JP2003117706A - Covered tool - Google Patents
Covered toolInfo
- Publication number
- JP2003117706A JP2003117706A JP2001308376A JP2001308376A JP2003117706A JP 2003117706 A JP2003117706 A JP 2003117706A JP 2001308376 A JP2001308376 A JP 2001308376A JP 2001308376 A JP2001308376 A JP 2001308376A JP 2003117706 A JP2003117706 A JP 2003117706A
- Authority
- JP
- Japan
- Prior art keywords
- film
- titanium
- gas
- lower layer
- carbonitride
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
- Granted
Links
Landscapes
- Cutting Tools, Boring Holders, And Turrets (AREA)
- Chemical Vapour Deposition (AREA)
Abstract
Description
【０００１】[0001]
【発明の属する技術分野】本願発明は炭窒化チタン膜又
は／及び炭窒酸化チタン膜を被覆した被覆工具に関す
る。TECHNICAL FIELD The present invention relates to a coated tool coated with a titanium carbonitride film and / or a titanium oxycarbonitride film.
【０００２】[0002]
【従来の技術】一般に、被覆工具は超硬質合金、高速度
鋼、特殊鋼からなる基体表面に硬質皮膜を化学蒸着法
や、物理蒸着法により成膜して製作される。このような
被覆工具は皮膜の耐摩耗性と基体の強靭性とを兼ね備え
ており、広く実用に供されている。特に、高硬度材を高
速で切削する場合、切削工具の刃先温度は１０００℃前
後まで上がり、被削材との接触による摩耗や断続切削等
の機械的衝撃に耐える必要がある。このため、耐摩耗性
と強靭性とを兼ね備えた被覆工具が重宝されている。2. Description of the Related Art Generally, a coated tool is manufactured by forming a hard coating on the surface of a substrate made of super hard alloy, high speed steel or special steel by chemical vapor deposition or physical vapor deposition. Such a coated tool has both the wear resistance of the coating and the toughness of the substrate, and is widely put to practical use. In particular, when cutting a high hardness material at a high speed, the cutting edge temperature of the cutting tool rises up to around 1000 ° C., and it is necessary to withstand mechanical impact such as wear due to contact with the work material and intermittent cutting. For this reason, a coated tool having both wear resistance and toughness is valued.
【０００３】上記の硬質皮膜には、耐摩耗性と靭性とが
優れる周期律表４ａ、５ａ、６ａ族金属の炭化物、窒化
物、炭窒化物、炭酸化物、窒酸化物、炭窒酸化物からな
る膜と、耐酸化性に優れる酸化アルミニウム膜が単層あ
るいは多層膜として用いられている。上記の周期律表４
ａ、５ａ、６ａ族金属にはチタンが主に用いられ、特
に、窒化チタン膜や炭化チタン膜あるいは炭窒化チタン
膜が重用されている。このため、煩雑を避けるため、以
降は、周期律表４ａ、５ａ、６ａ族金属の代表としてチ
タンを用いて具体的に詳述する。これらの皮膜の中で
も、炭窒化チタン膜や炭窒酸化チタン膜は窒化チタン膜
の靭性と炭化チタン膜の耐摩耗性の長所をバランス良く
有しており、被覆工具用皮膜として重用されている。本
発明者等は特許第２６６０１８０号や特開平１０−１５
７１１号により柱状晶の形態を持つ炭窒化膜を提案して
きた。また、他にも、特開平６−１５８３２４号や、特
開平６−１５８３２５号、特開平７−６２５４２号、特
開平７−１００７０１号等が提案されている。しかし、
これら炭窒化チタン膜や炭窒酸化チタン膜においても、
膜中にクラックが発生し膜の一部が脱落し易い欠点があ
った。The above hard coating is made of carbides, nitrides, carbonitrides, carbonates, oxynitrides, oxycarbonitrides of metals of Groups 4a, 5a and 6a of the Periodic Table, which have excellent wear resistance and toughness. And an aluminum oxide film having excellent oxidation resistance are used as a single layer or a multilayer film. Periodic table 4 above
Titanium is mainly used for the a, 5a, and 6a metals, and in particular, a titanium nitride film, a titanium carbide film, or a titanium carbonitride film is heavily used. For this reason, in order to avoid complication, titanium will be specifically described below as a representative of the metals of the periodic tables 4a, 5a, and 6a. Among these coatings, the titanium carbonitride film and the titanium oxycarbonitride film have a good balance between the toughness of the titanium nitride film and the wear resistance of the titanium carbide film, and are therefore heavily used as coatings for coated tools. The inventors of the present invention have disclosed Japanese Patent No. 2660180 and JP-A-10-15.
No. 711 has proposed a carbonitride film having a columnar crystal form. In addition, Japanese Patent Laid-Open Nos. 6-158324, 6-158325, 7-62542, and 7-10071 are proposed. But,
Also in these titanium carbonitride film and titanium carbonitride oxide film,
There is a defect that cracks are generated in the film and a part of the film is easily removed.
【０００４】本発明者らは、上記従来技術における欠点
を解決するために鋭意研究した結果、これらの膜のクラ
ックは粒界を中心にして発生していること、そして、双
晶構造を持った炭窒化チタン膜や炭窒酸化チタン膜を実
現することにより結晶粒界の強度や膜間の密着性が高め
られることを見出し、特開平１１−２５６３３６号、特
開２０００−２５９０５号として出願し、当該技術を開
示した。As a result of intensive studies to solve the above-mentioned drawbacks of the prior art, the present inventors have found that cracks in these films mainly occur at grain boundaries and have a twin structure. It was found that the strength of grain boundaries and the adhesion between films can be enhanced by realizing a titanium carbonitride film or a titanium oxycarbonitride film, and filed as JP-A Nos. 11-256336 and 2000-25905. The technique has been disclosed.
【０００５】[0005]
【発明が解決しようとする課題】本発明は、本願発明者
らが先に提案した上記発明を更に発展させ、炭窒化チタ
ン膜や炭窒酸化チタン膜の結晶粒界の強度を高めるとと
もに、耐クラック性をさらに高めることにより従来に比
して切削耐久特性が格段に優れる被覆工具を提供するこ
とである。DISCLOSURE OF THE INVENTION The present invention is a further development of the above-mentioned invention proposed by the present inventors to enhance the strength of the crystal grain boundaries of titanium carbonitride film and titanium oxycarbonitride film, and It is an object of the present invention to provide a coated tool which is much more excellent in cutting durability than conventional ones by further improving the cracking property.
