JPH08144045A - Cubic boron nitride coated member - Google Patents
Cubic boron nitride coated memberInfo
- Publication number
- JPH08144045A JPH08144045A JP28785794A JP28785794A JPH08144045A JP H08144045 A JPH08144045 A JP H08144045A JP 28785794 A JP28785794 A JP 28785794A JP 28785794 A JP28785794 A JP 28785794A JP H08144045 A JPH08144045 A JP H08144045A
- Authority
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- Japan
- Prior art keywords
- layer
- intermediate layer
- hard layer
- boron nitride
- hard
- 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.)
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- Physical Vapour Deposition (AREA)
Abstract
Description
【０００１】[0001]
【産業上の利用分野】本発明は、実質的に立方晶窒化ホ
ウ素（以下、ｃ−ＢＮという）からなる硬質層で被覆さ
れた部材に関し、さらに詳しくは、基材と該硬質層との
間に、実質的に六方晶窒化ホウ素（以下、ｈ−ＢＮとい
う）からなる中間層が介在している立方晶窒化ホウ素被
覆部材に関する。BACKGROUND OF THE INVENTION 1. Field of the Invention The present invention relates to a member coated with a hard layer consisting essentially of cubic boron nitride (hereinafter referred to as "c-BN"), and more specifically, a member coated between a substrate and the hard layer. In addition, the present invention relates to a cubic boron nitride coated member in which an intermediate layer substantially made of hexagonal boron nitride (hereinafter referred to as h-BN) is interposed.
【０００２】[0002]
【従来の技術】ｃ−ＢＮは、ダイヤモンドに次ぐ硬さを
有し、鉄系材料との反応性がダイヤモンドに比べて低い
ことから、切削工具や耐摩耗性用品に広く用いられてい
る。しかし、ｃ−ＢＮの製造には超高圧・高温による合
成を必要とするため、ｃ−ＢＮからなる成形体は量産性
が低く、複雑な形状のものが得にくいほか、製造コスト
も非常に高くつくので、その使用範囲は著しく制約され
ている。2. Description of the Related Art c-BN is widely used in cutting tools and wear resistant products because it has hardness second only to diamond and has a lower reactivity with iron-based materials than diamond. However, since the production of c-BN requires synthesis at ultra-high pressure and high temperature, the molded body made of c-BN has low mass productivity, it is difficult to obtain a complicated shape, and the manufacturing cost is very high. Therefore, its range of use is severely restricted.
【０００３】そこで、基材表面に、ｃ−ＢＮからなる被
覆層を形成することにより、低いコストで成形体を得る
ことが試みられている。このようなｃ−ＢＮによる被覆
には、ＣＶＤ法、ＰＶＤ法などにより、ｃ−ＢＮを基材
表面に析出させることが試みられ、ｃ−ＢＮの気相合成
による被覆が、工業的に可能になってきた。Therefore, it has been attempted to obtain a molded article at a low cost by forming a coating layer made of c-BN on the surface of the base material. For such coating with c-BN, it has been attempted to deposit c-BN on the surface of the substrate by a CVD method, a PVD method or the like, and coating by vapor phase synthesis of c-BN is industrially possible. It's coming.
【０００４】このようなｃ−ＢＮ被覆層の形成法とし
て、たとえば特開昭６３−４０５５号公報には、基材、
たとえばＳｉ基材の表面に、ｃ−ＢＮと六方晶窒化ホウ
素からなる窒化ホウ素を析出させた後、アルゴンガスを
用いるスパッタリングによってｈ−ＢＮを選択的にエッ
チングし、このような析出とエッチングを反覆すること
によって、ｃ−ＢＮからなる被覆層を得る方法が開示さ
れている。As a method for forming such a c-BN coating layer, for example, Japanese Patent Laid-Open No. 63-4055 discloses a substrate,
For example, after depositing boron nitride composed of c-BN and hexagonal boron nitride on the surface of a Si substrate, h-BN is selectively etched by sputtering using an argon gas, and such deposition and etching are repeated. By doing so, a method for obtaining a coating layer made of c-BN is disclosed.
【０００５】一方、特開昭６３−１８０５０号公報に
は、基材の表面にイオンプレーティングによって非晶質
または微結晶質の窒化ホウ素の被覆を形成させた後、窒
素イオンを照射して、ｃ−ＢＮ被覆を得る方法が開示さ
れている。On the other hand, in Japanese Patent Laid-Open No. 63-18050, a coating of amorphous or microcrystalline boron nitride is formed on the surface of a base material by ion plating, followed by irradiation with nitrogen ions. A method of obtaining a c-BN coating is disclosed.
