JP2875892B2 - Method of forming cubic boron nitride film - Google Patents

Method of forming cubic boron nitride film

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Publication number
JP2875892B2
JP2875892B2 JP2404168A JP40416890A JP2875892B2 JP 2875892 B2 JP2875892 B2 JP 2875892B2 JP 2404168 A JP2404168 A JP 2404168A JP 40416890 A JP40416890 A JP 40416890A JP 2875892 B2 JP2875892 B2 JP 2875892B2
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JP
Japan
Prior art keywords
nitrogen
cubic boron
boron nitride
forming
substrate
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.)
Expired - Lifetime
Application number
JP2404168A
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Japanese (ja)
Other versions
JPH04221059A (en
Inventor
敏郎 小林
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Mitsubishi Heavy Industries Ltd
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Mitsubishi Heavy Industries Ltd
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Priority to JP2404168A priority Critical patent/JP2875892B2/en
Publication of JPH04221059A publication Critical patent/JPH04221059A/en
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Description

【発明の詳細な説明】DETAILED DESCRIPTION OF THE INVENTION

【0001】[0001]

【産業上の利用分野】本発明は立方晶窒化ほう素膜の形
成方法に関し、機械一般の耐摩耗性を要する摺動部材等
の工具に適用されるものである。
BACKGROUND OF THE INVENTION 1. Field of the Invention The present invention relates to a method for forming a cubic boron nitride film, and is applied to a tool such as a sliding member which requires wear resistance in general machinery.

【0002】[0002]

【従来の技術】周知の如く、立方晶窒化ほう素はダイヤ
モンドに次いで硬く、鉄との親和力が小さいことより、
高温高圧で合成した粒を工具の刃先として実用されてお
り、近年は次のような方法で工具の刃先を立方晶窒化ほ
う素薄膜で被覆する研究が鋭意進められている。
2. Description of the Related Art As is well known, cubic boron nitride is harder than diamond and has a lower affinity for iron.
Granules synthesized at high temperature and high pressure have been practically used as cutting edges of tools, and in recent years, studies on coating the cutting edges of tools with a cubic boron nitride thin film by the following method have been earnestly made.

【0003】(1) イオンプレーティング方法;この方法
は、図1に示すような真空装置を用いて約10-3Torr
の窒素雰囲気で電子ビーム蒸発源1よりほう素2を蒸発
させ、熱フィラメント3と電極4間での放電によりほう
素蒸気及び窒素をイオン化し、基板6に印加した高周波
電力5の自己バイアスにより基板6にほう素イオン,窒
素イオンを引き寄せ、立方晶窒化ほう素を成膜する方法
である。
(1) Ion plating method: This method uses a vacuum apparatus as shown in FIG. 1 to obtain about 10 -3 Torr.
Boron 2 is evaporated from the electron beam evaporation source 1 in a nitrogen atmosphere, and boron vapor and nitrogen are ionized by a discharge between the hot filament 3 and the electrode 4, and the substrate is self-biased by the high-frequency power 5 applied to the substrate 6. 6 is a method of attracting boron ions and nitrogen ions to form a cubic boron nitride film.

【0004】(2) イオンビーム蒸着方法;この方法は、
図2に示すような真空装置を用いて電子ビーム蒸発源1
よりほう素2を蒸発させ、イオン銃7により窒素イオン
又は窒素とアルゴンの混合イオンを0.5 〜1KV程度に
加速し、立方晶窒化ほう素を成膜する方法である。
(2) Ion beam evaporation method;
Electron beam evaporation source 1 using a vacuum device as shown in FIG.
In this method, boron 2 is evaporated, and nitrogen ions or mixed ions of nitrogen and argon are accelerated by an ion gun 7 to about 0.5 to 1 KV to form cubic boron nitride.

