができるのである。
さらに、本発明では、上記蒸着工程の際に、反応を一時停止し、TiCl4エッチング工程を所定回数挟むことにより、複合炭窒化物層の立方晶結晶相の結晶粒の立方晶構造を有する結晶内に(Ti1−XAlX)(CYN1−Y)のTiとAlの周期的な濃度変化が存在し、周期的に変化するXの極大値と極小値及び、周期を所定の数値範囲に定めた場合には、複合炭窒化物層の更なる硬さの向上と耐逃げ面摩耗性の向上を図ることができるのである。
Furthermore, in the present invention, a (Ti 1-X Al X ) (C Y N 1-Y ) layer composed of a mixed structure of a cubic crystal phase and a hexagonal crystal phase is performed by performing the above deposition under more limited conditions. However, when the average grain width and average aspect ratio of the crystal grains of each crystal phase are set within a predetermined numerical range, the composite carbonitride layer is further improved in durability while maintaining the toughness of the composite carbonitride layer. Abrasion can be improved.
Furthermore, in the present invention, in the vapor deposition step, the reaction is temporarily stopped, and the TiCl 4 etching step is sandwiched a predetermined number of times, whereby a crystal having a cubic crystal structure of cubic crystal phases of the composite carbonitride layer is obtained. (Ti 1-X Al X ) (C Y N 1-Y ) have a periodic concentration change of Ti and Al, and the cyclically changing local maximum and minimum values of X and the period are set to a predetermined value. When the value is set within the numerical range, it is possible to further improve the hardness and flank wear resistance of the composite carbonitride layer.
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、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、ISO・SEEN1203AFSNに規定するインサート形状をもったWC基超硬合金製の基体A〜Dをそれぞれ製造した。 As raw material powders, WC powder, TiC powder, ZrC powder, TaC powder, NbC powder, Cr 3 C 2 powder, and Co powder all having an average particle diameter of 1 to 3 μm were prepared. Then, after adding wax, ball mill mixing in acetone for 24 hours, drying under reduced pressure, press-molding into a green compact of a predetermined shape at a pressure of 98 MPa. Substrate A made of WC-based cemented carbide having an insert shape defined in ISO / SEEN1203AFSN after vacuum sintering under vacuum at a predetermined temperature in the range of 1370 to 1470 ° C. for 1 hour. ~ D were produced respectively.
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、ISO規格・SEEN1203AFSNのインサート形状をもったTiCN基サーメット製の基体a〜dを作製した。 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 sintering, a substrate made of TiCN-based cermet having an ISO standard / SEEN1203AFSN insert shape a -D were produced.
つぎに、これらの工具基体A〜Dおよび工具基体a〜dの表面に、通常の化学蒸着装置を用い、表3および表4に示される条件で、本発明の(Ti1−XAlX)(CYN1−Y)層を目標層厚で蒸着形成することにより、表6、表7に示される本発明被覆工具1〜15を製造した。
なお、本発明被覆工具6〜13については、表3に示される形成条件で、下部層および/または上部層を形成した。
Next, on the surfaces of these tool bases A to D and tool bases a to d, an ordinary chemical vapor deposition apparatus is used, and under the conditions shown in Tables 3 and 4, the (Ti 1-X Al X ) of the present invention is used. The present invention coated tools 1 to 15 shown in Tables 6 and 7 were manufactured by vapor-depositing a (C Y N 1-Y ) layer with a target layer thickness.
In addition, about this invention coated tools 6-13, the lower layer and / or the upper layer were formed on the formation conditions shown in Table 3.
また、比較の目的で、同じく工具基体A〜Dおよび工具基体a〜dの表面に、通常の化学蒸着装置を用い、表3および表5に示される条件で、比較例の(Ti1−xAlx)(CyN1−y)を目標層厚で蒸着形成することにより、表6、表8に示される比較例被覆工具1〜13を製造した。
なお、本発明被覆工具6〜13と同様に、比較被覆工具6〜13については、表3に示される形成条件で、下部層および/または上部層を形成した。
Further, for the purpose of comparison, an ordinary chemical vapor deposition apparatus was similarly used on the surfaces of the tool bases A to D and the tool bases a to d, and the conditions of the comparative examples (Ti 1-x Comparative example coated tools 1 to 13 shown in Tables 6 and 8 were manufactured by vapor-depositing Al x ) (C y N 1-y ) with a target layer thickness.
In addition, similarly to this invention coated tool 6-13, about the comparative coated tool 6-13, the lower layer and / or the upper layer were formed on the formation conditions shown in Table 3.
参考のため、工具基体Dおよび工具基体cの表面に、従来の物理蒸着装置を用いて、アークイオンプレーティングにより、参考例の(Ti1−XAlX)(CYN1−Y)層を目標層厚で蒸着形成することにより、表6、表8に示される参考例被覆工具14、15を製造した。
なお、アークイオンプレーティングの条件は、次のとおりである。
(a)上記工具基体Aおよびaを、アセトン中で超音波洗浄し、乾燥した状態で、アークイオンプレーティング装置内の回転テーブル上の中心軸から半径方向に所定距離離れた位置に外周部にそって装着し、また、カソード電極(蒸発源)として、所定組成のAl−Ti合金を配置し、
(b)まず、装置内を排気して10−2Pa以下の真空に保持しながら、ヒーターで装置内を500℃に加熱した後、前記回転テーブル上で自転しながら回転する工具基体に−1000Vの直流バイアス電圧を印加し、かつAl−Ti合金からなるカソード電極とアノード電極との間に200Aの電流を流してアーク放電を発生させ、装置内にAlおよびTiイオンを発生させ、もって工具基体表面をボンバード洗浄し、
(c)次に、装置内に反応ガスとして窒素ガスを導入して4Paの反応雰囲気とすると共に、前記回転テーブル上で自転しながら回転する工具基体に−50Vの直流バイアス電圧を印加し、かつ、上記Al−Ti合金からなるカソード電極(蒸発源)とアノード電極との間に120Aの電流を流してアーク放電を発生させ、前記工具基体の表面に、表8に示される目標平均組成、目標平均層厚の(Ti1−XAlX)(CYN1−Y)層を蒸着形成し、
参考例被覆工具14、15を製造した。
For reference, the surface of the tool substrate D and tool substrate c, using conventional physical vapor deposition apparatus, by arc ion plating, (Ti 1-X Al X ) of Reference Example (C Y N 1-Y) layer Were formed by vapor deposition with a target layer thickness, to produce reference example coated tools 14 and 15 shown in Tables 6 and 8.