【０００６】ｃ−ＢＮ被覆層は、どのような製法によっ
ても内部応力が大きいので、被覆を形成した後に、基材
からの剥離を生じることが多い。それゆえ、このような
ｃ−ＢＮによる被覆の際に、種々の中間層を設けること
により、内部応力を緩和し、該ｃ−ＢＮ層の密着性を向
上させることが試みられている。Since the c-BN coating layer has a large internal stress by any manufacturing method, peeling from the substrate often occurs after the coating is formed. Therefore, it has been attempted to relax the internal stress and improve the adhesion of the c-BN layer by providing various intermediate layers during the coating with the c-BN.
【０００７】中間層として代表的なものに、立方晶系セ
ラミックスがある（特開昭６３−１９３８３２号公報）
が、窒化ホウ素との濡れ性を含む結合性が悪く、密着性
は十分に改善されてはいない。A typical example of the intermediate layer is cubic ceramics (Japanese Patent Laid-Open No. 63-193832).
However, the bondability including wettability with boron nitride is poor, and the adhesiveness is not sufficiently improved.
【０００８】一方、特開平３−２６００５４号公報に
は、中間層として、Ｂとの反応性の高いＴｉを用いるこ
とが開示されている。この中間層によっては、密着性は
改善されるものの、高純度のｃ−ＢＮ被覆層を得ること
は困難である。On the other hand, Japanese Patent Application Laid-Open No. 3-260054 discloses that Ti, which has a high reactivity with B, is used as the intermediate layer. Although this intermediate layer improves the adhesion, it is difficult to obtain a high-purity c-BN coating layer.
【０００９】また、中間層として、Ｂに富む、たとえば
Ｂ／Ｎ（原子比）が１．５〜９の非晶質窒化ホウ素（以
下、ａ−ＢＮという）の層を形成させた後、ＢとＮを
１：１にしてｃ−ＢＮ層を形成させている例もある（特
開昭６３−１７１８６８号公報、特開平３−２８５０６
２号公報など）。しかし、このように組成を変化させた
中間層を設ける方法では、被覆層の密着性は向上するも
のの、ｃ−ＢＮ被覆層中にａ−ＢＮやｈ−ＢＮが混在
し、純粋なｃ−ＢＮによる耐摩耗性の被覆層を形成させ
ることは困難であった。As an intermediate layer, a layer of B-rich amorphous boron nitride (hereinafter referred to as a-BN) having a B / N (atomic ratio) of 1.5 to 9 is formed, and then B is formed. There is also an example in which the c-BN layer is formed with N and N of 1: 1 (JP-A-63-171868, JP-A-3-28506).
No. 2, etc.). However, in the method of providing the intermediate layer with the composition changed in this way, although the adhesion of the coating layer is improved, a-BN and h-BN are mixed in the c-BN coating layer to form pure c-BN. It was difficult to form a wear-resistant coating layer according to.
【００１０】さらに、イオンプレーティング法によって
ｃ−ＢＮ層を形成させる初期の段階において、中間層と
してｈ−ＢＮが形成されるとの上月らの報告（粉体およ
び粉末冶金、41巻１号 57〜62頁（1944年１月）がある
が、ここで開示されている被覆は、本発明者らによる検
討の結果、該ｈ−ＢＮ層の結晶配向性の制御を行わない
と、高純度のｃ−ＢＮ被膜が得られないことが見出され
た。Furthermore, in the initial stage of forming the c-BN layer by the ion plating method, the report of Kozuki et al. (Powder and powder metallurgy, Vol. 41, No. 1) that h-BN is formed as an intermediate layer. 57-62 (January 1944), the coating disclosed herein has a high purity unless the crystal orientation of the h-BN layer is controlled as a result of studies by the present inventors. It was found that no c-BN coating of
【００１１】[0011]
【発明が解決しようとする課題】本発明の目的は、この
ような従来技術では得られていない、高純度のｃ−ＢＮ
からなる硬質層によって、密着性よく被覆された被覆部
材を提供することである。The object of the present invention is to obtain a high purity c-BN which has not been obtained by the prior art.