【０００６】[0006]
【課題を解決するための手段】本発明者らは上記課題を
解決するために鋭意研究してきた結果、周期律表４ａ、
５ａ、６ａ族金属の炭窒化膜及び／又は炭窒酸化膜、特
にチタン等の炭窒化膜及び／又は炭窒酸化膜を少なくと
も上下の二層で構成し下層に双晶構造を持たせることに
より、これら皮膜の結晶粒界の強度と耐クラック性が高
まり、優れた切削耐久特性を持つ被覆工具が得られるこ
とを見出し、本発明に想到した。Means for Solving the Problems The inventors of the present invention have earnestly studied to solve the above problems, and as a result, the periodic table 4a,
By forming a carbonitride film and / or a carbonitride oxide film of a metal of group 5a, 6a, particularly a carbonitride film and / or a carbonitride oxide film of titanium or the like in at least two upper and lower layers and providing a twin structure in the lower layer. The inventors have found that a coated tool having excellent cutting durability characteristics can be obtained by increasing the strength of crystal grain boundaries and crack resistance of these coatings, and conceived the present invention.
【０００７】すなわち本発明は、基体表面に周期律表の
４ａ、５ａ、６ａ族金属の炭化物、窒化物、酸化物、炭
窒化物、炭酸化物、窒酸化物、炭窒酸化物、並びに酸化
アルミニウムのいずれか一種の単層皮膜または二種以上
の多層皮膜を有し、その少なくとも一つが炭窒化チタン
膜又は／及び炭窒酸化チタン膜からなる被覆工具におい
て、前記炭窒化チタン膜又は／及び炭窒酸化チタン膜が
少なくとも互いに接触した下層と上層の二層からなり、
下層が双晶構造を持った結晶粒を含有していることを特
徴とする被覆工具である。本発明を適用することによ
り、下層が双晶構造を有しており結晶粒界が双晶面から
なっているため粒界の強度が高く、しかも、下層と上層
の二層に分かれていることにより下層でクラックが発生
した場合もその進展が上層との界面で抑制されるため、
優れた切削耐久特性が実現されていると判断される。That is, according to the present invention, a carbide, a nitride, an oxide, a carbonitride, a carbonitride, a nitrite, an oxycarbonitride, and an aluminum oxide of a group 4a, 5a, or 6a metal of the periodic table are formed on the surface of a substrate. A coated tool having a single-layer coating of any one of the following, or a multilayer coating of two or more thereof, at least one of which comprises a titanium carbonitride film and / or a titanium oxycarbonitride film. The titanium oxynitride film is composed of at least two layers, a lower layer and an upper layer, which are in contact with each other,
The coated tool is characterized in that the lower layer contains crystal grains having a twin structure. By applying the present invention, since the lower layer has a twin structure and the crystal grain boundaries are composed of twin planes, the strength of the grain boundary is high, and further, the lower layer and the upper layer are divided into two layers. Therefore, even if cracks occur in the lower layer, their progress is suppressed at the interface with the upper layer,
It is judged that excellent cutting durability characteristics have been realized.
【０００８】ここで、本発明における下層は双晶構造を
持った柱状で縦長の結晶粒から構成されていることが好
ましい。この場合、縦長・柱状であることにより横方向
の結晶粒径を大きくすることなく膜厚を厚くすることが
出来、工具としての耐摩耗性を高めることが出来る。し
かも、結晶粒界が双晶面から成っており粒間が高い密着
強度を有しているため、柱状結晶の縦長の結晶粒界を通
って膜厚方向にクラックが進展するのを抑える効果が現
れ、更に優れた切削耐久特性が実現できる。また、上層
は粒状の結晶粒から構成されていることが好ましい。こ
うすることにより、下層の双晶面が上層との界面で終了
し易くなるとともに上層の結晶粒が下層の双晶結晶粒に
たがをはめる形になり、更に優れた切削耐久特性が実現
できる。Here, it is preferable that the lower layer in the present invention is composed of vertically elongated crystal grains having a twin structure. In this case, because of the vertically long and columnar shape, the film thickness can be increased without increasing the crystal grain size in the horizontal direction, and the wear resistance as a tool can be improved. Moreover, since the crystal grain boundaries are composed of twin planes and have a high adhesion strength between the grains, the effect of suppressing the propagation of cracks in the film thickness direction through the longitudinal crystal grain boundaries of the columnar crystals is effective. Appearance can be realized, and more excellent cutting durability characteristics can be realized. Further, the upper layer is preferably composed of granular crystal grains. By doing so, the twin plane of the lower layer is likely to end at the interface with the upper layer, and the crystal grains of the upper layer follow the twin crystal grains of the lower layer, resulting in further excellent cutting durability characteristics. .
【０００９】次に、本発明の被覆工具は、前記下層の双
晶面の過半が該上層との界面で終了していることが好ま
しい。これにより該双晶面にクラックが発生した場合も
上層がクラックの進展を押さえ込むとともに、上層が該
双晶面の両側の結晶粒（双晶結晶粒）にたがをはめた形
になり、更に結晶粒界の耐クラック性が高まり、優れた
切削耐久特性が実現される。更に、本発明の被覆工具
は、前記双晶面が｛１１１｝面から成っていることが好
ましい。これにより、双晶面がより緻密に形成され、双
晶面の粒界強度が更に高められ、更に優れた切削耐久特
性が得られるものと判断される。Next, in the coated tool of the present invention, it is preferable that the majority of twin planes of the lower layer end at the interface with the upper layer. As a result, even when cracks occur in the twin plane, the upper layer suppresses the progress of cracks, and the upper layer has a shape in which the crystal grains on both sides of the twin plane (twin crystal grains) are fitted, The crack resistance of the grain boundaries is enhanced, and excellent cutting durability characteristics are realized. Further, in the coated tool of the present invention, it is preferable that the twin plane is composed of a {111} plane. As a result, it is considered that the twin planes are formed more densely, the grain boundary strength of the twin planes is further increased, and further excellent cutting durability characteristics are obtained.