The conditions for arc ion plating are as follows.
(A) The tool bases A and a are ultrasonically cleaned in acetone and dried, and in the outer peripheral portion at a predetermined distance in the radial direction from the central axis on the rotary table in the arc ion plating apparatus. Along with this, an Al-Ti alloy having a predetermined composition is arranged as a cathode electrode (evaporation source),
(B) First, the inside of the apparatus is evacuated and kept at a vacuum of 10 −2 Pa or less, the inside of the apparatus is heated to 500 ° C. with a heater, and then the tool base that rotates while rotating on the rotary table is −1000 V. A DC bias voltage is applied, and a current of 200 A is passed between a cathode electrode and an anode electrode made of an Al—Ti alloy to generate an arc discharge, thereby generating Al and Ti ions in the apparatus, thereby providing a tool base. Clean the surface with bombard,
(C) Next, nitrogen gas is introduced as a reaction gas into the apparatus to form a reaction atmosphere of 4 Pa, a DC bias voltage of −50 V is applied to the tool base that rotates while rotating on the rotary table, and A current of 120 A is passed between the cathode electrode (evaporation source) made of the Al—Ti alloy and the anode electrode to generate arc discharge, and the target average composition and target shown in Table 8 are formed on the surface of the tool base. the average layer thickness of (Ti 1-X Al X) (C Y N 1-Y) layer and the vapor deposited,
Reference Example Coated tools 14 and 15 were produced.
ついで、上記の本発明被覆工具1〜15の硬質被覆層について、硬質被覆層の各層の平均層厚、複合炭窒化物層の平均Al含有割合X、平均C含有割合Y、六方晶結晶相の占める面積割合Sh、六方晶結晶相の結晶粒の(0001)面の法線の測定傾斜角が、基体表面の法線に対して傾斜角区分2〜12度に存在する度数割合と最高ピークが存在する傾斜角区分、立方晶構造を有する結晶内に存在するTiとAlの濃度変化についてXの極大値と極小値の差、濃度変化の周期を測定した。 Next, for the hard coating layers of the present invention coated tools 1 to 15, the average thickness of each layer of the hard coating layer, the average Al content ratio X, the average C content ratio Y of the composite carbonitride layer, the hexagonal crystal phase Occupied area ratio S h , measured inclination angle of normal line of (0001) plane of crystal grains of hexagonal crystal phase, frequency ratio and highest peak existing in inclination angle category of 2 to 12 degrees with respect to normal line of substrate surface The difference between the maximum value and the minimum value of X and the period of concentration change were measured for the tilt angle section in which there is, the concentration change of Ti and Al present in the crystal having a cubic structure.
なお、具体的な測定は次のとおりである。
平均Al含有割合X、平均C含有割合Yの測定:
二次イオン質量分析(SIMS, Secondary-Ion-Mass-Spectroscopy) 装置を用いて、イオンビームを試料表面側から70μm×70μm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深さ方向の濃度測定を行った。平均Al含有割合X、平均C含有割合Yは深さ方向の平均値を示す。
The specific measurement is as follows.
Measurement of average Al content ratio X and average C content ratio Y:
Using a secondary ion mass spectrometry (SIMS) device, the ion beam is irradiated in the range of 70 μm × 70 μm from the sample surface side, and the concentration in the depth direction of the components emitted by the sputtering action Measurements were made. The average Al content ratio X and the average C content ratio Y indicate average values in the depth direction.
硬質被覆層の各層の平均層厚の測定:
走査型電子顕微鏡を用い断面測定を行い、硬質被覆層を構成する各層についてそれぞれ5ヶ所の層厚を測定し、平均値を求め、その平均値を硬質被覆層の平均層厚とした。
Measurement of the average layer thickness of each hard coating layer:
Cross-sectional measurement was performed using a scanning electron microscope, and the layer thickness of each of the five layers constituting the hard coating layer was measured to obtain an average value. The average value was taken as the average layer thickness of the hard coating layer.
六方晶結晶相の占める面積割合Shの測定:
電子線後方散乱回折装置を用いて、TiとAlの複合炭窒化物層からなる複合炭窒化物層の断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、0.1μm/stepの間隔で、電子線後方散乱回折像を測定し、個々の結晶粒の結晶構造を解析することで立方晶構造あるいは六方晶構造であるかを同定し、立方晶結晶相と六方晶結晶相との合計に占める六方晶結晶相の面積割合を求めた。
Measurement of the area ratio S h occupied by the hexagonal crystal phase:
Using an electron beam backscatter diffractometer, in a state where the cross-section of the composite carbonitride layer composed of a composite carbonitride layer of Ti and Al is a polished surface, set in a lens barrel of a field emission scanning electron microscope, An electron beam with an acceleration voltage of 15 kV at an incident angle of 70 degrees is irradiated onto the polished surface with an irradiation current of 1 nA, and each crystal grain existing within the measurement range of the cross-sectional polished surface is irradiated at intervals of 0.1 μm / step. Measure the electron backscatter diffraction image and analyze the crystal structure of each crystal grain to identify whether it is a cubic or hexagonal crystal structure. The area ratio of the occupied hexagonal crystal phase was determined.
六方晶結晶相の結晶粒の(0001)面の法線の測定傾斜角が、基体表面の法線に対して傾斜角区分2〜12度に存在する度数割合の測定:
複合炭窒化物層中の六方晶結晶相を構成する結晶粒について、電界放出型走査電子顕微鏡と電子線後方散乱回折装置を用いて基体表面の法線方向に対する六方晶結晶相の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、該測定傾斜角のうち、基体表面の法線方向に対して0〜90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して各区分内に存在する度数を集計し、最高ピークが存在する傾斜角区分を求めるとともに、2〜12度の傾斜角区分に存在する度数の合計を求め、該2〜12度の傾斜角区分に存在する度数の合計が傾斜角度数分布全体に占める度数割合を求めた。
Measurement of frequency ratio in which the measurement inclination angle of the normal line of the (0001) plane of the crystal grains of the hexagonal crystal phase is present in the inclination angle section of 2 to 12 degrees with respect to the normal line of the substrate surface:
About the crystal grains constituting the hexagonal crystal phase in the composite carbonitride layer, the crystal grains of the hexagonal crystal phase with respect to the normal direction of the substrate surface using a field emission scanning electron microscope and an electron beam backscatter diffractometer The tilt angle formed by the normal line of the (0001) plane, which is a plane, is measured, and the measured tilt angle within the range of 0 to 90 degrees with respect to the normal direction of the substrate surface is 0.25 of the measured tilt angle. The number of degrees existing in each section is tabulated for each degree pitch, and the inclination angle section where the highest peak exists is obtained, and the total of the frequencies existing in the inclination angle section of 2 to 12 degrees is obtained. The frequency ratio that the total of the frequencies existing in the inclination angle section of ˜12 degrees occupies the entire inclination angle frequency distribution was determined.