【0005】その際、成膜の前にイオン銃の加速電圧を
数KV以上とすると、ほう素及び窒素が基板6中に注入
され、同時に基板6の元素はスパッタされて飛び出すた
め、数百A以上のほう素,窒素,及び基板の元素が混合
されたミキシング層が形成される。これにひきつづき、
上記の立方晶窒化ほう素のできる条件で成膜すると、基
材と立方晶窒化ほう素皮膜との間に明確な界面がなくな
り、組成が連続し、応力集中も少ない密着力の良い皮膜
が得られる。
At this time, if the acceleration voltage of the ion gun is set to several KV or more before film formation, boron and nitrogen are implanted into the substrate 6 and at the same time, the elements of the substrate 6 are sputtered and fly out. A mixing layer in which the above-described boron, nitrogen, and substrate elements are mixed is formed. Following this,
When the film is formed under the above-mentioned conditions of cubic boron nitride, a clear interface between the substrate and the cubic boron nitride film disappears, the composition is continuous, the stress concentration is small, and a film with good adhesion is obtained. Can be

【0006】[0006]

【発明が解決しようとする課題】しかしながら、従来技
術によれば、高速鋼や超硬等の工具材料の表面に窒化ほ
う素皮膜を形成した場合、以下に述べる問題点を有す
る。
However, according to the prior art, when a boron nitride film is formed on the surface of a tool material such as high-speed steel or carbide, there are the following problems.

【0007】(1) イオンプレ−ティング方法; この方法では、図3に示すように高周波の自己バイアス
電圧が基板にかかっているため、複雑形状の基板8の場
合でも等電位線9は基材表面と平行にできるため、イオ
ンは基板表面に垂直に入射でき付き回り性が良く、特に
複雑形状基板への立方晶BN薄膜形成において生産性が
高い。しかし、自己バイアス電圧は真空容器内のインピ
−ダンスより制限があり、実質的には1KV以下で大き
くできないので、イオンミキシング効果が小さい。即
ち、イオンが注入される深さが浅いため、ほう素,窒
素,基材元素の厚い混合層ができないため、立方晶窒化
ほう素の大きな内部応力及び外力により容易に剥離す
る。つまり、十分な密着力が得られない。なお、図3に
おいて、10はイオンの軌跡である。
(1) Ion plating method: In this method, a high frequency self-bias voltage is applied to the substrate as shown in FIG. because it parallel to, ions rather goodness around resistance with possible incident perpendicular to the substrate surface, in particular
Productivity in cubic BN thin film formation on complex shaped substrates
high. However, since the self-bias voltage is more limited than the impedance in the vacuum vessel and can not be substantially increased below 1 KV , the ion mixing effect is small. That is, since the depth at which the ions are implanted is small, a thick mixed layer of boron, nitrogen, and the base element cannot be formed, and thus the cubic boron nitride is easily peeled off due to the large internal stress and external force. That is, a sufficient adhesive force cannot be obtained. In FIG. 3, reference numeral 10 denotes a locus of ions.

【0008】(2) イオン蒸着方法; この方法では、前述のようにイオン銃の加速電圧Vaを
変えることにより厚いミキシング層が得られるため、密
着力の良い立方晶窒化ほう素皮膜をえることができる
しかし、図4に示すように加速されたイオンは直進性が
あり、複雑形状の基板8の場合、イオンの入射方向と垂
直に近い面しか成膜できないため、図5のように基材を
動かすか、イオン銃を動かすことによってイオンが複雑
形状基材の表面に垂直に入射するようにしてやる必要が
ある。また、その際、イオンが斜めに入射する基材表面
はスパッタリングにより減肉するため、図5のようにマ
スキング11をする必要が生じる。従って、複雑形状基板
への立方晶BN薄膜の形成においては生産性が低い。
に、イオン銃は現在未だ発展途上の技術であるため、大
電流密度で大面積を取り出せるものが開発されておら
ず、立方晶窒化ほう素の成膜速度自体もイオンプレ−テ
ィング方法に比較して小さい。
(2) Ion vapor deposition method: In this method, since a thick mixing layer can be obtained by changing the acceleration voltage Va of the ion gun as described above, a cubic boron nitride film having good adhesion can be obtained. I can .
However, as shown in FIG. 4, the accelerated ions have rectilinearity, and in the case of the substrate 8 having a complicated shape, only the surface perpendicular to the incident direction of the ions can be formed, so that the base material is moved as shown in FIG. 5. Alternatively, it is necessary to move the ion gun so that the ions are perpendicularly incident on the surface of the substrate having a complicated shape. At this time, the surface of the base material on which the ions are obliquely incident is reduced in thickness by sputtering, so that it is necessary to mask 11 as shown in FIG. Therefore, complex shaped substrates
Productivity is low in forming a cubic BN thin film. Further, since the ion gun is still a developing technology, a device capable of extracting a large area with a large current density has not been developed, and the deposition rate of cubic boron nitride itself is lower than that of the ion plating method. small.

