JPH0742571B2 - CBN coating method - Google Patents
CBN coating methodInfo
- Publication number
- JPH0742571B2 JPH0742571B2 JP61162142A JP16214286A JPH0742571B2 JP H0742571 B2 JPH0742571 B2 JP H0742571B2 JP 61162142 A JP61162142 A JP 61162142A JP 16214286 A JP16214286 A JP 16214286A JP H0742571 B2 JPH0742571 B2 JP H0742571B2
- Authority
- JP
- Japan
- Prior art keywords
- cbn
- film
- coating
- temperature
- coating method
- 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
Links
- 238000000576 coating method Methods 0.000 title claims description 20
- 239000011248 coating agent Substances 0.000 claims description 14
- IJGRMHOSHXDMSA-UHFFFAOYSA-N nitrogen Substances N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 claims description 3
- 229910052757 nitrogen Inorganic materials 0.000 claims description 3
- -1 nitrogen ions Chemical class 0.000 claims description 3
- 239000000463 material Substances 0.000 claims description 2
- 230000001678 irradiating effect Effects 0.000 claims 1
- 239000013080 microcrystalline material Substances 0.000 claims 1
- 238000000034 method Methods 0.000 description 13
- 229910052751 metal Inorganic materials 0.000 description 5
- 239000002184 metal Substances 0.000 description 5
- 150000002500 ions Chemical class 0.000 description 4
- 238000004544 sputter deposition Methods 0.000 description 4
- 238000002441 X-ray diffraction Methods 0.000 description 3
- 238000007796 conventional method Methods 0.000 description 3
- 238000007733 ion plating Methods 0.000 description 3
- 239000002245 particle Substances 0.000 description 3
- 238000005240 physical vapour deposition Methods 0.000 description 3
- 238000003746 solid phase reaction Methods 0.000 description 3
- 239000000758 substrate Substances 0.000 description 3
- 239000012808 vapor phase Substances 0.000 description 3
- 229910052582 BN Inorganic materials 0.000 description 2
- PZNSFCLAULLKQX-UHFFFAOYSA-N Boron nitride Chemical compound N#B PZNSFCLAULLKQX-UHFFFAOYSA-N 0.000 description 2
- 239000011230 binding agent Substances 0.000 description 2
- 230000003197 catalytic effect Effects 0.000 description 2
- 239000002131 composite material Substances 0.000 description 2
- 238000005520 cutting process Methods 0.000 description 2
- 239000007789 gas Substances 0.000 description 2
- 229910052759 nickel Inorganic materials 0.000 description 2
- 238000005121 nitriding Methods 0.000 description 2
- 239000011347 resin Substances 0.000 description 2
- 229920005989 resin Polymers 0.000 description 2
- 229910000997 High-speed steel Inorganic materials 0.000 description 1
- 239000000853 adhesive Substances 0.000 description 1
- 230000001070 adhesive effect Effects 0.000 description 1
- 230000015572 biosynthetic process Effects 0.000 description 1
- 238000006243 chemical reaction Methods 0.000 description 1
- 150000001875 compounds Chemical class 0.000 description 1
- 239000013078 crystal Substances 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 238000004070 electrodeposition Methods 0.000 description 1
- 238000005516 engineering process Methods 0.000 description 1
- 238000000227 grinding Methods 0.000 description 1
- 238000003754 machining Methods 0.000 description 1
- 150000002739 metals Chemical class 0.000 description 1
- 238000007747 plating Methods 0.000 description 1
- 239000000843 powder Substances 0.000 description 1
- 239000002994 raw material Substances 0.000 description 1
- 239000000376 reactant Substances 0.000 description 1
- 239000004065 semiconductor Substances 0.000 description 1
- 238000005245 sintering Methods 0.000 description 1
- 238000005477 sputtering target Methods 0.000 description 1
- 238000003786 synthesis reaction Methods 0.000 description 1
- 238000010189 synthetic method Methods 0.000 description 1
Landscapes
- Physical Vapour Deposition (AREA)
Description
【発明の詳細な説明】 〔産業上の利用分野〕 本発明は切削工具あるいは紙工機械等の刃物類等に適用
される超硬質皮膜であるCBNコーテイング、又、半導体
分野における絶縁膜としても利用可能なCBNコーテイン
グに関する。DETAILED DESCRIPTION OF THE INVENTION [Industrial field of application] The present invention can also be used as a CBN coating which is a super hard coating applied to cutting tools or cutting tools such as paperworking machines, and also as an insulating film in the semiconductor field. About CBN coating.
CBN（立方晶窒化ホウ素）は、天然には存在しない人工
合成化合物であり、従来は六方晶窒化ホウ素（以下ｈ−
BNと記す）を超高温・高圧（温度1600K以上、圧力40Kba
r以上）処理することによつて得られていた。CBN (cubic boron nitride) is an artificial synthetic compound that does not exist in nature, and is conventionally hexagonal boron nitride (h-
BN) is ultra high temperature and high pressure (temperature over 1600K, pressure 40Kba
It was obtained by processing.