さらに、複合炭窒化物層中の立方晶結晶相の各結晶粒について、基体表面と平行な方向の粒子幅Wc、基体表面に垂直な方向の粒子長さLcを測定し、各結晶粒のアスペクト比Ac(=Lc/Wc)を算出するとともに、個々の結晶粒について求めたアスペクト比Acの平均値を平均アスペクト比αcとして算出し、また、個々の結晶粒について求めた粒子幅Wcの平均値を平均粒子幅ωcとして算出した。
同様にして、複合炭窒化物層中の六方晶結晶相の各結晶粒について、基体表面と平行な方向の粒子幅Wh、基体表面に垂直な方向の粒子長さLhを測定し、各結晶粒のアスペクト比Ah(=Lh/Wh)を算出するとともに、個々の結晶粒について求めたアスペクト比Ahの平均値を平均アスペクト比αhとして算出し、また、個々の結晶粒について求めた粒子幅Whの平均値を平均粒子幅ωhとして算出した。
ここで、Wc、Lc、Wh、Lhの測定は、以下のように行った。
TiとAlの複合炭窒化物層からなる複合炭窒化物層の断面を研磨面とした状態で、複合炭窒化物層中の結晶粒について、走査電子顕微鏡(倍率20000倍)を用いて幅10μmに亘って複数視野観察し、個々の結晶粒についてWc、Lc、Wh、Lhを測定した。
表7に、これらの値を示す。
Further, for each crystal grain of the cubic crystal phase in the composite carbonitride layer, the particle width W c in the direction parallel to the substrate surface and the particle length L c in the direction perpendicular to the substrate surface are measured. The aspect ratio A c (= L c / W c ) was calculated, the average value of the aspect ratios A c obtained for the individual crystal grains was calculated as the average aspect ratio α c , and the individual crystal grains were obtained. and the average value of the particle width W c is calculated as the average particle width omega c.
Similarly, for each crystal grain of the hexagonal crystal phase in the composite carbonitride layer, the particle width W h in the direction parallel to the substrate surface and the particle length L h in the direction perpendicular to the substrate surface are measured, The aspect ratio A h (= L h / W h ) of the crystal grains is calculated, the average value of the aspect ratio A h obtained for each crystal grain is calculated as the average aspect ratio α h , and the individual crystal grains The average value of the particle widths W h obtained for was calculated as the average particle width ω h .
Here, W c, L c, W h, the measurement of L h was performed as follows.
With the cross section of the composite carbonitride layer composed of the composite carbonitride layer of Ti and Al as a polished surface, the crystal grains in the composite carbonitride layer are 10 μm wide using a scanning electron microscope (magnification 20000 times). A plurality of visual fields were observed, and W c , L c , W h , and L h were measured for each crystal grain.
Table 7 shows these values.
立方晶構造を有する結晶内に存在するTiとAlの濃度変化:
さらに、透過型電子顕微鏡(倍率200000倍)を用いて、複合炭窒化物層の微小領域の観察を行い、エネルギー分散型X線分光法(EDS)を用いて、断面側から組成分析を行ったところ、複合炭窒化物層中の立方晶構造を有する結晶内にTiとAlの周期的な濃度変化が観察され、Xが相対的に大きい領域と小さい領域が存在した。複合炭窒化物層中の立方晶構造を有する結晶のTiとAlの周期的な濃度変化が存在する結晶の中の5個の結晶について、Xが相対的に大きい領域と小さい領域の周期的な濃度変化の存在する方向に線分析を行い、測定した結晶のXの極大値と極小値のそれぞれの平均をとることで、Xが相対的に大きい領域と小さい領域のそれぞれの平均組成を求め、その差を測定した結晶のXの極大値と極小値の差として求め、測定した5個の結晶について平均することで、Xの極大値と極小値の差の平均値を求めた。同様に、複合炭窒化物層中の立方晶構造を有する結晶のTiとAlの周期的な濃度変化が存在する結晶の中の5個の結晶について、上記線分析の結果から、Xが相対的に大きい領域の距離の平均を算出することで、測定した結晶のTiとAlの濃度変化の周期を求め、測定した5個の結晶について平均することで、TiとAlの濃度変化の周期の平均値を求めた。
Change in concentration of Ti and Al present in a crystal having a cubic structure:
Furthermore, the micro area | region of the composite carbonitride layer was observed using the transmission electron microscope (magnification 200000 times), and the compositional analysis was performed from the cross section side using the energy dispersive X-ray spectroscopy (EDS). However, periodic concentration changes of Ti and Al were observed in the crystal having a cubic structure in the composite carbonitride layer, and there were a region where X was relatively large and a region where X was relatively small. For five crystals in the crystal having a cubic structure in the composite carbonitride layer in which periodic concentration changes of Ti and Al exist, periodicity of a region where X is relatively large and a region where X is relatively small By performing line analysis in the direction in which the concentration change exists, and taking the average of the maximum and minimum values of X of the measured crystal, the average composition of each of the regions where X is relatively large and small is obtained, The difference was obtained as the difference between the maximum value and the minimum value of X of the measured crystal, and the average value of the difference between the maximum value and the minimum value of X was determined by averaging the measured five crystals. Similarly, from the results of the above line analysis, X is a relative value for five of the crystals having a periodic concentration change of Ti and Al in the composite carbonitride layer having a cubic structure. By calculating the average of the distance of the large area, the period of change in the concentration of Ti and Al in the measured crystal was obtained, and the average of the period of change in the concentration of Ti and Al was obtained by averaging over the five measured crystals. The value was determined.