It is to provide a covering member which is covered with a hard layer consisting of
【００１２】[0012]
【課題を解決するための手段】本発明者らは、上記の目
的を達成するために研究を重ねた結果、ｃ−ＢＮに比べ
て硬さが著しく劣るために、従来から、被覆としては、
潤滑性を利用したものや、電気絶縁を保つための静的な
ものにのみ利用され、切削工具や耐摩耗性用品には利用
されていなかったｈ−ＢＮを、結晶の方向性を与えて中
間層として用いることにより、その上にｃ−ＢＮが優先
的にヘテロエピタキシャルに成長し、高純度のｃ−ＢＮ
から実質的になる硬質層を形成できることを見出して、
本発明を完成するに至った。Means for Solving the Problems As a result of repeated studies for achieving the above object, the present inventors have found that the hardness is significantly inferior to that of c-BN.
The h-BN, which was used only for lubricity and static for maintaining electrical insulation, and was not used for cutting tools and wear-resistant products, gives crystal orientation to intermediate By using it as a layer, c-BN preferentially grows heteroepitaxially on it, and high purity c-BN is obtained.
From the finding that it is possible to form a hard layer consisting essentially of
The present invention has been completed.
【００１３】すなわち、本発明は、基材が、実質的にｃ
−ＢＮからなる硬質層で被覆され、該基材と該硬質層と
の間に、膜厚が０．０１〜１．０μm の実質的にｈ−Ｂ
Ｎからなる中間層が介在していることを特徴とする立方
晶窒化ホウ素被覆部材に関する。That is, in the present invention, the substrate is substantially c
-Substantially h-B coated with a hard layer made of BN and having a film thickness of 0.01 to 1.0 μm between the base material and the hard layer.
The present invention relates to a cubic boron nitride coated member having an intermediate layer of N interposed.
【００１４】本発明に用いられる基材は、その目的に応
じて任意に選択できるが、イオン注入、アニーリングな
どの処理によって密着性をさらに向上させるためには、
そのような処理に伴う温度上昇に耐える材質のものが好
ましい。このような基材としては、ＷＣ−Ｃｏ系、ＷＣ
−ＴｉＣ−Ｃｏ系、ＷＣ−ＴｉＣ−ＴａＣ−Ｃｏ系など
の超硬合金；ＴｉＣ系などのサーメット；Ａｌ2 Ｏ3 、
ＳｉＯ2 、ＺｒＯ2 、ＳｉＣ、ＴｉＣ、Ｓｉ3 Ｎ4 、Ｔ
ｉＮなどのセラミックスが例示される。The base material used in the present invention can be arbitrarily selected according to its purpose, but in order to further improve the adhesion by a treatment such as ion implantation or annealing,
It is preferable to use a material that can withstand a temperature rise due to such treatment. As such a base material, WC-Co type, WC
-TiC-Co system, WC-TiC-TaC-Co based cemented carbide and the like; cermet such as TiC system; Al 2 O 3,
SiO 2 , ZrO 2 , SiC, TiC, Si 3 N 4 , T
Ceramics such as iN are exemplified.
【００１５】基材の形状は、イオンプレーティング、Ｃ
ＶＤなどによって、表面に被膜を形成しうる形状であれ
ば、どのような形状でもよい。The shape of the base material is ion plating, C
Any shape may be used as long as a film can be formed on the surface by VD or the like.
【００１６】本発明の被覆部材において、最外被覆層で
ある硬質層は、実質的に高純度のｃ−ＢＮからなる。ｃ
−ＢＮの純度は、被膜硬さおよび実用上の点から、少な
くとも７０重量％であり、好ましくは、該硬質層はエピ
タキシャル成長によって形成され、ほぼ１００重量％の
ｃ−ＢＮからなる。純度が７０重量％未満では、十分な
硬さと耐摩耗性が得られない。In the coated member of the present invention, the hard layer, which is the outermost coating layer, is substantially made of highly pure c-BN. c
The purity of -BN is at least 70% by weight from the viewpoint of coating hardness and practical use, and preferably, the hard layer is formed by epitaxial growth and consists of approximately 100% by weight of c-BN. If the purity is less than 70% by weight, sufficient hardness and abrasion resistance cannot be obtained.
【００１７】硬質層の膜厚は特に限定されないが、０．
０５〜２０μm が好ましく、０．５〜１０μm が特に好
ましい。０．０５μm 未満では、該硬質層を形成するこ
とによる耐摩耗性を向上する効果が十分でなく、２０μ
m を越えると、該硬質層の内部応力が高くなり、剥離し
やすくなる。Although the film thickness of the hard layer is not particularly limited, it may be 0.