【００１０】[0010]
【発明の実施の形態】本発明の被覆工具において、皮膜
のミクロ組織は、後述の実施例に示すように、透過型電
子顕微鏡により膜断面を観察し評価した。膜中に含まれ
る酸素量は、研磨した膜断面中の５点を、電子プローブ
マイクロアナライザー（ＥＰＭＡ、日本電子（株）製Ｊ
ＸＡ−８９００Ｒ）を用い、加速電圧１５ＫＶ、試料電
流０．２μＡで分析し、その平均値より求めた。BEST MODE FOR CARRYING OUT THE INVENTION In the coated tool of the present invention, the microstructure of the coating was evaluated by observing the section of the coating with a transmission electron microscope, as shown in Examples below. Regarding the amount of oxygen contained in the film, five points in the polished film cross section were measured with an electron probe microanalyzer (EPMA, JEOL Ltd. J.
XA-8900R) at an acceleration voltage of 15 KV and a sample current of 0.2 μA, and the average value was obtained.
【００１１】本発明の被覆工具において、チタンは周期
律表の４ａ、５ａ、６ａ族金属の代表として表記したも
のであり、他の同族金属、例えばＺｒ、Ｈｆ、Ｖ、Ｎ
ｂ、Ｔａ、Ｃｒ、Ｍｏ、Ｗのいずれかであっても略同様
の効果が得られる。また、炭窒化チタン膜や炭窒酸化チ
タン膜はＣＨ３ＣＮとＴｉＣｌ４等を反応させて成膜す
る膜に限るものではなく、ＣＨ４、Ｎ２、ＴｉＣｌ４等
を反応させて成膜するＴｉＣＮやＴｉＣＮＯ膜でもよ
い。更に、炭窒化チタン膜や炭窒酸化チタン膜はＴｉＣ
ＮやＴｉＣＮＯに限るものではない。例えば、ＴｉＣＮ
やＴｉＣＮＯにＣｒ、Ｚｒ、Ｔａ、Ｍｇ、Ｙ、Ｓｉ、Ｂ
の一種又は二種以上を０．３〜１０質量％添加した膜で
も良い。０．３質量％未満ではこれらを添加する効果が
現れず、１０質量％を超えるとＴｉＣＮやＴｉＣＮＯ膜
の高耐摩耗や高靭性の効果が低くなる欠点が現れる。In the coated tool of the present invention, titanium is represented as a representative of metals of groups 4a, 5a and 6a in the periodic table, and other metals of the same group, for example, Zr, Hf, V and N.
Even if any of b, Ta, Cr, Mo, and W is used, substantially the same effect can be obtained. Further, the titanium carbonitride film or the titanium oxycarbonitride film is not limited to a film formed by reacting CH 3 CN and TiCl 4 or the like, and is formed by reacting CH 4 , N 2 , TiCl 4 or the like. A TiCN or TiCNO film may be used. Furthermore, the titanium carbonitride film and titanium oxycarbonitride film are made of TiC.
It is not limited to N and TiCNO. For example, TiCN
Or TiCNO with Cr, Zr, Ta, Mg, Y, Si, B
One or two or more of the above may be added to the film in an amount of 0.3 to 10% by mass. If it is less than 0.3% by mass, the effect of adding these does not appear, and if it exceeds 10% by mass, the effects of high wear resistance and high toughness of the TiCN or TiCNO film become poor.
【００１２】次に、本発明の被覆工具において、炭窒化
チタン膜や炭窒酸化チタン膜の上に成膜する膜はＴｉＣ
膜やＴｉＮ膜、ＴｉＣＯ膜、ＴｉＮＯ膜又はＴｉＣＮＯ
膜に限るものではない。例えば、前記膜の成分にＣｒ、
Ｚｒ、Ｔａ、Ｍｇ、Ｙ、Ｓｉ、Ｂの一種又は二種以上を
０．３〜１０質量％添加したものでもよい。また、炭窒
化チタン膜や炭窒酸化チタン膜の上に、直接、酸化アル
ミニウムや酸化ジルコニウム等を主とする酸化膜を成膜
するのも有効である。また、下地膜はＴｉＮに限るもの
ではなく、例えば、下地膜としてＴｉＣ膜、ＴｉＣＮ
膜、ＺｒＮ膜、ＨｆＮ膜を成膜した場合も本発明に包含
される。Next, in the coated tool of the present invention, the film formed on the titanium carbonitride film or titanium oxycarbonitride film is TiC.
Film, TiN film, TiCO film, TiNO film or TiCNO
It is not limited to the membrane. For example, the film component is Cr,
One containing one or more of Zr, Ta, Mg, Y, Si, and B may be added in an amount of 0.3 to 10% by mass. Further, it is also effective to directly form an oxide film mainly containing aluminum oxide, zirconium oxide or the like on the titanium carbonitride film or the titanium oxycarbonitride film. The base film is not limited to TiN. For example, a TiC film or TiCN film may be used as the base film.
The present invention also includes the case where a film, a ZrN film, or a HfN film is formed.
【００１３】本発明の被覆工具に有用な酸化アルミニウ
ム膜として、κ型酸化アルミニウム単相又はα型酸化ア
ルミニウム単相の膜が例示される。また、κ型酸化アル
ミニウムとα型酸化アルミニウムとの混合膜でもよい。
また、κ型酸化アルミニウム及び／又はα型酸化アルミ
ニウムと、γ型酸化アルミニウム、θ型酸化アルミニウ
ム、δ型酸化アルミニウム、χ型酸化アルミニウムの少
なくとも一種以上とからなる混合膜でもよい。また、酸
化アルミニウムと酸化ジルコニウム等に代表される他の
酸化物との混合膜でもよい。本発明の被覆工具の製作は
既知の成膜方法を採用できる。例えば、通常の化学蒸着
法（熱ＣＶＤ）、プラズマを付加した化学蒸着法（ＰＡ
ＣＶＤ）、イオンプレーティング法等を用いることがで
きる。用途は切削工具に限るものではなく、周期律表の
４ａ、５ａ、６ａ族金属（特に、チタン）の一種又は二
種以上の炭窒化物や炭窒酸化物を主とする膜を含む単層
あるいは多層の硬質皮膜を被覆した耐摩耗材や金型、溶
湯部品等でもよい。以下、本発明の被覆工具を実施例に
より具体的に説明するが、それら実施例により本発明が
限定されるものではない。As the aluminum oxide film useful for the coated tool of the present invention, a κ type aluminum oxide single phase film or an α type aluminum oxide single phase film is exemplified. Alternatively, a mixed film of κ-type aluminum oxide and α-type aluminum oxide may be used.