ついで、比較例被覆工具1〜13および参考例被覆工具14、15のそれぞれについても、本発明被覆工具1〜15と同様にして、平均Al含有割合X、平均C含有割合Y、硬質被覆層の平均層厚t、六方晶結晶相の占める面積割合Sh、六方晶結晶相の結晶粒の(0001)面の法線の測定傾斜角が、基体表面の法線に対して傾斜角区分2〜12度に存在する度数割合と最高ピークが存在する傾斜角区分を測定した。
さらに、Wc、Lc、Wh、Lhを測定するとともに、αc、ωc、αh、ωhを算出した。
表8に、これらの値を示す。
Next, for each of the comparative example coated tools 1 to 13 and the reference example coated tools 14 and 15, similarly to the present coated tools 1 to 15, the average Al content ratio X, the average C content ratio Y, and the hard coating layer The average layer thickness t, the area ratio S h occupied by the hexagonal crystal phase, and the measured tilt angle of the normal line of the (0001) plane of the crystal grains of the hexagonal crystal phase are 2 The frequency ratio existing at 12 degrees and the inclination angle section where the highest peak exists were measured.
Furthermore, W c , L c , W h , and L h were measured, and α c , ω c , α h , and ω h were calculated.
Table 8 shows these values.
つぎに、上記の各種の被覆工具をいずれもカッタ径125mmの工具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1〜15、比較例被覆工具1〜13および参考例被覆工具14、15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た。
被削材: JIS・SCM440幅100mm、長さ400mmのブロック材
回転速度: 943 min−1、
切削速度: 370 m/min、
切り込み: 1.2 mm、
一刃送り量: 0.10 mm/刃、
切削時間: 8分、
表9に、上記切削試験の結果を示す。
Next, in the state where each of the above various coated tools is clamped to the tool steel cutter tip portion having a cutter diameter of 125 mm by a fixing jig, the present coated tools 1 to 15, the comparative coated tools 1 to 13, and the reference Example For the coated tools 14 and 15, the following dry high-speed face milling, which is a kind of high-speed intermittent cutting of alloy steel, and a center-cut cutting test were performed, and the flank wear width of the cutting edge was measured.
Work material: Block material of JIS / SCM440 width 100mm, length 400mm
Rotational speed: 943 min −1 ,
Cutting speed: 370 m / min,
Cutting depth: 1.2 mm,
Single blade feed amount: 0.10 mm / tooth,
Cutting time: 8 minutes,
Table 9 shows the results of the cutting test.
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10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α〜ε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 and Co powder all having an average particle diameter of 1 to 3 μm are prepared as raw material powders. The powder was blended into the blending composition shown in Table 10, added with wax, ball mill mixed in acetone for 24 hours, dried under reduced pressure, and then press-molded into a compact of a predetermined shape at a pressure of 98 MPa. The powder is sintered in a vacuum of 5 Pa at a predetermined temperature within a range of 1370 to 1470 ° C. for 1 hour, and after sintering, the cutting edge is subjected to a honing process of R: 0.07 mm. Thus, tool bases α to ε made of a WC-base cemented carbide having an insert shape of ISO standard CNMG120212 were manufactured.
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11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:0.09mmのホーニング加工を施すことによりISO規格・CNMG120412のインサート形状をもったTiCN基サーメット製の工具基体ζ〜κ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 were prepared, and these raw material powders were blended into the blending composition shown in Table 11, wet mixed by a ball mill for 24 hours, dried, and then 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. After sintering, the cutting edge portion was subjected to a honing process of R: 0.09 mm. Tool bases ζ to κ made of TiCN-based cermet having a standard / CNMG12041 insert shape were formed.
つぎに、これらの工具基体α〜εおよび工具基体ζ〜κの表面に、通常の化学蒸着装置を用い、表3および表4に示される条件で、本発明の(Ti1−XAlX)(CYN1−Y)層を目標層厚で蒸着形成することにより、表12、表13に示される本発明被覆工具16〜30を製造した。
なお、本発明被覆工具19〜28については、表3に示される形成条件で、下部層および/または上部層を形成した。
Next, on the surfaces of these tool bases α to ε and tool bases ζ to κ, a normal chemical vapor deposition apparatus is used, and (Ti 1-X Al X ) of the present invention is used under the conditions shown in Tables 3 and 4. The present invention coated tools 16 to 30 shown in Tables 12 and 13 were manufactured by vapor-depositing (C Y N 1-Y ) layers at a target layer thickness.
In addition, about this invention coated tools 19-28, the lower layer and / or the upper layer were formed on the formation conditions shown in Table 3.
また、比較の目的で、同じく工具基体α〜εおよび工具基体ζ〜κの表面に、通常の化学蒸着装置を用い、表3および表5に示される条件で、比較例の(Ti1−xAlx)(CyN1−y)を目標層厚で蒸着形成することにより、表12、表14に示される比較例被覆工具16〜28を製造した。
なお、本発明被覆工具19〜28と同様に、比較被覆工具19〜28については、表3に示される形成条件で、下部層および/または上部層を形成した。
Further, for the purpose of comparison, an ordinary chemical vapor deposition apparatus was used on the surfaces of the tool bases α to ε and the tool bases ζ to κ, and under the conditions shown in Tables 3 and 5, (Ti 1-x Comparative example coated tools 16 to 28 shown in Tables 12 and 14 were manufactured by vapor-depositing Al x ) (C y N 1-y ) with a target layer thickness.
In addition, similarly to this invention coated tool 19-28, about the comparison coated tool 19-28, the lower layer and / or the upper layer were formed on the formation conditions shown by Table 3. FIG.
参考のため、工具基体βおよび工具基体θの表面に、従来の物理蒸着装置を用いて、アークイオンプレーティングにより、参考例の(Ti1−XAlX)(CYN1−Y)層を目標層厚で蒸着形成することにより、表12、表14に示される参考例被覆工具29、30を製造した。
なお、アークイオンプレーティングの条件は、実施例1に示される条件と同様の条件を用い、前記工具基体の表面に、表14に示される目標平均組成、目標平均層厚の(Ti1−XAlX)(CYN1−Y)層を蒸着形成し、参考例被覆工具29、30を製造した。
For reference, the (Ti 1-X Al X ) (C Y N 1-Y ) layer of the reference example is formed on the surfaces of the tool base β and the tool base θ by arc ion plating using a conventional physical vapor deposition apparatus. Were formed by vapor deposition with a target layer thickness to produce reference example-coated tools 29 and 30 shown in Tables 12 and 14.