The thickness is preferably from 05 to 20 μm, particularly preferably from 0.5 to 10 μm. If it is less than 0.05 μm, the effect of improving the wear resistance by forming the hard layer is not sufficient,
When it exceeds m, the internal stress of the hard layer becomes high, and the hard layer easily peels off.
【００１８】本発明において特徴的なことは、基材と硬
質層との間に、該硬質層に隣接して、実質的にｈ−ＢＮ
からなる中間層が介在することである。このような中間
層が存在することにより、その上にエピタキシャル成長
によって、所望の高純度ｃ−ＢＮからなる硬質層が得ら
れる。さらに、このような中間層の存在によって、硬質
層の内部応力が緩和されて、その剥離を防止できるとい
う効果がある。A feature of the present invention is that, between the substrate and the hard layer, adjacent to the hard layer, substantially h-BN is provided.
The intermediate layer consisting of Due to the presence of such an intermediate layer, a desired hard layer of high-purity c-BN can be obtained by epitaxial growth thereon. Furthermore, the presence of such an intermediate layer has an effect that the internal stress of the hard layer is relaxed and its peeling can be prevented.
【００１９】中間層の膜厚は、０．０１〜１．０μm で
あり、０．０５〜０．５μm の範囲が好ましく、０．１
〜０．３μm が特に好ましい。０．０１μm 未満では、
硬質層の内部応力を緩和する効果が不十分であり、０．
２μm を越えると、強度が低下する。The thickness of the intermediate layer is 0.01 to 1.0 μm, preferably 0.05 to 0.5 μm, and 0.1 to 1.0 μm.
.About.0.3 .mu.m is particularly preferred. Below 0.01 μm,
The effect of relaxing the internal stress of the hard layer is insufficient, and
If it exceeds 2 μm, the strength is reduced.
【００２０】このような中間層のｈ−ＢＮは、その結晶
軸Ｃ軸の３０％以上が基材に平行になるように配向され
ている。基材に平行なＣ軸の割合は、１００％近く、た
とえば７０〜１００％であることが好ましい。このこと
によって、ｈ−ＢＮ層の底面が成長方向に対して垂直に
なり、膜全体の応力が有効に緩和される。The h-BN of such an intermediate layer is oriented so that 30% or more of its crystal axis C axis is parallel to the substrate. The proportion of the C axis parallel to the substrate is preferably close to 100%, for example 70 to 100%. As a result, the bottom surface of the h-BN layer becomes perpendicular to the growth direction, and the stress of the entire film is effectively relaxed.
【００２１】さらに、中間層のｈ−ＢＮは、硬質層に接
する上面において、２０％以上が(101-0) 結晶面および
／または(112-0) 結晶面からなるプリズムになるように
形成されることが好ましい。このような結晶面は、上面
の８０〜１００％であることがさらに好ましい。ｈ−Ｂ
Ｎの(0001)面はファンデルワールス力で結合しており、
活性種に対して不活性なので、核形成は期待できないか
らである。このような結晶配向性を中間層のｈ−ＢＮに
与えることによって、該中間層の上面に接して、その中
間層に接する面の２０％以上が(112-)結晶面および／ま
たは(110) 結晶面からなるｃ−ＢＮのエピタキシャルな
成長を容易にすることができる。また、このことによっ
て、中間層の(101-0) 結晶面が硬質層の(112-)結晶面
と、中間層の112-0)結晶面が硬質層の(110) 結晶面と、
それぞれ２０％以上、さらに好ましくは８０〜１００％
が平行である結晶方位関係が形成され、ｃ−ＢＮ層のエ
ピタキシャルな成長を助ける。Furthermore, the intermediate layer h-BN is the upper surface in contact with the hard layer, more than 20 percent (101 - 0) crystal plane and / or (112 - 0) are formed such that the prism made of crystal face Preferably. It is more preferable that such a crystal plane is 80 to 100% of the upper surface. h-B
The (0001) plane of N is connected by Van der Waals force,
Because it is inactive against active species, nucleation cannot be expected. By providing such a crystal orientation in the h-BN of the intermediate layer, in contact with the upper surface of the intermediate layer, more than 20% of the surface in contact with the intermediate layer (112 -) crystal plane and / or (110) Epitaxial growth of c-BN having a crystal plane can be facilitated. Further, by this fact, the intermediate layer (101 - 0) crystal plane of the hard layer (112 -) and crystal plane, 112 of the intermediate layer - and 0) crystal plane of the hard layer (110) crystal face,
20% or more, more preferably 80 to 100%
Are parallel to each other, which facilitates epitaxial growth of the c-BN layer.