【0009】本発明は上記事情に鑑みてなされたもの
で、基材との密着力が強く、かつ複雑な形状の基材でも
高い生産性で形成できる立方晶ほう素膜の形成方法を提
供することを目的とする。
The present invention has been made in view of the above circumstances, and provides a method of forming a cubic boron film having high adhesion to a substrate and capable of forming a substrate having a complicated shape with high productivity. The purpose is to:

【0010】[0010]

【課題を解決するための手段】本発明は、基板表面に加
速電圧を高めたイオン銃により、数KV以上で窒素又は
アルゴン+窒素ガスイオンを照射しつつほう素を蒸着さ
せて基板表面に窒素,ほう素及び基板元素の混合層を形
成する第1工程と、上記イオン銃の加速電圧を0.5〜
1KVで同様の処理を行い上記混合層上に立方晶窒化ほ
う素の薄膜を形成する第2工程と、フィラメントと電極
間の放電により窒素又は窒素+アルゴンガスをイオン化
しつつ、ほう素を蒸着させて前記薄膜上に立方晶ほう素
膜を形成する第3工程とを具備することを特徴とする立
方晶ほう素膜の形成方法である。
SUMMARY OF THE INVENTION According to the present invention, boron is deposited on a substrate surface by irradiating the substrate surface with nitrogen or argon + nitrogen gas ions at a rate of several kV or more by an ion gun with an increased accelerating voltage. a first step of forming a mixed layer of boron and the substrate element, 0.5 the acceleration voltage of the ion gun
A second step of forming a cubic boron nitride thin film on the mixed layer by performing the same treatment at 1 KV, and depositing boron while ionizing nitrogen or nitrogen + argon gas by discharging between the filament and the electrode. a cubic boron Motomaku forming method, characterized by comprising a third step of forming a cubic boron Motomaku on the thin film Te.

【0011】[0011]

【作用】本発明においては、イオン蒸着方法で初期にほ
う素を蒸着しながら数KV以上の加速電圧で窒素イオン
又は窒素とアルゴンの混合イオンを照射し、厚いミキシ
ング層を形成した後、0.5 〜1KV程度の加速電圧で薄
い立方晶窒化ホウ素皮膜を形成し、密着性を確保し、ひ
きつづき高速度で大面積,複雑形状の基材の成膜が可能
なイオンプレ−ティング方法で立方晶窒化ホウ素皮膜を
厚膜化することにより、高い生産性が確保できる。
According to the present invention, a thick mixing layer is formed by irradiating nitrogen ions or mixed ions of nitrogen and argon at an acceleration voltage of several KV or more while depositing boron initially by an ion deposition method. A thin cubic boron nitride film is formed at an accelerating voltage of about 1 KV to secure adhesion, and it is possible to form a large-area, complex-shaped substrate at high speed.
The coating cubic boron nitride film by a method - a Yi Onpure
By increasing the film thickness , high productivity can be secured.

【0012】[0012]

【実施例】以下、本発明の一実施例について説明する。An embodiment of the present invention will be described below.

【0013】即ち、本実施例では、まず、複雑形状な基
板8表面に加速電圧を高めたイオン銃7により、窒素又
はアルゴン+窒素ガスイオンを照射しつつ、ほう素を蒸
着させて基板8表面に窒素,ほう素及び基板元素の混合
層を形成した。つづいて、上記イオン銃7の加速電圧を
低下させ、同様の処理を行って上記混合層上に立方晶窒
化ほう素の薄膜を形成した。更に、熱フィラメント3と
電極4間の放電により窒素又は窒素+アルゴンガスをイ
オン化しつつ、ほう素を蒸着させて前記薄膜上に目的と
する立方晶ほう素膜を形成した。
That is, in the present embodiment, first, boron is vapor-deposited while irradiating nitrogen or argon + nitrogen gas ions with an ion gun 7 having an increased acceleration voltage on the surface of the substrate 8 having a complicated shape. Then, a mixed layer of nitrogen, boron and a substrate element was formed. Subsequently, the acceleration voltage of the ion gun 7 was lowered, and the same processing was performed to form a cubic boron nitride thin film on the mixed layer. Further, while ionizing nitrogen or nitrogen + argon gas by the discharge between the hot filament 3 and the electrode 4, boron was deposited to form a target cubic boron film on the thin film.