しかし、従来法では粉末あるいは粒状でしか製造でき
ず、これを研削砥石等の工具として使用する場合には、
樹脂あるいは金属を結合材として焼結して用いるかある
いはCBN粒子を金属めつき膜中に分散させた電着工具と
して用いるという方法が採られている。However, the conventional method can only be manufactured in powder or granular form, and when it is used as a tool such as a grinding wheel,
A method of sintering resin or metal as a binder or using it as an electrodeposition tool in which CBN particles are dispersed in a metal plating film is adopted.
しかし、これらの方法では、（１）CBNが粒子であるた
め寸法精度が不良（最小でも＃3000;平均粒径５〜６μ
ｍ）で精密加工に使用できない、（２）樹脂や金属を結
合材としているため付着力（CBN保持力）が低い、
（３）超高温高圧処理のため生産性が低くコスト高とな
る、等の欠点を有している。However, in these methods, (1) dimensional accuracy is poor because CBN is particles (minimum # 3000; average particle size 5 to 6 μ).
m) can not be used for precision processing, (2) Adhesive force (CBN holding force) is low because resin or metal is used as a binder,
(3) It has drawbacks such as low productivity and high cost due to ultra-high temperature and high pressure treatment.
このため、CBNをコーテイングすることができれば、上
記問題点が解消されるため、各種PVD（物理的蒸着）法
によるCBNコーテイングが鋭意研究中であるがいまだ成
功には到つていない。Therefore, if CBN can be coated, the above-mentioned problems will be solved. Therefore, CBN coating by various PVD (physical vapor deposition) methods is under intensive research, but has not yet succeeded.
従来の高温高圧処理による粒子状CBNの利用に代わる新
しいCBNの利用法としてコーテイングがあり、特にサブ
ミクロンオーダーの超精密加工用工具としてはCBNコー
テイングが必要不可欠であるとも云われている。このCB
NコーテイングとしてPVD法、中でもイオンプレーテイン
グ、スパツタリング法による方法が研究されているが、
まだ完全なCBNコーテイングは完成されていない。すな
わち、これらの方法はＢ又は六方晶BNを原料として気相
反応によりCBNを析出しようとするものであるが、すで
に述べたようにCBNは超高温・高圧処理で合成されるも
のであり、これらの方法は、低温処理であるため合成が
困難であるためと思われる。又このような気相コーテイ
ング法は得られる皮膜は基本的には非平衡状態の膜であ
り、元来、非晶質膜になりやすく、この点もCBN合成困
難な理由と思われる。There is coating as a new method of using CBN instead of the conventional use of particulate CBN by high-temperature and high-pressure treatment, and it is said that CBN coating is indispensable especially as a tool for ultra-precision machining on the order of submicrons. This CB
As the N coating, PVD method, especially ion plating and sputtering method are being studied.
The complete CBN coating is not yet complete. That is, these methods are intended to deposit CBN by vapor phase reaction using B or hexagonal BN as a raw material, but as already mentioned, CBN is synthesized by ultra-high temperature / high pressure treatment. It is considered that the method of 1) is difficult to synthesize because it is a low temperature treatment. In addition, the film obtained by such a vapor-phase coating method is basically a film in a non-equilibrium state, and by nature, it tends to be an amorphous film, which is also the reason why CBN synthesis is difficult.
本発明は上記従来法におけるような欠点を解消したCBN
コーテイングを形成させる方法を提供しようとするもの
である。The present invention eliminates the drawbacks of the conventional method described above.
It is intended to provide a method of forming a coating.
本発明は母材上にあらかじめ非晶質又は微結晶状のBN皮
膜をコーテイングした後、同皮膜に窒素イオンを照射し
CBNを形成することを特徴とするCBN被覆法である。According to the present invention, after coating an amorphous or microcrystalline BN film on a base material in advance, the film is irradiated with nitrogen ions.
It is a CBN coating method characterized by forming CBN.
従来の手法では非晶質BN膜になることが多いが、本発明
はこの非晶質膜の非平衡エネルギーを利用して固相反応
によりCBNを合成するものである。すなわち気相法によ
つて非晶質膜を作成しその後この皮膜をイオン照射処理
することにより固相反応を生じさせてCBNを合成するも
のである。又、このBN中にFe,Ni,Cr等の触媒金属を添加
すると固相反応条件が緩和されるためさらに有利とな
る。The conventional method often produces an amorphous BN film, but the present invention utilizes the nonequilibrium energy of this amorphous film to synthesize CBN by a solid-phase reaction. That is, an amorphous film is formed by a vapor phase method, and then this film is subjected to an ion irradiation treatment to cause a solid phase reaction to synthesize CBN. Further, it is more advantageous to add catalytic metals such as Fe, Ni and Cr to this BN because the solid-phase reaction conditions are relaxed.