【００２２】基材と中間層の間に、さらに、実質的にａ
−ＢＮからなる内層が介在することが好ましい。このこ
とによって、中間層の密着性をさらに向上させるととも
に、硬質層の内部応力を緩和させる効果がある。Between the substrate and the intermediate layer, in addition, substantially a
It is preferable that an inner layer made of -BN is interposed. This has the effects of further improving the adhesion of the intermediate layer and relaxing the internal stress of the hard layer.
【００２３】このような中間層の膜厚は、０．０１〜
０．５μm が好ましく、０．０７〜０．３μm の範囲が
さらに好ましい。０．０１μm 未満では、内層を設ける
効果、とくに応力緩和効果が十分でなく、０．５μm を
越えると、硬さや機械的強さが減少する。また、内層を
構成するａ−ＢＮが傾斜組成を有するので、内層の膜厚
は中間層より多少厚めにするのが一般的である。The thickness of such an intermediate layer is from 0.01 to
The thickness is preferably 0.5 μm, more preferably 0.07 to 0.3 μm. If it is less than 0.01 μm, the effect of providing the inner layer, particularly the stress relaxation effect, is not sufficient, and if it exceeds 0.5 μm, the hardness and mechanical strength decrease. Further, since the a-BN forming the inner layer has a gradient composition, it is general that the thickness of the inner layer is slightly thicker than that of the intermediate layer.
【００２４】これらの硬質層および中間層、ならびに必
要に応じて内層は、目的に応じて、基材表面の全面に形
成させてもよく、その一部、たとえば図１の（ａ）
（ｂ）のように一方の面に形成させてもよい。The hard layer, the intermediate layer, and, if necessary, the inner layer may be formed on the entire surface of the substrate according to the purpose, and a part thereof, for example, (a) in FIG.
You may form on one side like (b).
【００２５】本発明の被覆部材は、たとえば、下記のよ
うな方法で、イオンプレーティング装置を用いて形成す
ることができる。The covering member of the present invention can be formed, for example, by the following method using an ion plating device.
【００２６】基材を、イオンプレーティング装置の処理
室に置き、所定の真空度および温度にして、必要に応じ
て、基材への濡れ性の良好なＴｉ膜を形成させた後、Ｔ
ｉに対する反応性の良好なＢを成膜させる。Ｔｉ膜の厚
さは０．３μm 以下が好ましい。その後、漸次、窒素ガ
スを導入して、原子比Ｂ／Ｎ＝１に調節し、基板のＲＦ
バイアスを２００Ｗ程度、磁界を３０〜３５Oeとして、
イオンプレーティングを行い、ａ−ＢＮからなる内層を
形成させる。The base material is placed in a processing chamber of an ion plating apparatus, and a predetermined vacuum degree and temperature are set to form a Ti film having good wettability on the base material, if necessary.
A film of B having good reactivity to i is formed. The thickness of the Ti film is preferably 0.3 μm or less. After that, nitrogen gas was gradually introduced to adjust the atomic ratio B / N = 1 to adjust the RF of the substrate.
With a bias of about 200 W and a magnetic field of 30 to 35 Oe,
Ion plating is performed to form an inner layer made of a-BN.
【００２７】基材に直接、または上記のようにして内層
を形成させた基材に、ＲＦバイアスを２５０以上、３５
０Ｗ未満に上げて、Ｃ軸が基材に平行になるように、ｈ
−ＢＮからなる中間層を形成させる。この際、ＲＦバイ
アスが２５０Ｗ未満ではｈ−ＢＮのＣ軸が基材に平行に
ならず、３５０Ｗ以上になると、ｃ−ＢＮが形成され
る。An RF bias of 250 or more, 35 or more is applied directly to the substrate or to the substrate on which the inner layer is formed as described above.
Raise it to less than 0 W so that the C axis is parallel to the substrate, h
Forming an intermediate layer of BN. At this time, when the RF bias is less than 250 W, the C axis of h-BN is not parallel to the base material, and when it is 350 W or more, c-BN is formed.
【００２８】ついで、ＲＦバイアスを３５０〜５００Ｗ
に上げて、ｃ−ＢＮを形成させる。ＲＦバイアスが３５
０Ｗ未満ではｃ−ＢＮが得られず、５００Ｗを越えると
スパッタ効果が高くなって、膜を形成できない。この
際、磁界を４０Oe程度まで上げることにより、プラズマ
密度を上げて、ＢとＮの反応を高め、ｈ−ＢＮとの界面
における結晶面を制御して、ｃ−ＢＮのエピタキシャル
成長を行わせる。Then, the RF bias is set to 350 to 500 W.