【0014】後掲する表1は、比較例及び本発明の実施
例1、2の成膜条件及び皮膜の評価結果を示す。ただ
し、表1において、条件Aはミキシング条件,条件Bは
立方晶窒化ほう素成膜条件、条件Cは立方晶窒化ホウ素
成膜条件、V1,V2 はイオン加速電圧[KV]、
1 ,I2 はイオン電流密度[μA/cm2 ]、Wは高周
波電力[W]、Pは真空槽内圧力[Torr]、有無と
はイオンバード(前処理)の有無をいう。
Table 1 below shows the film forming conditions and the evaluation results of the films of the comparative example and Examples 1 and 2 of the present invention. However, in Table 1, condition A is mixing condition, condition B is cubic boron nitride film forming condition, condition C is cubic boron nitride film forming condition, V 1 and V 2 are ion acceleration voltage [KV],
I 1 and I 2 are the ion current density [μA / cm 2 ], W is the high frequency power [W], P is the pressure in the vacuum chamber [Torr], and the presence / absence refers to the presence / absence of ion bird (pretreatment).

【0015】また、表1において、成膜は比較例1では
図1に示すイオンプレーティング装置を、比較例2では
図2に示すイオン蒸着装置を、本発明の実施例1,2で
は両者を用いた。また、密着性の評価は、成膜後の光学
顕微鏡観察と切削試験により行った。ここで、切削条件
は、硬さHv170 のSCM415 を用い切削速度100 m/
min で、切削長25mmを切り込み深さ0.2mm 断続的に繰返
し切削した。切削寿命は、工具刃先の逃げ面の磨耗幅V
B を逐次測定し、VB が0.2mm になった時の切削回数と
比較して示した。比較例1では、成膜中及び成膜後にう
ろこ状に皮膜が剥離し、切削試験を行うことができなか
った。
In Table 1, in Comparative Example 1, the ion plating apparatus shown in FIG. 1 was used, in Comparative Example 2, the ion deposition apparatus shown in FIG. 2 was used, and in Examples 1 and 2 of the present invention, both were used. Using. The evaluation of adhesion was performed by optical microscope observation after film formation and a cutting test. Here, the cutting conditions were as follows: SCM415 having a hardness of Hv170 was used and the cutting speed was 100 m /
At min, the cutting length was 25 mm and the cutting depth was 0.2 mm. The cutting life is the wear width V of the flank of the tool tip.
B was measured successively and shown in comparison with the number of cuts when VB was 0.2 mm. In Comparative Example 1, the coating peeled in a scaly shape during and after the film formation, and a cutting test could not be performed.

【0016】これに対し、本発明の実施例では切削試験
においても、基材と立方晶窒化ホウ素皮膜界面、及びイ
オン蒸着による立方晶窒化ホウ素皮膜とイオンプレーテ
ィングによった立方晶窒化ホウ素皮膜の界面両者とも剥
離は認められず、良好な密着性を示した。また、切削寿
命も比較例2のイオン蒸着法によるものと略同様で、窒
化チタン皮膜の約2.5 倍が得られた。
On the other hand, in the embodiment of the present invention, even in the cutting test, the interface between the substrate and the cubic boron nitride film, and the cubic boron nitride film formed by ion vapor deposition and the cubic boron nitride film formed by ion plating were formed. No delamination was observed at both interfaces, indicating good adhesion. The cutting life was also substantially the same as that obtained by the ion vapor deposition method of Comparative Example 2, and was about 2.5 times that of the titanium nitride film.

【0017】[0017]

【発明の効果】以上詳述した如く本発明によれば、基材
との密着力が強く、かつ複雑な形状の基材でも高い生産
性で形成できる立方晶ほう素膜の形成方法を提供でき
る。
As described above in detail, according to the present invention, it is possible to provide a method of forming a cubic boron film having a high adhesion to a substrate and a high productivity even with a substrate having a complicated shape. .