The arc ion plating conditions are the same as the conditions shown in Example 1, and the target average composition and target average layer thickness (Ti 1-X shown in Table 14) are formed on the surface of the tool base. The Al X ) (C Y N 1-Y ) layer was formed by vapor deposition, and Reference Example-coated tools 29 and 30 were produced.
ついで、上記の本発明被覆工具16〜30の硬質被覆層について、実施例1に示される方法と同様の方法を用いて、硬質被覆層の各層の平均層厚、複合炭窒化物層の平均Al含有割合X、平均C含有割合Y、六方晶結晶相の占める面積割合Sh、六方晶結晶相の結晶粒の(0001)面の法線の測定傾斜角が、基体表面の法線に対して傾斜角区分2〜12度に存在する度数割合と最高ピークが存在する傾斜角区分を測定した。
また、複合炭窒化物層中の立方晶結晶相の各結晶粒について、Wc、Lc、Ac(=Lc/Wc)、αc、ωcを測定・算出し、さらに、複合炭窒化物層中の六方晶結晶相の各結晶粒について、Wh、Lh、Ah(=Lh/Wh)、αh、ωhを測定・算出した。
表13に、その結果を示す。
Next, with respect to the hard coating layers of the above-described coated tools 16 to 30 of the present invention, using the same method as shown in Example 1, the average layer thickness of each layer of the hard coating layer, the average Al of the composite carbonitride layer The content ratio X, the average C content ratio Y, the area ratio S h occupied by the hexagonal crystal phase, and the measured inclination angle of the normal line of the (0001) plane of the crystal grains of the hexagonal crystal phase are relative to the normal line of the substrate surface The frequency ratio existing in the inclination angle section of 2 to 12 degrees and the inclination angle section where the highest peak exists were measured.
In addition, W c , L c , A c (= L c / W c ), α c , and ω c are measured and calculated for each crystal grain of the cubic crystal phase in the composite carbonitride layer. For each crystal grain of the hexagonal crystal phase in the carbonitride layer, W h , L h , A h (= L h / W h ), α h , and ω h were measured and calculated.
Table 13 shows the results.
ついで、比較例被覆工具16〜28および参考例被覆工具29、30についても、本発明被覆工具16〜30と同様にして、硬質被覆層の各層の平均層厚、複合炭窒化物層の平均Al含有割合X、平均C含有割合Y、六方晶結晶相の占める面積割合Sh、六方晶結晶相の結晶粒の(0001)面の法線の測定傾斜角が、基体表面の法線に対して傾斜角区分2〜12度に存在する度数割合と最高ピークが存在する傾斜角区分、複合炭窒化物層中の立方晶結晶相の各結晶粒のWc、Lc、Ac(=Lc/Wc)、αc、ωc、また、複合炭窒化物層中の六方晶結晶相の各結晶粒について、Wh、Lh、Ah(=Lh/Wh)、αh、ωhを測定・算出した。
表14に、その結果を示す。
Subsequently, the comparative example coated tools 16 to 28 and the reference example coated tools 29 and 30 were similarly processed in the same manner as the coated tools 16 to 30 of the present invention, with the average layer thickness of each layer of the hard coating layer and the average Al of the composite carbonitride layer. The content ratio X, the average C content ratio Y, the area ratio S h occupied by the hexagonal crystal phase, and the measured inclination angle of the normal line of the (0001) plane of the crystal grains of the hexagonal crystal phase are relative to the normal line of the substrate surface W c , L c , A c (= L c) of each crystal grain in the cubic crystal phase in the composite carbonitride layer, the tilt angle section having the highest peak and the frequency ratio existing in the tilt angle section of 2 to 12 degrees / W c ), α c , ω c , and for each crystal grain of the hexagonal crystal phase in the composite carbonitride layer, W h , L h , A h (= L h / W h ), α h , ω h was measured and calculated.
Table 14 shows the results.
つぎに、前記各種の被覆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、本発明被覆工具16〜30、比較被覆工具16〜28および参考被覆工具29,30について、以下に示す、炭素鋼の乾式高速断続切削試験、鋳鉄の湿式高速断続切削試験を実施し、いずれも切刃の逃げ面摩耗幅を測定した。
切削条件2:
被削材:JIS・SCM435の長さ方向等間隔4本縦溝入り丸棒、
切削速度:350m/min、
切り込み:1.2mm、
送り:0.2mm/rev、
切削時間:5分、
(通常の切削速度は、220m/min)、
切削条件3:
被削材:JIS・FCD450の長さ方向等間隔4本縦溝入り丸棒、
切削速度:340m/min、
切り込み:1.0mm、
送り:0.2mm/rev、
切削時間:5分、
(通常の切削速度は、200m/min)、
表15に、前記切削試験の結果を示す。
Next, in the state where each of the various coated tools is screwed to the tip of the tool steel tool with a fixing jig, the present coated tools 16 to 30, comparative coated tools 16 to 28, and reference coated tools 29, About 30, the dry high speed intermittent cutting test of the carbon steel and the wet high speed intermittent cutting test of cast iron which were shown below were implemented, and all measured the flank wear width of the cutting edge.
Cutting condition 2:
Work material: JIS / SCM435 lengthwise equally spaced 4 rods with vertical grooves,
Cutting speed: 350 m / min,
Cutting depth: 1.2mm,
Feed: 0.2mm / rev,
Cutting time: 5 minutes
(Normal cutting speed is 220 m / min),
Cutting condition 3:
Work material: JIS / FCD450 lengthwise equidistant round bars with 4 vertical grooves,
Cutting speed: 340 m / min,
Cutting depth: 1.0 mm,
Feed: 0.2mm / rev,
Cutting time: 5 minutes
(Normal cutting speed is 200 m / min),
Table 15 shows the results of the cutting test.