Further, a mixed film of κ-type aluminum oxide and / or α-type aluminum oxide and at least one of γ-type aluminum oxide, θ-type aluminum oxide, δ-type aluminum oxide, and χ-type aluminum oxide may be used. Further, a mixed film of aluminum oxide and another oxide typified by zirconium oxide may be used. The coated tool of the present invention can be manufactured by a known film forming method. For example, a normal chemical vapor deposition method (thermal CVD), a chemical vapor deposition method with addition of plasma (PA
CVD), an ion plating method, etc. can be used. The use is not limited to cutting tools, but a single layer containing a film mainly containing one or more carbonitrides or carbonitride oxides of 4a, 5a, and 6a metals (especially titanium) of the periodic table. Alternatively, a wear resistant material coated with a multilayer hard coating, a mold, a molten metal component, or the like may be used. Hereinafter, the coated tool of the present invention will be specifically described with reference to Examples, but the present invention is not limited to these Examples.
【００１４】（実施例１）ＷＣ：８０質量％、ＴｉＣ：
５質量％、（Ｔａ、Ｎｂ）Ｃ：６質量％、Ｃｏ：９質量
％の組成よりなる切削工具用超硬合金製基板をＣＶＤ炉
内にセットし、その表面に、化学蒸着法によりＨ２キャ
リヤーガスとＴｉＣｌ４ガスとＮ２ガスとを原料ガスに
用いて０．３μｍ厚さのＴｉＮを９００℃でまず形成し
た。続いて、ＴｉＣｌ４ガスを０．５ｖｏｌ％、ＣＨ３
ＣＮガスを１ｖｏｌ％、Ｎ２ガスを４０ｖｏｌ％、ＣＯ
ガスを１ｖｏｌ％、残Ｈ２キャリヤーガスで構成された
原料ガスを毎分５５００ｍｌだけＣＶＤ炉内に流し、成
膜温度９００℃、成膜圧力５０Ｔｏｏｒの条件で６μｍ
厚さのＴｉＣＮＯ膜を成膜した。その後、続けてＴｉＣ
ｌ４ガスを１ｖｏｌ％、ＣＨ４ガスを２．５ｖｏｌ％、
Ｎ２ガスを３０ｖｏｌ％、残Ｈ２キャリヤーガスで構成
された原料ガスを毎分５５００ｍｌだけＣＶＤ炉内に流
し、成膜温度９９０℃、成膜圧力２０Ｔｏｏｒの条件で
１μｍ厚さのＴｉＣＮ膜を成膜した。そして、上記Ｔｉ
ＣＮの成膜に用いた原料ガスにＣＯ２とＣＯとの混合ガ
スを５ｖｏｌ％追加した混合ガスを流し、上記ＴｉＣＮ
と同じ成膜温度、成膜圧力で反応させることにより０．
３μｍ厚のＴｉＣＮＯから成る結合膜を作製した。続い
て、Ａｌ金属小片を詰め３５０℃に保温した小筒中にＨ
２ガス３１０ｍｌ／分とＨＣｌガス１３０ｍｌ／分とを
流すことにより発生させたＡｌＣｌ３ガスとＨ２ガス２
ｌ／分とＣＯ２ガス１００ｍｌ／分とをＣＶＤ炉内に流
し、１０２０℃で反応させることにより所定の厚さのα
型酸化アルミニウム膜を成膜した。そして最後に１０２
０℃でＨ２キャリヤーガスとＴｉＣｌ４ガスとＮ２ガス
とを原料ガスに用いて０．５μｍ厚さのＴｉＮを成膜す
ることにより本発明の被覆工具を得た。(Example 1) WC: 80% by mass, TiC:
A substrate made of cemented carbide for a cutting tool having a composition of 5% by mass, (Ta, Nb) C: 6% by mass, Co: 9% by mass is set in a CVD furnace, and H 2 is formed on the surface thereof by a chemical vapor deposition method. First, a carrier gas, TiCl 4 gas, and N 2 gas were used as raw material gases to form TiN having a thickness of 0.3 μm at 900 ° C. Then, 0.5% by volume of TiCl 4 gas and CH 3
1 vol% CN gas, 40 vol% N 2 gas, CO
Gas of 1 vol% and raw material gas composed of residual H 2 carrier gas were flowed into the CVD furnace at a rate of 5500 ml / min, and the film deposition temperature was 900 ° C., and the film deposition pressure was 50 Toor.
A TiCNO film having a thickness was formed. After that, continue with TiC
l 4 gas 1 vol%, CH 4 gas 2.5 vol%,
A source gas composed of 30 vol% N 2 gas and 5500 ml / min of the residual H 2 carrier gas was flowed into the CVD furnace to form a 1 μm thick TiCN film under the conditions of a film forming temperature of 990 ° C. and a film forming pressure of 20 Torr. Filmed And the above Ti
A mixed gas obtained by adding 5 vol% of a mixed gas of CO 2 and CO to the raw material gas used for forming the CN film is flowed, and the above TiCN is used.
When the film formation temperature and film formation pressure are the same,
A bonding film made of TiCNO having a thickness of 3 μm was prepared. Subsequently, H in small tube was kept in 350 ° C. stuffed Al metal pieces
AlCl 3 gas and H 2 gas 2 generated by flowing 310 ml / min of 2 gas and 130 ml / min of HCl gas
l / min and 100 ml / min of CO 2 gas are caused to flow in the CVD furnace and reacted at 1020 ° C. to obtain α of a predetermined thickness.
A type aluminum oxide film was formed. And finally 102
A coated tool of the present invention was obtained by forming a 0.5 μm thick film of TiN at 0 ° C. using H 2 carrier gas, TiCl 4 gas and N 2 gas as source gases.