【0018】[0018]

【表1】 [Table 1]

【図面の簡単な説明】[Brief description of the drawings]

【図1】イオンプレーティング装置の説明図。FIG. 1 is an explanatory diagram of an ion plating apparatus.

【図2】イオン蒸着装置の説明図。FIG. 2 is an explanatory diagram of an ion deposition apparatus.

【図3】イオンプレーティングによる複雑形状基材の成
膜の説明図。
FIG. 3 is an explanatory diagram of film formation of a substrate having a complicated shape by ion plating.

【図4】イオン蒸着法による複雑形状基材の成膜の説明
図。
FIG. 4 is an explanatory diagram of film formation of a complex-shaped substrate by an ion vapor deposition method.

【図5】イオン蒸着法による複雑形状基材の成膜の説明
図。
FIG. 5 is an explanatory diagram of film formation of a complex-shaped substrate by an ion vapor deposition method.

【符号の説明】[Explanation of symbols]

1…電子ビーム蒸発源,2…ホウ素、3…熱フィラメン
ト、4…電極、5…講習は電力、6,8…基板、7…イ
オン銃、9…等電位線。
Reference numeral 1 denotes an electron beam evaporation source, 2 denotes boron, 3 denotes a hot filament, 4 denotes an electrode, 5 denotes a course of electric power, 6, 8 ... a substrate, 7 ... an ion gun, 9 ... equipotential lines.

Claims (1)

(57)【特許請求の範囲】(57) [Claims] 【請求項1】 基板表面に加速電圧を高めたイオン銃に
より、数KV以上で窒素又はアルゴン+窒素ガスイオン
を照射しつつほう素を蒸着させて基板表面に窒素,ほう
素及び基板元素の混合層を形成する第1工程と、上記イ
オン銃の加速電圧を0.5〜1KVで同様の処理を行い
上記混合層上に立方晶窒化ほう素の薄膜を形成する第2
工程と、フィラメントと電極間の放電により窒素又は窒
素+アルゴンガスをイオン化しつつ、ほう素を蒸着させ
て前記薄膜上に立方晶ほう素膜を形成する第3工程とを
具備することを特徴とする立方晶ほう素膜の形成方法。
1. A method of mixing nitrogen, boron and a substrate element on a substrate surface by depositing boron while irradiating nitrogen or argon + nitrogen gas ions at several KV or more with an ion gun having an increased accelerating voltage on the substrate surface. A first step of forming a layer and a second step of forming a thin film of cubic boron nitride on the mixed layer by performing the same treatment at an acceleration voltage of the ion gun of 0.5 to 1 KV .
A step, and characterized by comprising a third step of forming a filament and while nitrogen or nitrogen + argon gas by a discharge between the electrodes to ionize, boron cubic on the thin layer by depositing a boron Motomaku Method of forming a cubic boron film.
JP2404168A 1990-12-20 1990-12-20 Method of forming cubic boron nitride film Expired - Lifetime JP2875892B2 (en)

Priority Applications (1)

Application Number Priority Date Filing Date Title
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Applications Claiming Priority (1)

Application Number Priority Date Filing Date Title
JP2404168A JP2875892B2 (en) 1990-12-20 1990-12-20 Method of forming cubic boron nitride film

Publications (2)

Publication Number Publication Date
JPH04221059A JPH04221059A (en) 1992-08-11
JP2875892B2 true JP2875892B2 (en) 1999-03-31

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Country Link
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Publication number Priority date Publication date Assignee Title
JP2011524640A (en) * 2008-06-11 2011-09-01 インテバック・インコーポレイテッド Solar cell forming method and solar cell
US8749053B2 (en) 2009-06-23 2014-06-10 Intevac, Inc. Plasma grid implant system for use in solar cell fabrications
CN106847736B (en) 2011-11-08 2020-08-11 因特瓦克公司 Substrate processing system and method
TWI570745B (en) 2012-12-19 2017-02-11 因特瓦克公司 Grid for plasma ion implant

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* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
JPS6176662A (en) * 1984-09-21 1986-04-19 Nippon Telegr & Teleph Corp <Ntt> Method and device for forming thin film

Also Published As

Publication number Publication date
JPH04221059A (en) 1992-08-11

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