原料粉末として、いずれも0.5〜4μmの範囲内の平均粒径を有するcBN粉末、TiN粉末、TiCN粉末、TiC粉末、Al粉末、Al2O3粉末を用意し、これら原料粉末を表16に示される配合組成に配合し、ボールミルで80時間湿式混合し、乾燥した後、120MPaの圧力で直径:50mm×厚さ:1.5mmの寸法をもった圧粉体にプレス成形し、ついでこの圧粉体を、圧力:1Paの真空雰囲気中、900〜1300℃の範囲内の所定温度に60分間保持の条件で焼結して切刃片用予備焼結体とし、この予備焼結体を、別途用意した、Co:8質量%、WC:残りの組成、並びに直径:50mm×厚さ:2mmの寸法をもったWC基超硬合金製支持片と重ね合わせた状態で、通常の超高圧焼結装置に装入し、通常の条件である圧力:4GPa、温度:1200〜1400℃の範囲内の所定温度に保持時間:0.8時間の条件で超高圧焼結し、焼結後上下面をダイヤモンド砥石を用いて研磨し、ワイヤー放電加工装置にて所定の寸法に分割し、さらにCo:5質量%、TaC:5質量%、WC:残りの組成およびISO規格CNGA120412の形状(厚さ:4.76mm×内接円直径:12.7mmの80°菱形)をもったWC基超硬合金製インサート本体のろう付け部(コーナー部)に、体積%で、Zr:37.5%、Cu:25%、Ti:残りからなる組成を有するTi−Zr−Cu合金のろう材を用いてろう付けし、所定寸法に外周加工した後、切刃部に幅:0.13mm、角度:25°のホーニング加工を施し、さらに仕上げ研摩を施すことによりISO規格CNGA120412のインサート形状をもった工具基体イ〜ニをそれぞれ製造した。 As the raw material powder, cBN powder, TiN powder, TiCN powder, TiC powder, Al powder, and Al 2 O 3 powder each having an average particle diameter in the range of 0.5 to 4 μm are prepared. The mixture is blended in the composition shown in FIG. 1, wet mixed with a ball mill for 80 hours, dried, and then pressed into a green compact having a diameter of 50 mm × thickness: 1.5 mm under a pressure of 120 MPa. The green compact is sintered in a vacuum atmosphere at a pressure of 1 Pa at a predetermined temperature within a range of 900 to 1300 ° C. for 60 minutes to obtain a presintered body for a cutting edge piece. In addition, Co: 8% by mass, WC: remaining composition, and diameter: 50 mm × thickness: 2 mm, superposed on a WC-based cemented carbide support piece with a normal super-high pressure Insert into the sintering machine, normal conditions A certain pressure: 4 GPa, temperature: 1200 ° C. to 1400 ° C. within a predetermined temperature, holding time: 0.8 hour sintering, and after sintering, the upper and lower surfaces are polished with a diamond grindstone, and wire discharge It is divided into predetermined dimensions by a processing device, and further Co: 5 mass%, TaC: 5 mass%, WC: remaining composition and ISO standard CNGA1204112 shape (thickness: 4.76 mm × inscribed circle diameter: 12. The brazing part (corner part) of the insert body made of a WC-based cemented carbide with a 7 mm 80 ° rhombus) has a composition consisting of Zr: 37.5%, Cu: 25%, Ti: the rest in volume%. After brazing using a brazing material of Ti-Zr-Cu alloy and having a predetermined dimension, the cutting edge is subjected to honing with a width of 0.13 mm and an angle of 25 °, followed by finishing polishing. ISO regulations The tool substrate (a) to (k) two having the insert shape of CNGA120412 were produced, respectively.
つぎに、これらの工具基体イ〜ニの表面に、通常の化学蒸着装置を用い、表3および表4に示される条件で、本発明の(Ti1−XAlX)(CYN1−Y)層を目標層厚で蒸着形成することにより、表17、表18に示される本発明被覆工具31〜40を製造した。
なお、本発明被覆工具34〜38については、表3に示される形成条件で、下部層および/または上部層を形成した。
Then, these tool substrate i ~ the surface of the two, using a conventional chemical vapor deposition apparatus under the conditions shown in Table 3 and Table 4, the present invention (Ti 1-X Al X) (C Y N 1- Y ) The present coated tools 31 to 40 shown in Tables 17 and 18 were manufactured by vapor-depositing layers with a target layer thickness.
In addition, about this invention coated tools 34-38, the lower layer and / or the upper layer were formed on the formation conditions shown in Table 3.
また、比較の目的で、同じく工具基体イ〜ニの表面に、通常の化学蒸着装置を用い、表4に示される条件で、比較例の(Ti1−xAlx)(CyN1−y)を目標層厚で蒸着形成することにより、表17、表19に示される比較例被覆工具31〜38を製造した。
なお、本発明被覆工具34〜38と同様に、比較被覆工具34〜38については、表3に示される形成条件で、下部層および/または上部層を形成した。
For the purpose of comparison, the same tool substrate i ~ the surface of the two, using a conventional chemical vapor deposition apparatus under the conditions shown in Table 4, (Ti 1-x Al x) of Comparative Example (C y N 1- Comparative example-coated tools 31 to 38 shown in Tables 17 and 19 were manufactured by vapor-depositing y ) with a target layer thickness.
In addition, similarly to this invention coating tool 34-38, about the comparison coating tool 34-38, the lower layer and / or the upper layer were formed on the formation conditions shown in Table 3.
参考のため、工具基体イおよび工具基体ロの表面に、従来の物理蒸着装置を用いて、アークイオンプレーティングにより、参考例の(Ti1−XAlX)(CYN1−Y)層を目標層厚で蒸着形成することにより、表17、表19に示される参考例被覆工具39、40を製造した。
なお、アークイオンプレーティングの条件は、実施例1に示される条件と同様の条件を用い、前記工具基体の表面に、表19に示される目標平均組成、目標平均層厚の(Ti1−XAlX)(CYN1−Y)層を蒸着形成し、参考例被覆工具39、40を製造した。
For reference, the (Ti 1-X Al X ) (C Y N 1-Y ) layer of the reference example is formed on the surfaces of the tool base A and the tool base B by arc ion plating using a conventional physical vapor deposition apparatus. Were formed by vapor deposition with a target layer thickness to produce reference example coated tools 39 and 40 shown in Tables 17 and 19.
The arc ion plating conditions are the same as the conditions shown in Example 1, and the target average composition and target average layer thickness (Ti 1-X shown in Table 19) are formed on the surface of the tool base. The Al X ) (C Y N 1-Y ) layer was formed by vapor deposition to produce reference example coated tools 39 and 40.