To form c-BN. RF bias is 35
If it is less than 0 W, c-BN cannot be obtained, and if it exceeds 500 W, the sputtering effect becomes high and a film cannot be formed. At this time, by increasing the magnetic field to about 40 Oe, the plasma density is increased, the reaction between B and N is increased, the crystal plane at the interface with h-BN is controlled, and c-BN is epitaxially grown.
【００２９】[0029]
【作用】本発明において、硬質層は高純度のｃ−ＢＮか
らなり、本発明の被覆部材に、優れた表面硬さと耐摩耗
性を与える。また、中間層は実質的にｈ−ＢＮからな
り、また必要に応じて設けられる内層は実質的にａ−Ｂ
Ｎからなり、いずれも密着性を向上させ、応力を緩和さ
せることによって、ｃ−ＢＮ層の剥離を防止する効果が
ある。In the present invention, the hard layer is made of high-purity c-BN and imparts excellent surface hardness and wear resistance to the coated member of the present invention. Further, the intermediate layer is substantially composed of h-BN, and the inner layer provided as necessary is substantially a-B.
It is made of N, and both have an effect of preventing peeling of the c-BN layer by improving adhesion and relieving stress.
【００３０】特に、中間層のｈ−ＢＮを、そのＣ軸の３
０％以上が基材に平行に配向して形成させることによ
り、応力緩和効果を高めることができる。さらに、該中
間層の硬質層に接する面の２０％以上を(101-0) 結晶面
および／または(112-0) 結晶面とすることにより、硬質
層のｃ−ＢＮを高い純度でエピタキシャル成長させて、
優れた耐摩耗性を与えることができる。In particular, the h-BN of the intermediate layer is defined by 3 of its C axis.
The stress relaxation effect can be enhanced by forming 0% or more in parallel with the base material. Furthermore, more than 20% of the surface in contact with the hard layer of the intermediate layer (101 - 0) crystal plane and / or - by the (112 0) crystal plane, grown epitaxially c-BN hard layer in high purity hand,
It can provide excellent wear resistance.
【００３１】[0031]
【実施例】以下の実施例および比較例により、本発明を
さらに詳細に説明する。本発明は、これらの実施例によ
って限定されるものではない。The present invention will be described in more detail with reference to the following examples and comparative examples. The invention is not limited by these examples.
【００３２】基材として、市販のＰ１０超硬合金（ＪＩ
Ｓ Ｂ４０５３）の、鏡面研摩した１０×１０×４mmの
基材を用いた。これを、磁界発生に電磁石を用いる磁界
励起型イオンプレーティング装置を用いて、図１（ｂ）
に示すような被覆部材を作成した。Commercially available P10 cemented carbide (JI
S B4053) of 10 × 10 × 4 mm, which was mirror-polished. This is shown in FIG. 1B using a magnetic field excitation type ion plating device that uses an electromagnet for generating a magnetic field.
A coating member as shown in was prepared.
【００３３】まず、基材を上記装置の処理チャンバーに
置き、５×１０-6Torrまで排気し、２５０℃まで加熱し
た。ボンバードによって基材を清浄にした後、Ｔｉを蒸
発源として、基材ＲＦバイアス４０〜５０Ｗ、Ａｒ流量
５０SCCM、磁界３５Oeで、０．２μm のＴｉ膜を形成さ
せた。ただし、表１に示すように、一部の試料ではＴｉ
膜の形成を行わなかった。First, the substrate was placed in the processing chamber of the above apparatus, evacuated to 5 × 10 -6 Torr, and heated to 250 ° C. After the base material was cleaned by bombarding, a Ti film of 0.2 μm was formed using Ti as an evaporation source and a base material RF bias of 40 to 50 W, an Ar flow rate of 50 SCCM and a magnetic field of 35 Oe. However, as shown in Table 1, in some samples, Ti
No film was formed.