【００１５】図１は、実施例１の条件で作製した本発明
の代表的な被覆工具の膜断面を透過型電子顕微鏡（ＴＥ
Ｍ、（株）日立製作所製Ｈ−８００、２００ｋＶ）で撮
影したミクロ組織の一例を示しており、図２は図１に対
応した模式図である。図２には、上層の炭窒酸化チタン
膜（符号２）と下層の炭窒化チタン膜（符号１）及び結
合膜（符号３）と酸化アルミニウム膜（符号４）が撮影
されている。図１より、下層の炭窒酸化チタン膜は膜厚
方向に細長い柱状の結晶粒から構成されており、上層の
炭窒化チタン膜は縦横の比が３以下の粒状の結晶粒から
構成されていることがわかる。図１、２より、下層の炭
窒酸化チタン膜中の１ｃ、１ｄ、１ｅの結晶粒界が直線
的であり双晶面である可能性が高いことがわかる。１ｆ
も粒界はあまり明瞭ではないが双晶面である可能性があ
る。尚、炭窒酸化チタン膜１中に基体表面と略平行な縞
状の濃淡が多数個観察されているが、これは炭窒酸化チ
タンの結晶方位が層状に微妙に変動し入射電子線の透過
率が異なっているためである。この濃淡の縞が各結晶粒
界を境にして略対称であることからも各結晶粒界の両側
の結晶粒が双晶になっている可能性が高いことがわか
る。FIG. 1 shows a cross section of a film of a typical coated tool of the present invention manufactured under the conditions of Example 1 by a transmission electron microscope (TE).
M, an H-800 manufactured by Hitachi, Ltd., 200 kV) is shown as an example of the microstructure, and FIG. 2 is a schematic diagram corresponding to FIG. In FIG. 2, the upper layer of titanium carbonitride oxide film (reference numeral 2), the lower layer of titanium carbonitride film (reference numeral 1), the bonding film (reference numeral 3) and the aluminum oxide film (reference numeral 4) are photographed. From FIG. 1, the lower titanium oxycarbonitride film is composed of elongated crystal grains in the film thickness direction, and the upper titanium carbonitride film is composed of granular crystal grains having an aspect ratio of 3 or less. I understand. From FIGS. 1 and 2, it is understood that the crystal grain boundaries of 1c, 1d, and 1e in the lower titanium oxycarbonitride film are linear and are likely to be twin planes. 1f
The grain boundaries are not so clear, but may be twin planes. It should be noted that in the titanium oxycarbonitride film 1, a large number of striped shades substantially parallel to the substrate surface are observed. This is because the crystallographic orientation of titanium oxycarbonitride subtly changes in a layered manner and the incident electron beam is transmitted. This is because the rates are different. Since the light and shade stripes are substantially symmetrical with respect to each grain boundary, it is understood that the crystal grains on both sides of each grain boundary are likely to be twinned.
【００１６】図３は図１、２中の炭窒酸化チタン膜の１
ａ、１ｂの粒界１ｃの近傍を高倍率で撮影したＴＥＭ写
真である。図３の左右に１ａ、１ｂの結晶粒の格子像が
撮影され、中央部に両者間の粒界１ｃが撮影されてい
る。図３より、１ａ、１ｂの格子縞が粒界１ｃを境にし
て対称であることから、結晶粒１ａと１ｂとが双晶関係
にあり、１ｃが双晶面であることがわかる。また、図３
の１ａ、１ｂの格子像をフーリエ変換し電子線回折図形
として解析した結果、両像は面心立方晶の（１１０）面
の格子像であり、双晶面１ｃは（１１１）面から成って
いることがわかった。FIG. 3 shows one of the titanium oxycarbonitride films in FIGS.
3A is a TEM photograph of the vicinity of the grain boundary 1c of a and 1b taken at high magnification. The lattice images of the crystal grains 1a and 1b are photographed on the left and right of FIG. 3, and the grain boundary 1c between the two is photographed in the center. From FIG. 3, since the lattice fringes of 1a and 1b are symmetric with respect to the grain boundary 1c, it is understood that the crystal grains 1a and 1b have a twinning relationship and 1c is a twin plane. Also, FIG.
As a result of Fourier-transforming the lattice images of 1a and 1b of Fig. 1 and analyzing them as electron beam diffraction patterns, both images are lattice images of the (110) plane of face-centered cubic, and the twin plane 1c is composed of the (111) plane. I found out that
【００１７】一方、上層の炭窒化チタン膜中では下層の
１ｃ、１ｅ、１ｆの直上に直線的な結晶粒界が見られ
ず、結晶粒界１ｃ、１ｅ、１ｆが上層との界面付近で終
了していることがわかる。尚、２ａ付近で多数個観察さ
れている曲線は転移である可能性が高い。上層の膜中で
は２ｂの結晶粒界のみが直線的な形状を示しており、こ
れのみが双晶面である可能性が高いことがわかる。下層
膜の双晶面が上層膜中に続いている可能性がある箇所は
この部分だけである。On the other hand, in the upper titanium carbonitride film, no linear crystal grain boundaries are found immediately above the lower layers 1c, 1e, 1f, and the crystal grain boundaries 1c, 1e, 1f end near the interface with the upper layer. You can see that Note that a large number of curves observed near 2a are highly likely to be transitions. In the upper layer film, only the grain boundaries of 2b show a linear shape, and it is understood that only this is highly likely to be a twin plane. This is the only place where the twin plane of the lower layer film may continue in the upper layer film.
【００１８】上記の結果、ＴＥＭ解析で実際に双晶面で
あることが確かめられた下層の双晶面１ｃは上層との界
面付近で終了していることがわかった。また、直線的な
形状を持ち双晶面である可能性が高いその他の結晶粒界
１ｄ、１ｅ、１ｆの中でも唯一１ｄのみが上層に連続し
ている可能性があり他は連続していないことがわかっ
た。この場合、下層の双晶面が上層に連続している可能
性は四分の一である。即ち、多く見積もっても、下層の
双晶面の過半が上層との界面で終了していることが図１
〜３からわかる。ここで、図１のＴＥＭ写真は皮膜の断
面を厚さ２０μｍ以下に研磨した後、更にイオンミリン
グにより極端に厚さを薄くした膜の断面に電子線を透過
させて撮影したものである。このため、炭窒化チタン膜
や炭窒酸化チタン膜に含有されている双晶部分が実際に
観察される確率は低いと考えられる。したがって、図１
のように双晶部分が観測される確率は低く、観察された
場合はかなりの高い頻度で他の箇所にも双晶部分が存在
していると判断できる。次に、本発明品の膜断面を研摩
し、炭窒酸化チタン膜断面の５点の組成を電子プローブ
マイクロアナライザー（ＥＰＭＡ、日本電子（株）製Ｊ
ＸＡ−８９００Ｒ）を用いて、加速電圧１５ＫＶ、試料
電流０．２μＡで分析した結果、炭窒酸化チタン膜から
はＴｉ、Ｃ、Ｎ、Ｏが検出され、酸素量は５点平均で
０．６質量％であった。As a result of the above, it was found that the twin plane 1c of the lower layer, which was confirmed to be a twin plane by TEM analysis, ended near the interface with the upper layer. Of the other crystal grain boundaries 1d, 1e, 1f that have a linear shape and are likely to be twin planes, only 1d may be continuous with the upper layer and the others are not continuous. I understood. In this case, the possibility that the twin plane of the lower layer is continuous with the upper layer is 1/4. In other words, even if many estimates are made, it is found that the majority of twin planes in the lower layer ends at the interface with the upper layer.