さらに、厚膜が必要な場合には本発明方法を数回繰返す
ことにより所望の厚みの膜を得ることができる。Further, when a thick film is required, the method of the present invention can be repeated several times to obtain a film having a desired thickness.
非晶質膜には大きな非平衡エネルギーが存在するため、
通常の合成法に比べて低温・低圧で処理可能である。
又、本発明方法によれば従来不可能であつたCBNコーテ
イングが可能となる。Since there is a large nonequilibrium energy in an amorphous film,
It can be processed at low temperature and low pressure as compared with ordinary synthetic methods.
Further, according to the method of the present invention, CBN coating, which has hitherto been impossible, can be performed.
〔実験例１〕 30mm×30mm×5mm厚さの高速度鋼（SKH55）を基板とし
て、その表面に反応性高周波イオンプレーテイングおよ
び高周波スパツタリング法により、BNをコーテイングし
た。膜厚は１μｍでありコーテイング条件は以下の通り
である。[Experimental Example 1] A high-speed steel (SKH55) having a thickness of 30 mm x 30 mm x 5 mm was used as a substrate, and BN was coated on its surface by reactive high frequency ion plating and high frequency sputtering. The film thickness is 1 μm, and the coating conditions are as follows.
１）反応性高周波イオンプレーテイング 電子銃出力:10KV×0.2A 高周波出力:600W バイアス電圧:500V 反応ガス（N2）流量:12cc./min 基板温度：常温 ２）高周波スパツタリング ターゲツト:100mmφ×mmt、BN純度99％ 高周波電力:300W 雰囲気ガス:N2（20mmTorr） 基板温度：常温 以上の方法で得られた各BN膜のＸ線回折分析を実施した
結果、いずれの皮膜からも回折ピークは認められず、非
晶質状であつた。1) Reactive high frequency ion plating Electron gun output: 10KV × 0.2A High frequency output: 600W Bias voltage: 500V Reactant gas (N 2 ) Flow rate: 12cc./min Substrate temperature: room temperature 2) High frequency sputtering target: 100mmφ × mmt, BN purity 99% High frequency power: 300W Atmosphere gas: N 2 (20mmTorr) Substrate temperature: normal temperature As a result of X-ray diffraction analysis of each BN film obtained by the above method, diffraction peaks were observed from all films. Instead, it was amorphous.
〔実験例２〕 実験例１で述べた高周波スパツタリング法において、タ
ーゲツトとして、Ni又はFeを1.3面積％含む複合ターゲ
ツト（BN＋Ni又はBN＋Fe）を用い、実験例１の高周波ス
パツタリングと同じ条件でBN＋NiおよびBN＋Fe複合膜を
作成し、その結晶構造をＸ線回折分析で調べた結果、い
ずれの皮膜も非晶質状であつた。[Experimental Example 2] In the high frequency sputtering method described in Experimental Example 1, a composite target (BN + Ni or BN + Fe) containing 1.3 area% of Ni or Fe was used as a target, and BN + Ni and BN + Fe were used under the same conditions as the high frequency sputtering of Experimental Example 1. As a result of forming a composite film and examining its crystal structure by X-ray diffraction analysis, all the films were amorphous.
実験例１および実験例２で作成した４種類の皮膜に窒素
イオン照射処理を実施した。イオン照射は、N2中のグロ
ー放電によるイオン窒化処理とした。イオン窒化条件お
よび処理後の皮膜のＸ線回折分析結果を表１に示す。Nitrogen ion irradiation treatment was performed on the four types of coatings prepared in Experimental Example 1 and Experimental Example 2. The ion irradiation was an ion nitriding treatment by glow discharge in N 2 . Table 1 shows the results of X-ray diffraction analysis of the film after the ion nitriding conditions and the treatment.
この結果、いずれの皮膜もCBNとなつていることが明ら
かとなり、又、触媒金属を添加することにより、より低
温、低加速電圧下で合成可能となることが明らかとなつ
た。As a result, it was clarified that all of the coatings became CBN, and it was clarified that by adding a catalytic metal, it could be synthesized at lower temperature and lower accelerating voltage.
〔発明の効果〕 以上、実施例で詳述したように、本発明方法によれば、
従来超高温・高圧でしか合成できなかつたCBNが、低温
・低圧で合成でき、しかも、従来は粒状でしか合成でき
なかつたものを、コーテイングの形で利用することがで
き、工業的に意義あるものである。 [Effects of the Invention] As described above in detail in the examples, according to the method of the present invention,
CBN, which was previously only synthesized at ultra-high temperature and high pressure, can be synthesized at low temperature and low pressure, and can be used in the form of coating, which was conventionally only granular, and is industrially significant. It is a thing.