【００３４】蒸発源をＢに切り替え、まずＢのみの蒸発
を行い、ついで窒素ガスをチャンバーに導入して、Ｎ2
を徐々にチャンバー内に導入して、その流量を原子比Ｂ
／Ｎ＝１になるまで増やし、以下、前述のようにＲＦバ
イアスと磁界を調節して、ａ−ＢＮ層（内層）、ｈ−Ｂ
Ｎ（中間層）およびｃ−ＢＮ層（硬質層）を順次形成さ
せた。The evaporation source is switched to B, first only B is evaporated, then nitrogen gas is introduced into the chamber, and N 2
Is gradually introduced into the chamber, and the flow rate is changed to the atomic ratio B
/ N = 1, and then the RF bias and magnetic field are adjusted as described above, and the a-BN layer (inner layer), h-B
An N (intermediate layer) and a c-BN layer (hard layer) were sequentially formed.
【００３５】このようにして得られた本発明による試料
１〜２５および比較品試料１〜５について、各被覆層の
膜厚、結晶の性質、および剥離の有無と、スクラッチテ
ストにおける臨界剥離荷重を表１に示す。ただし、膜厚
は透過電子線回折によって測定を行った。なお、比較品
試料１は中間層の膜厚の薄いもの、比較品試料２はａ−
ＢＮ層の上に直接硬質層を形成させようとしたが、ｈ−
ＢＮとｃ−ＢＮの混合層しか得られなかったもの、比較
品試料３は最外層がｈ−ＢＮからなるもの、比較品試料
４は内層を設けず、中間層がａ−ＢＮとｈ−ＢＮの混合
層からなり、最外層が比較品試料２と同様の混合層しか
得られなかったもの、比較品試料５は同様に内層を設け
ず、中間層が厚さ１μm のＴｉＮ層であり、最外層が比
較品試料２と同様の混合層からなるものである。With respect to Samples 1 to 25 according to the present invention and Comparative Samples 1 to 5 thus obtained, the film thickness of each coating layer, the nature of the crystal, the presence or absence of peeling, and the critical peeling load in the scratch test are It shows in Table 1. However, the film thickness was measured by transmission electron beam diffraction. The comparative sample 1 has a thin intermediate layer, and the comparative sample 2 has a-
I tried to form a hard layer directly on the BN layer, but h-
A sample in which only a mixed layer of BN and c-BN was obtained, the comparative sample 3 had the outermost layer of h-BN, and the comparative sample 4 had no inner layer, and the intermediate layer had a-BN and h-BN. In the same manner, the outermost layer was the same as the comparative sample 2 and the comparative sample 5 did not have an inner layer, and the intermediate layer was a 1 μm thick TiN layer. The outer layer is a mixed layer similar to the comparative sample 2.
【００３６】[0036]
【表１】 [Table 1]
【００３７】[0037]
【表２】 [Table 2]
【００３８】表１から明らかなように、本発明による試
料は剥離が認められず、またスクラッチテストにおいて
高い臨界剥離荷重を示し、耐摩耗性および密着性に優れ
ている。As is clear from Table 1, the samples according to the present invention showed no peeling, showed a high critical peeling load in the scratch test, and were excellent in wear resistance and adhesion.
【００３９】[0039]
【発明の効果】本発明によって、高純度のｃ−ＢＮから
なる硬質層によって密着性よく被覆された被覆部材が得
られる。本発明の被覆部材は、高硬度で耐摩耗性に優
れ、かつ硬質層の基板への密着性が優れているので、切
削工具や耐摩耗性用品としてきわめて有用である。According to the present invention, it is possible to obtain a covering member which is covered with a hard layer made of high-purity c-BN with good adhesion. Since the coated member of the present invention has high hardness and excellent wear resistance and excellent adhesion of the hard layer to the substrate, it is extremely useful as a cutting tool or wear resistant article.
【図１】本発明の被覆部材の構造の例を示す断面図であ
る。（ａ）は内層をもたない例、（ｂ）は内層を有する
例である。FIG. 1 is a cross-sectional view showing an example of the structure of a covering member of the present invention. (A) is an example having no inner layer, and (b) is an example having an inner layer.
【符号の説明】 １ 硬質層（ｃ−ＢＮ層） ２ 中間層（ｈ−ＢＮ層） ３ 内層 （ａ−ＢＮ層） ４ 基材[Description of Reference Signs] 1 hard layer (c-BN layer) 2 intermediate layer (h-BN layer) 3 inner layer (a-BN layer) 4 substrate
Claims (6)
なる硬質層で被覆され、該基材と該硬質層との間に、該
硬質層に隣接して、膜厚が０．０１〜１．０μm の実質
的に六方晶窒化ホウ素からなる中間層が介在しているこ
とを特徴とする立方晶窒化ホウ素被覆部材。1. A substrate is coated with a hard layer consisting essentially of cubic boron nitride, having a thickness of 0.01 between the substrate and the hard layer, adjacent to the hard layer. A cubic boron nitride coated member having an intermediate layer of ˜1.0 μm consisting essentially of hexagonal boron nitride interposed.