It can be understood from ~ 3. Here, the TEM photograph of FIG. 1 is obtained by polishing the cross section of the film to a thickness of 20 μm or less and then transmitting the electron beam to the cross section of the film extremely thinned by ion milling. Therefore, it is considered that the probability of actually observing the twinned portion contained in the titanium carbonitride film or the titanium oxycarbonitride film is low. Therefore, FIG.
As described above, the probability of twinned portions being observed is low, and if observed, it can be determined that twinned portions also exist at other locations with a fairly high frequency. Next, the film cross section of the product of the present invention was polished, and the composition of the five points of the titanium oxycarbonitride film cross section was measured with an electron probe microanalyzer (EPMA, JEOL Ltd. J.
XA-8900R) at an accelerating voltage of 15 KV and a sample current of 0.2 μA. As a result, Ti, C, N, and O were detected from the titanium oxycarbonitride film, and the oxygen content was 0.6 on a 5-point average. It was mass%.
【００１９】（実施例２）炭窒化チタン膜又は／及び炭
窒酸化チタン膜が上下の二層からなり下層が双晶構造を
持つものの、下層の双晶面の過半が上層との界面付近で
終了していない場合の影響を明確にするために行った実
施例２を以下に説明する。実施例１と同様の組成から成
る切削工具用超硬基板の表面に、実施例１と同じ条件で
ＴｉＮを成膜した後、続いて、ＴｉＣｌ４ガスを０．５
ｖｏｌ％、ＣＨ３ＣＮガスを１ｖｏｌ％、ＣＯガスを１
ｖｏｌ％、Ｎ２ガスを４０ｖｏｌ％、残Ｈ２キャリヤー
ガスで構成された原料ガスを毎分５５００ｍｌだけＣＶ
Ｄ炉内に流し、成膜温度９００℃、成膜圧力５０Ｔｏｏ
ｒの条件で６μｍ厚さのＴｉＣＮＯ膜を成膜した。その
後、続けて、成膜ガス中にＣＯガスが含まれていない以
外は上記ＴｉＣＮＯ膜と全く同じ成膜条件でＴｉＣＮ膜
を成膜した。そして更に、上記ＴｉＣＮの成膜に用いた
原料ガスにＣＯ２とＣＯとから成る混合ガスを５ｖｏｌ
％追加した混合ガスを流し、上記ＴｉＣＮと同じ成膜温
度、成膜圧力で反応させることにより０．３μｍ厚のＴ
ｉＣＮＯから成る結合膜を成膜した。そして、続いて実
施例１と同じ条件で酸化アルミニウム膜とＴｉＮ膜を成
膜することにより本発明例２を作製した。本発明例２の
炭窒酸化チタン膜と炭窒化チタン膜の界面近傍をＴＥＭ
で観察した結果、下層の炭窒酸化チタン膜と上層の炭窒
化チタン膜の双方が双晶構造を有し、下層の炭窒化チタ
ン膜の双晶面の過半が上層の炭窒酸化チタン膜の双晶面
に連続的につながっていることが確認された。(Example 2) Although the titanium carbonitride film and / or the titanium carbonitride oxide film are composed of two upper and lower layers and the lower layer has a twin structure, a majority of the twin planes of the lower layer is near the interface with the upper layer. Example 2 performed to clarify the effect when the processing is not completed will be described below. After forming a TiN film on the surface of a carbide substrate for a cutting tool having the same composition as in Example 1 under the same conditions as in Example 1, subsequently, TiCl 4 gas was added at 0.5
vol%, CH 3 CN gas 1 vol%, CO gas 1
CV of raw material gas composed of vol%, N 2 gas of 40 vol% and residual H 2 carrier gas of 5500 ml / min
Flowing in D furnace, film forming temperature 900 ° C., film forming pressure 50 Too
A TiCNO film having a thickness of 6 μm was formed under the condition of r. Then, subsequently, a TiCN film was formed under exactly the same film forming conditions as the above TiCNO film except that the film forming gas did not contain CO gas. Further, 5 vol of a mixed gas composed of CO 2 and CO is used as the raw material gas used for forming the TiCN film.
% Additional mixed gas is caused to flow, and the reaction is performed at the same film-forming temperature and film-forming pressure as that of TiCN, whereby T
A bonding film made of iCNO was formed. Then, subsequently, an aluminum oxide film and a TiN film were formed under the same conditions as in Example 1 to prepare Example 2 of the present invention. The vicinity of the interface between the titanium oxycarbonitride film and the titanium carbonitride film of Example 2 of the present invention was TEM
As a result of observation, the lower titanium oxycarbonitride film and the upper titanium oxycarbonitride film both have a twin structure, and the majority of twin planes of the lower titanium carbonitride film are of the upper titanium oxycarbonitride film. It was confirmed that the twin planes were continuously connected.