───────────────────────────────────────────────────── フロントページの続き (72)発明者 中川 義清 広島県広島市西区観音新町４丁目６番22号 三菱重工業株式会社広島研究所内 (72)発明者 花中 勝保 広島県広島市西区観音新町４丁目６番22号 三菱重工業株式会社広島研究所内 (56)参考文献 特開 昭57−174453（ＪＰ，Ａ) ＪＡＰＡＮＥＳＥ ＪＯＵＲＮＡＬ Ｏ Ｆ ＡＰＰＬＩＥＤ ＰＨＩＳＩＣＳ Ｖ ｏｌ．22，Ｎｏ．３，ＭＡＲＣＨ，1983 Ｐ．Ｌ171−Ｌ172 ─────────────────────────────────────────────────── ─── Continuation of front page (72) Yoshiyoshi Nakagawa Yoshinaka Nakagawa 4-6-22 Kannon Shinmachi, Nishi-ku, Hiroshima City, Hiroshima Prefecture Mitsubishi Heavy Industries, Ltd. Hiroshima Research Laboratory (72) Inventor Katsuho Hananaka 4 Kannon Shinmachi, Nishi-ku, Hiroshima City, Hiroshima Prefecture 6-22 No. 22 Hiroshima Research Laboratory, Mitsubishi Heavy Industries, Ltd. (56) Reference JP-A-57-174453 (JP, A) JAPANESE JOURNAL OF APPLIED PHISICS Vol. 22, No. 3, MARCH, 1983 P.I. L171-L172
Claims (1)
BN皮膜をコーテイングした後、同皮膜に窒素イオンを照
射しCBNを形成することを特徴とするCBN被覆法。1. An amorphous or microcrystalline material is previously formed on a base material.
A CBN coating method comprising coating a BN film and then irradiating the film with nitrogen ions to form CBN.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| JP61162142A JPH0742571B2 (en) | 1986-07-11 | 1986-07-11 | CBN coating method |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| JP61162142A JPH0742571B2 (en) | 1986-07-11 | 1986-07-11 | CBN coating method |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| JPS6318050A JPS6318050A (en) | 1988-01-25 |
| JPH0742571B2 true JPH0742571B2 (en) | 1995-05-10 |
Family
ID=15748832
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| JP61162142A Expired - Lifetime JPH0742571B2 (en) | 1986-07-11 | 1986-07-11 | CBN coating method |
Country Status (1)
| Country | Link |
|---|---|
| JP (1) | JPH0742571B2 (en) |
Families Citing this family (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JPS63262457A (en) * | 1987-04-20 | 1988-10-28 | Nissin Electric Co Ltd | Preparation of boron nitride film |
| JPH0216847U (en) * | 1988-07-20 | 1990-02-02 | ||
| JPH083720Y2 (en) * | 1988-11-25 | 1996-01-31 | エヌエスケー・ワーナー株式会社 | Fixed structure such as one-way clutch outer ring |
| JP3298059B2 (en) * | 1995-01-20 | 2002-07-02 | エヌオーケー株式会社 | Stator |
| FI980884A7 (en) * | 1998-04-22 | 1999-10-23 | Metso Paper Inc | Parts of a paper/board or finishing machine that are subject to high wear and tear and a method for manufacturing these parts |
Family Cites Families (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JPS57174453A (en) * | 1981-04-17 | 1982-10-27 | Sumitomo Electric Ind Ltd | Coated superhard alloy tool |
| JPS5980775A (en) * | 1982-11-01 | 1984-05-10 | Sumitomo Electric Ind Ltd | Hard thin film manufacturing method |
| JPS6063372A (en) * | 1983-09-19 | 1985-04-11 | Agency Of Ind Science & Technol | Manufacture of thin boron nitride film of high hardness |
| JPS60181262A (en) * | 1984-02-29 | 1985-09-14 | Agency Of Ind Science & Technol | Production of boron nitride film having high hardness |
| JPS6176662A (en) * | 1984-09-21 | 1986-04-19 | Nippon Telegr & Teleph Corp <Ntt> | Method and device for forming thin film |
-
1986
- 1986-07-11 JP JP61162142A patent/JPH0742571B2/en not_active Expired - Lifetime
Non-Patent Citations (1)
| Title |
|---|
| ＪＡＰＡＮＥＳＥＪＯＵＲＮＡＬＯＦＡＰＰＬＩＥＤＰＨＩＳＩＣＳＶｏｌ．２２，Ｎｏ．３，ＭＡＲＣＨ，１９８３Ｐ．Ｌ１７１−Ｌ１７２ |
Also Published As
| Publication number | Publication date |
|---|---|
| JPS6318050A (en) | 1988-01-25 |
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