ついで、上記の本発明被覆工具31〜40の硬質被覆層について、実施例1に示される方法と同様の方法を用いて、複合炭窒化物層の平均Al含有割合X、平均C含有割合Y、硬質被覆層の平均層厚t、六方晶結晶相の占める面積割合Sh、六方晶結晶相の結晶粒の(0001)面の法線の測定傾斜角が、基体表面の法線に対して傾斜角区分2〜12度に存在する度数割合と最高ピークが存在する傾斜角区分を測定した。
また、複合炭窒化物層中の立方晶結晶相の各結晶粒について、Wc、Lc、Ac(=Lc/Wc)、αc、ωcを測定・算出し、さらに、複合炭窒化物層中の六方晶結晶相の各結晶粒について、Wh、Lh、Ah(=Lh/Wh)、αh、ωhを測定・算出した。
表18に、その結果を示す。
Next, with respect to the hard coating layers of the present invention-coated tools 31 to 40, using the same method as the method shown in Example 1, the average Al content ratio X, the average C content ratio Y of the composite carbonitride layer, The average thickness t of the hard coating layer, the area ratio S h occupied by the hexagonal crystal phase, and the measured inclination angle of the normal line of the (0001) plane of the crystal grains of the hexagonal crystal phase are inclined with respect to the normal line of the substrate surface The frequency ratio existing in the angle section of 2 to 12 degrees and the tilt angle section where the highest peak exists were measured.
In addition, W c , L c , A c (= L c / W c ), α c , and ω c are measured and calculated for each crystal grain of the cubic crystal phase in the composite carbonitride layer. For each crystal grain of the hexagonal crystal phase in the carbonitride layer, W h , L h , A h (= L h / W h ), α h , and ω h were measured and calculated.
Table 18 shows the results.
ついで、比較例被覆工具31〜38および参考例被覆工具39、40についても、本発明被覆工具31〜40と同様にして、複合炭窒化物層の平均Al含有割合X、平均C含有割合Y、硬質被覆層の平均層厚t、六方晶結晶相の占める面積割合Sh、六方晶結晶相の結晶粒の(0001)面の法線の測定傾斜角が、基体表面の法線に対して傾斜角区分2〜12度に存在する度数割合と最高ピークが存在する傾斜角区分、複合炭窒化物層中の立方晶結晶相の各結晶粒のWc、Lc、Ac(=Lc/Wc)、αc、ωc、また、複合炭窒化物層中の六方晶結晶相の各結晶粒について、Wh、Lh、Ah(=Lh/Wh)、αh、ωhを測定・算出した。
表19に、その結果を示す。
Next, for the comparative example coated tools 31 to 38 and the reference example coated tools 39 and 40, the average Al content ratio X, the average C content ratio Y of the composite carbonitride layer, as in the present invention coated tools 31 to 40, The average thickness t of the hard coating layer, the area ratio S h occupied by the hexagonal crystal phase, and the measured inclination angle of the normal line of the (0001) plane of the crystal grains of the hexagonal crystal phase are inclined with respect to the normal line of the substrate surface tilt angle sections power ratio and the highest peak present at the corner segment 2-12 degrees exists, of each crystal grain cubic crystalline phase of the composite carbonitride layer W c, L c, a c (= L c / W c ), α c , ω c , and for each crystal grain of the hexagonal crystal phase in the composite carbonitride layer, W h , L h , A h (= L h / W h ), α h , ω h was measured and calculated.
Table 19 shows the results.
つぎに、上記の各種の被覆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、本発明被覆工具31〜40、比較例被覆工具31〜38および参考例被覆工具39、40について、以下に示す、浸炭焼入れ合金鋼の乾式高速断続切削加工試験を実施し、切刃の逃げ面摩耗幅を測定した。
被削材: JIS・SCr420(硬さ:HRC60)の長さ方向等間隔4本縦溝入り丸棒、
切削速度: 220 m/min、
切り込み: 0.10 mm、
送り: 0.10mm/rev、
切削時間: 4分、
表20に、上記切削試験の結果を示す。
Next, the coated tools 31 to 40 of the present invention, the comparative coated tools 31 to 38, and the reference example coated with the above various coated tools screwed to the tip of the tool steel tool with a fixing jig. About the tools 39 and 40, the dry high-speed intermittent cutting test of the carburizing hardening alloy steel shown below was implemented, and the flank wear width of the cutting edge was measured.
Work material: JIS · SCr420 (Hardness: HRC60) lengthwise equidistant 4 round bars with longitudinal grooves,
Cutting speed: 220 m / min,
Cutting depth: 0.10 mm,
Feed: 0.10mm / rev,
Cutting time: 4 minutes
Table 20 shows the results of the cutting test.
表6〜9、表12〜15および表17〜20に示される結果から、本発明被覆工具1〜40は、立方晶結晶相と六方晶結晶相との混合組織からなる(Ti1−XAlX)(CYN1−Y)層が蒸着形成され、しかも、該層は、高い耐摩耗性を保ちつつ靭性が向上していることから、合金鋼の高速ミーリング切削加工または外径高速断続切削加工ですぐれた密着性、潤滑性、耐チッピング性、耐摩耗性を発揮する。
特に、本発明被覆工具4〜7、9〜15、19〜22、24〜30、34〜38、40については、立方晶結晶相と六方晶結晶相の各結晶粒の平均粒子幅、平均アスペクト比を所定の数値範囲にあることから、さらに、より一段と耐摩耗性が向上する。
これに対して、比較例被覆工具1〜13、16〜28、31〜38および参考例被覆工具14、15、29、30、39、40については、いずれも、硬質被覆層にチッピング、欠損、剥離等の異常損傷が発生するばかりか、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 6-9, Tables 12-15, and Tables 17-20, the coated tools 1-40 of the present invention are composed of a mixed structure of a cubic crystal phase and a hexagonal crystal phase (Ti 1-X Al X ) ( CY N 1-Y ) layer is formed by vapor deposition, and the layer is improved in toughness while maintaining high wear resistance. Exhibits excellent adhesion, lubricity, chipping resistance, and wear resistance in cutting.
Especially about this invention coated tool 4-7, 9-15, 19-22, 24-30, 34-38, 40, the average grain width of each crystal grain of a cubic crystal phase and a hexagonal crystal phase, an average aspect Since the ratio is in the predetermined numerical range, the wear resistance is further improved.
On the other hand, as for the comparative example coated tools 1-13, 16-28, 31-38 and the reference example coated tools 14, 15, 29, 30, 39, 40, all are chipped, chipped, It is clear that not only abnormal damage such as peeling occurs but also 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、合金鋼の高速ミーリング切削加工等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 tool of the present invention can be used not only for high-speed intermittent cutting such as high-speed milling cutting of alloy steel but also as a coating tool for various work materials, and for long-term use. Since it exhibits excellent wear resistance, it can satisfactorily respond to higher performance of cutting equipment, labor saving and energy saving of cutting, and cost reduction.