【００２０】比較例３として、炭窒化チタン膜又は／及
び炭窒酸化チタン膜が上下の二層から成るものの、下層
が双晶構造を持たない場合の影響を明確にするために行
った比較例３を以下に説明する。本発明例２と同様の組
成から成る切削工具用超硬基板の表面に、本発明例２と
同じ条件でＴｉＮを成膜した後、続いて、９９０℃でＴ
ｉＣｌ４ガスを３ｖｏｌ％、ＣＨ４ガスを２ｖｏｌ％、
Ｎ２ガスを３２ｖｏｌ％、ＣＯ２とＣＯの混合ガスを１
２ｖｏｌ％、残Ｈ２キャリヤーガスで構成された原料ガ
スを毎分５５００ｍｌだけＣＶＤ炉内に流し成膜圧力７
５Ｔｏｏｒの条件で反応させることにより６μｍ厚さの
ＴｉＣＮＯ膜を成膜した。続いて同じ条件でＴｉＣｌ４
ガスを２ｖｏｌ％、ＣＨ４ガスを３ｖｏｌ％、Ｎ２ガス
を３２ｖｏｌ％、残Ｈ２キャリヤーガスで構成された原
料ガスを毎分５５００ｍｌだけＣＶＤ炉内に流し１μｍ
厚さのＴｉＣＮ膜を成膜した。その後、本発明例２と同
じ条件でＴｉＣＮＯから成る結合膜と酸化アルミニウム
膜とＴｉＮ膜とを成膜することにより比較例３を作製し
た。この比較例３を本発明例１、２と同様にＴＥＭで観
察したが、下層である炭窒酸化チタン膜中に双晶構造部
は見いだせなかった。In Comparative Example 3, a titanium carbonitride film and / or a titanium oxycarbonitride film are composed of two upper and lower layers, but a comparative example was conducted to clarify the effect when the lower layer does not have a twin structure. 3 will be described below. After forming a TiN film on the surface of a cemented carbide substrate for a cutting tool having the same composition as that of Inventive Example 2 under the same conditions as in Inventive Example 2, subsequently, T at 990 ° C.
LiCl 4 gas 3 vol%, 2 vol% of CH 4 gas,
32 vol% of N 2 gas and 1 of mixed gas of CO 2 and CO
A raw material gas composed of 2 vol% and a residual H2 carrier gas was flowed into the CVD furnace at a rate of 5500 ml / min to form a film at a deposition pressure of 7
A TiCNO film having a thickness of 6 μm was formed by reacting under the condition of 5 Toor. Then, under the same conditions, TiCl 4
Gas of 2 vol%, CH 4 gas of 3 vol%, N 2 gas of 32 vol%, and a raw material gas composed of the remaining H 2 carrier gas were flowed into the CVD furnace at 5500 ml / min to 1 μm.
A TiCN film having a thickness was formed. Then, Comparative Example 3 was prepared by forming a bonding film made of TiCNO, an aluminum oxide film, and a TiN film under the same conditions as in Inventive Example 2. This Comparative Example 3 was observed by TEM in the same manner as Examples 1 and 2 of the present invention, but no twin structure part was found in the lower titanium oxycarbonitride film.
【００２１】上記のようにして作製した本発明例１、２
と比較例３を各５個を以下の条件で断続切削し、欠損に
至るまでの断続切削回数を求めた。刃先先端の欠け状況
は倍率５０倍の実体顕微鏡で観察した。
被削材：Ｓ５３Ｃ溝入材（ＨＳ３８）
工具形状：ＣＮＭＧ１２０４０８
切削条件：２２０ｍ／分
送り：０．２ｍｍ／ｒｅｖ
切り込み：２．０ｍｍ
切削液：水溶性Inventive Examples 1 and 2 produced as described above
And Comparative Example 3 were intermittently cut into 5 pieces each under the following conditions, and the number of times of intermittent cutting until chipping was obtained. The chipped state of the tip of the blade was observed with a stereoscopic microscope at a magnification of 50 times. Work Material: S53C Grooved Material (HS38) Tool Shape: CNMG120408 Cutting Condition: 220m / min Feed: 0.2mm / rev Cutting Depth: 2.0mm Cutting Fluid: Water Soluble
【００２２】本発明例１はいずれも５０００回までは異
常が無く、５２００回衝撃切削後に刃先先端に欠けが発
生した。本発明例２はいずれも３０００回までは異常が
無く、３２００回衝撃切削後に刃先先端に欠けが発生し
た。比較例３は１８００回の衝撃切削後に大きな欠けが
発生し切削工具として劣っていることが判明した。上記
の断続切削試験済品の膜の剥離やクラックの発生状況及
び刃先の欠け状況をミクロ観察したところ、膜の剥離や
クラックが多数見られ、これらが理由で刃先に欠けが生
じたと考えられることがわかった。本発明例１、２は、
比較例３に比べて２．７倍以上、１．６倍以上工具特性
が優れていることがわかる。このように、炭窒化チタン
膜や炭窒酸化チタン膜からなる層が少なくとも上下の二
層からなり、下層が双晶構造を持った結晶粒を含有して
いる本発明の被覆工具は従来に比して格段に工具寿命が
優れ、しかも下層の双晶面の過半が上層との界面で終了
している本発明の被覆工具はさらに工具寿命が優れるも
のであることがわかる。In each of Inventive Example 1, there was no abnormality up to 5000 times, and a chip was formed at the tip of the cutting edge after 5200 impact cuttings. In each of Inventive Example 2, there was no abnormality up to 3000 times, and chipping occurred at the tip of the cutting edge after 3,200 impact cuttings. It was found that Comparative Example 3 was inferior as a cutting tool because a large chipping occurred after 1800 impact cuttings. When microscopically observing the occurrence of film peeling or cracking and the chipping condition of the cutting edge of the above interrupted cutting tested product, a large number of film peeling or cracking were observed, and it is considered that chipping occurred at the cutting edge for these reasons. I understood. Inventive Examples 1 and 2 are
It can be seen that the tool characteristics are 2.7 times or more and 1.6 times or more better than those of Comparative Example 3. As described above, the coated tool of the present invention in which the layer formed of the titanium carbonitride film or the titanium oxycarbonitride film is composed of at least two upper and lower layers, and the lower layer contains the crystal grains having the twin structure is It can be seen that the tool life of the coated tool of the present invention in which the tool life is remarkably excellent and the majority of twin planes in the lower layer ends at the interface with the upper layer is further excellent.