０．０１〜０．５μm の実質的に非晶質窒化ホウ素から
なる内層が介在している請求項１記載の被覆部材。2. The coating according to claim 1, wherein an inner layer made of substantially amorphous boron nitride having a film thickness of 0.01 to 0.5 μm is interposed between the base material and the intermediate layer. Element.
基材に平行に配向されている請求項１または２記載の被
覆部材。3. The covering member according to claim 1, wherein 30% or more of the C axis of the intermediate layer is oriented parallel to the base material.
２０％以上が(101-0) 結晶面および／または(112-0) 結
晶面からなり、該硬質層は、該中間層に接する面の２０
％以上が(112-)結晶面および／または(110) 結晶面から
なる請求項１〜３のいずれか１項に記載の被覆部材。The method according to claim 4 wherein the intermediate layer, more than 20% of the surface in contact with the hard layer (101 - 0) crystal plane and / or - consists (1120) crystal plane, the rigid layer, the intermediate layer 20 of the contact surface
% Or more (112 -) crystal plane and / or (110) covering member according to claim 1, comprising a crystal plane.
間層の(101-0) 結晶面が上記硬質層の(112-)結晶面と平
行であり、また該中間層の(112-0) 結晶面が該硬質層の
(110) 結晶面と平行である結晶方位関係にある請求項１
〜４のいずれか１項に記載の被覆部材。Wherein said intermediate layer is least 20% of the intermediate layer (101 - 0) crystal plane of the hard layer (112 -) is parallel to the crystal surface, also of the intermediate layer (112 - 0) crystal surface of the hard layer
A crystal orientation relationship parallel to the (110) crystal plane.
The covering member according to any one of to 4.
である請求項１〜５のいずれか１項に記載の被覆部材。6. The hard layer has a thickness of 0.05 to 20 μm.
The covering member according to any one of claims 1 to 5.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| JP28785794A JPH08144045A (en) | 1994-11-22 | 1994-11-22 | Cubic boron nitride coated member |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| JP28785794A JPH08144045A (en) | 1994-11-22 | 1994-11-22 | Cubic boron nitride coated member |
Publications (1)
| Publication Number | Publication Date |
|---|---|
| JPH08144045A true JPH08144045A (en) | 1996-06-04 |
Family
ID=17722672
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| JP28785794A Withdrawn JPH08144045A (en) | 1994-11-22 | 1994-11-22 | Cubic boron nitride coated member |
Country Status (1)
| Country | Link |
|---|---|
| JP (1) | JPH08144045A (en) |
Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1059935C (en) * | 1998-01-21 | 2000-12-27 | 吉林大学 | Isometric nanometer boron nitride film and its preparation |
| US8101286B2 (en) * | 2008-06-26 | 2012-01-24 | GM Global Technology Operations LLC | Coatings for clutch plates |
| JP5189222B1 (en) * | 2012-07-18 | 2013-04-24 | サンアロイ工業株式会社 | Cemented carbide provided with low friction reducing ability, manufacturing method thereof, and cemented carbide tool |
| JP2016078137A (en) * | 2014-10-10 | 2016-05-16 | 新日鐵住金株式会社 | Cemented-carbide tool |
-
1994
- 1994-11-22 JP JP28785794A patent/JPH08144045A/en not_active Withdrawn
Cited By (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1059935C (en) * | 1998-01-21 | 2000-12-27 | 吉林大学 | Isometric nanometer boron nitride film and its preparation |
| US8101286B2 (en) * | 2008-06-26 | 2012-01-24 | GM Global Technology Operations LLC | Coatings for clutch plates |
| JP5189222B1 (en) * | 2012-07-18 | 2013-04-24 | サンアロイ工業株式会社 | Cemented carbide provided with low friction reducing ability, manufacturing method thereof, and cemented carbide tool |
| WO2014013715A1 (en) * | 2012-07-18 | 2014-01-23 | サンアロイ工業株式会社 | Superhard alloy imparted with low friction ability, method for producing same, and superhard tool |
| JP2016078137A (en) * | 2014-10-10 | 2016-05-16 | 新日鐵住金株式会社 | Cemented-carbide tool |
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