Claims (4)
(a)上記硬質被覆層は、平均層厚1〜20μmのTiとAlの複合炭窒化物層を少なくとも含み、その平均組成を、
組成式:(Ti1−XAlX)(CYN1−Y)
で表した場合、Al含有割合XおよびC含有割合Y(但し、X、Yは何れも原子比)は、それぞれ、0.60≦X≦0.95、0.0005≦Y≦0.005を満足し、
(b)上記複合炭窒化物層は、電子線後方散乱回折装置を用いて個々の結晶粒の結晶構造を、上記TiとAlの複合炭窒化物層の縦断面方向から解析した場合、立方晶結晶格子の電子線後方散乱回折像が観察される立方晶結晶相と六方晶結晶格子の電子線後方散乱回折像が観察される六方晶結晶相との混合組織からなり、かつ、立方晶結晶相と六方晶結晶相との合計に占める六方晶結晶相の面積割合は10〜50面積%であり、
(c)基体表面の法線方向に対する上記複合炭窒化物層の六方晶結晶相の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、該測定傾斜角のうち、基体表面の法線方向に対して0〜90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して各区分内に存在する度数を集計した場合、2〜12度の範囲内の傾斜角区分に最高ピークが存在するとともに、該2〜12度の傾斜角区分に存在する度数の合計は、傾斜角度数分布における度数全体の40%以上であることを特徴とする表面被覆切削工具。 A surface-coated cutting tool in which a hard coating layer is coated on the surface of a substrate composed of any of tungsten carbide-based cemented carbide, titanium carbonitride-based cermet, or cubic boron nitride-based ultrahigh-pressure sintered body. ,
(A) the hard coating layer comprises at least a complex carbonitride layer of Ti and Al flat HitoshisoAtsu 1 to 20 [mu] m, the average composition,
Formula: (Ti 1-X Al X ) (C Y N 1-Y)
In this case, the Al content ratio X and the C content ratio Y (where X and Y are atomic ratios) satisfy 0.60 ≦ X ≦ 0.95 and 0.0005 ≦ Y ≦ 0.005, respectively. Satisfied,
(B) When the composite carbonitride layer is analyzed from the longitudinal cross-sectional direction of the composite carbonitride layer of Ti and Al using an electron beam backscattering diffractometer, the crystal structure of each crystal grain is cubic. It consists of a mixed structure of a cubic crystal phase in which an electron beam backscatter diffraction image of the crystal lattice is observed and a hexagonal crystal phase in which an electron beam backscatter diffraction image of the hexagonal crystal lattice is observed, and the cubic crystal phase The area ratio of the hexagonal crystal phase to the total of the hexagonal crystal phase is 10 to 50 area%,
(C) measuring an inclination angle formed by a normal line of a (0001) plane which is a crystal plane of a crystal grain of a hexagonal crystal phase of the composite carbonitride layer with respect to a normal direction of the substrate surface; When the measured inclination angles within the range of 0 to 90 degrees with respect to the normal direction of the substrate surface are divided into pitches of 0.25 degrees and the frequencies existing in each section are tabulated, 2 to 12 degrees The maximum peak exists in the inclination angle section within the range of 2 to 12, and the sum of the frequencies existing in the inclination angle section of 2 to 12 degrees is 40% or more of the entire frequency in the inclination angle frequency distribution. Surface coated cutting tool.
上記複合炭窒化物層の六方晶結晶相の結晶粒の平均粒子幅ωhが0.1〜2μmであり、平均アスペクト比αhが2以上、
であることを特徴とする請求項1に記載の表面被覆切削工具。 The average grain width ω c of the cubic crystal phase grains of the composite carbonitride layer is 0.3 μm or less, the average aspect ratio α c is less than 2, and
The average grain width ω h of the crystal grains of the hexagonal crystal phase of the composite carbonitride layer is 0.1 to 2 μm, the average aspect ratio α h is 2 or more,
The surface-coated cutting tool according to claim 1, wherein
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JP3416938B2 (en) * | 1994-10-28 | 2003-06-16 | 住友電気工業株式会社 | Laminate |
JP3416937B2 (en) * | 1994-10-28 | 2003-06-16 | 住友電気工業株式会社 | Laminate |
JP4507308B2 (en) * | 1999-09-27 | 2010-07-21 | 三菱マテリアル株式会社 | Surface coated cemented carbide milling tool throwaway tip with excellent fracture resistance |
JP4099081B2 (en) * | 2003-02-17 | 2008-06-11 | 京セラ株式会社 | Surface coated cutting tool |
DE102005032860B4 (en) * | 2005-07-04 | 2007-08-09 | Fraunhofer-Gesellschaft zur Förderung der angewandten Forschung e.V. | Hard material coated bodies and process for their production |
JP4942495B2 (en) * | 2007-01-26 | 2012-05-30 | 京セラ株式会社 | Surface coating tool |
DE102007000512B3 (en) * | 2007-10-16 | 2009-01-29 | Fraunhofer-Gesellschaft zur Förderung der angewandten Forschung e.V. | Hard-coated body with a multi-layer system for tools and components such as drills, millers and indexable inserts, comprises a bonding layer applied on the body, a single- or multi-phase hard layer, and a phase gradient layer |
JP5187570B2 (en) * | 2007-12-28 | 2013-04-24 | 三菱マテリアル株式会社 | Surface coated cutting tool with excellent wear resistance due to hard coating layer |
DE102008013966A1 (en) * | 2008-03-12 | 2009-09-17 | Kennametal Inc. | Hard material coated body |
DE102008013965A1 (en) * | 2008-03-12 | 2009-09-17 | Kennametal Inc. | Hard material coated body |
DE102009046667B4 (en) * | 2009-11-12 | 2016-01-28 | Fraunhofer-Gesellschaft zur Förderung der angewandten Forschung e.V. | Coated bodies of metal, hardmetal, cermet or ceramic, and methods of coating such bodies |
JP5483110B2 (en) * | 2010-09-30 | 2014-05-07 | 三菱マテリアル株式会社 | Surface coated cutting tool with excellent chipping resistance due to hard coating layer |
JP2012152878A (en) * | 2011-01-28 | 2012-08-16 | Hitachi Tool Engineering Ltd | Coating tool having superior wear resistance and slide resistance, and manufacturing method of the same |
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2012
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CN103801718B (en) | 2017-09-15 |
JP2014097536A (en) | 2014-05-29 |
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