【００２３】[0023]
【発明の効果】上述のように、本発明によれば、炭窒化
チタン膜や炭窒酸化チタン膜から成る層の耐クラック性
が優れ、切削耐久特性の優れた有用な被覆工具を実現す
ることができる。As described above, according to the present invention, it is possible to realize a useful coated tool having excellent crack resistance of a layer formed of a titanium carbonitride film or a titanium oxycarbonitride film and excellent cutting durability characteristics. You can
【図１】図１は、本発明例の炭窒化チタン被覆工具のセ
ラミック材料の組織写真を示す。FIG. 1 shows a microstructure photograph of a ceramic material of a titanium carbonitride coated tool of an example of the present invention.
【図２】図２は、図１の模式図を示す。FIG. 2 shows a schematic diagram of FIG.
【図３】図３は、図２の１ａ、１ｂの粒界１ｃの近傍を
高倍率で撮影したＴＥＭ写真を示す。FIG. 3 shows a TEM photograph of the vicinity of grain boundaries 1c of 1a and 1b in FIG. 2 taken at high magnification.
１ 炭窒化チタン膜 ２ 炭窒酸化チタン膜 ３ 結合膜 ４ 酸化アルミニウム膜 １ａ 炭窒酸化チタン膜の結晶粒 １ｂ 炭窒酸化チタン膜の結晶粒 １ｃ １ｄ １ｅ １ｆ 結晶粒界 1 Titanium carbonitride film 2 Titanium oxycarbonitride film 3 binding membrane 4 Aluminum oxide film 1a Crystal grains of titanium oxycarbonitride film 1b Crystal grains of titanium oxycarbonitride film 1c 1d 1e 1f grain boundary
フロントページの続き Ｆターム(参考） 3C046 FF10 FF13 FF16 4K030 AA03 AA10 AA14 AA17 AA18 BA18 BA35 BA36 BA38 BA41 BA43 BA53 BA56 BA57 BB03 BB13 CA03 LA21 Continued front page F term (reference) 3C046 FF10 FF13 FF16 4K030 AA03 AA10 AA14 AA17 AA18 BA18 BA35 BA36 BA38 BA41 BA43 BA53 BA56 BA57 BB03 BB13 CA03 LA21
Claims (3)
金属の炭化物、窒化物、酸化物、炭窒化物、炭酸化物、
窒酸化物、炭窒酸化物、並びに酸化アルミニウムのいず
れか一種の単層皮膜または二種以上の多層皮膜を有し、
その少なくとも一つが炭窒化チタン膜又は／及び炭窒酸
化チタン膜からなる被覆工具において、前記炭窒化チタ
ン膜又は／及び炭窒酸化チタン膜が少なくとも互いに接
触した下層と上層の二層からなり、下層が双晶構造を持
った結晶粒を含有していることを特徴とする被覆工具。1. A carbide, nitride, oxide, carbonitride, or carbonate of a metal of group 4a, 5a, or 6a of the periodic table on the surface of a substrate.
It has a single-layer coating of any one of nitric oxide, oxycarbonitride, and aluminum oxide, or a multi-layer coating of two or more,
A coated tool, at least one of which comprises a titanium carbonitride film or / and a titanium carbonitride oxide film, wherein the titanium carbonitride film or / and the titanium carbonitride oxide film is composed of at least two layers of a lower layer and an upper layer in contact with each other. Contains a crystal grain having a twin crystal structure.
層の双晶面の過半が該上層との界面で終了していること
を特徴とする被覆工具。2. The coated tool according to claim 1, wherein a majority of twin planes of the lower layer ends at an interface with the upper layer.
前記下層の双晶面が｛１１１｝面から成っていることを
特徴とする被覆工具。3. A coated tool according to claim 1, wherein:
A coated tool characterized in that the twin crystal plane of the lower layer is composed of a {111} plane.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| JP2001308376A JP3768136B2 (en) | 2001-10-04 | 2001-10-04 | Coated tool |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| JP2001308376A JP3768136B2 (en) | 2001-10-04 | 2001-10-04 | Coated tool |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| JP2003117706A true JP2003117706A (en) | 2003-04-23 |
| JP3768136B2 JP3768136B2 (en) | 2006-04-19 |
Family
ID=19127702
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| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| JP2001308376A Expired - Lifetime JP3768136B2 (en) | 2001-10-04 | 2001-10-04 | Coated tool |
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| Country | Link |
|---|---|
| JP (1) | JP3768136B2 (en) |
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| JP2006297579A (en) * | 2005-03-24 | 2006-11-02 | Mitsubishi Materials Corp | Surface coated cermet cutting tool having hard coating layer exhibiting excellent chipping resistance in high-speed intermittent cutting of high hardness steel |
| JP2006297519A (en) * | 2005-04-19 | 2006-11-02 | Mitsubishi Materials Corp | Surface coated cermet cutting tool having hard coating layer exhibiting excellent chipping resistance in high-speed heavy cutting |
| JP2006326713A (en) * | 2005-05-24 | 2006-12-07 | Mitsubishi Materials Corp | CUTTING TOOL OF SURFACE-COATED CERMET WITH THICK FILM alpha-TYPE ALUMINUM OXIDE LAYER ACHIEVING EXCELLENT CHIPPING RESISTANCE |
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| JP2007098503A (en) * | 2005-10-04 | 2007-04-19 | Mitsubishi Materials Corp | Cutting tool made of coated cemented carbide having hard coating layer exhibiting excellent chipping resistance in high speed deep cutting |
| JP2007237329A (en) * | 2006-03-08 | 2007-09-20 | Mitsubishi Materials Corp | Cutting throwaway tip made of surface coated cermet having hard coating layer exhibiting excellent chipping resistance in high-speed cutting of high hardened steel |
| JP2007245292A (en) * | 2006-03-16 | 2007-09-27 | Mitsubishi Materials Corp | Coated cermet throwaway cutting tip having hard coating layer exerting excellent anti-chipping performance in high-speed cutting of high-hardness steel |
| JP2008049470A (en) * | 2006-07-24 | 2008-03-06 | Mitsubishi Materials Corp | Surface coated cutting tool having hard coating layer showing superior chipping resistance |
| JP2008073821A (en) * | 2006-09-22 | 2008-04-03 | Mitsubishi Materials Corp | Surface coated cutting tool with hard coating layer exhibiting excellent chipping resistance |
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| JP2011152601A (en) * | 2010-01-27 | 2011-08-11 | Mitsubishi Materials Corp | Surface-coated cutting tool provided with hard coated layer demonstrating superior chipping resistance |
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