JPH0830264B2 - Method for forming multilayer film - Google Patents
Method for forming multilayer filmInfo
- Publication number
- JPH0830264B2 JPH0830264B2 JP5136887A JP5136887A JPH0830264B2 JP H0830264 B2 JPH0830264 B2 JP H0830264B2 JP 5136887 A JP5136887 A JP 5136887A JP 5136887 A JP5136887 A JP 5136887A JP H0830264 B2 JPH0830264 B2 JP H0830264B2
- Authority
- JP
- Japan
- Prior art keywords
- film
- substrate
- multilayer film
- tin
- bias voltage
- 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
- 238000000034 method Methods 0.000 title claims description 14
- ATJFFYVFTNAWJD-UHFFFAOYSA-N Tin Chemical compound [Sn] ATJFFYVFTNAWJD-UHFFFAOYSA-N 0.000 claims description 20
- 239000000758 substrate Substances 0.000 claims description 19
- 239000011248 coating agent Substances 0.000 claims description 14
- 238000000576 coating method Methods 0.000 claims description 14
- 238000007733 ion plating Methods 0.000 claims description 10
- 239000013078 crystal Substances 0.000 description 7
- 230000000694 effects Effects 0.000 description 7
- 230000001070 adhesive effect Effects 0.000 description 4
- 238000010586 diagram Methods 0.000 description 4
- 230000003628 erosive effect Effects 0.000 description 4
- 238000005530 etching Methods 0.000 description 4
- 239000000853 adhesive Substances 0.000 description 3
- 238000010894 electron beam technology Methods 0.000 description 3
- 238000002441 X-ray diffraction Methods 0.000 description 2
- 230000001687 destabilization Effects 0.000 description 2
- 150000002500 ions Chemical class 0.000 description 2
- 239000000463 material Substances 0.000 description 2
- 238000001228 spectrum Methods 0.000 description 2
- 238000005299 abrasion Methods 0.000 description 1
- 238000004458 analytical method Methods 0.000 description 1
- 230000015572 biosynthetic process Effects 0.000 description 1
- 239000000919 ceramic Substances 0.000 description 1
- 150000001875 compounds Chemical class 0.000 description 1
- 230000007423 decrease Effects 0.000 description 1
- 238000000151 deposition Methods 0.000 description 1
- 229910003460 diamond Inorganic materials 0.000 description 1
- 239000010432 diamond Substances 0.000 description 1
- 238000005516 engineering process Methods 0.000 description 1
- 238000011156 evaluation Methods 0.000 description 1
- 238000001704 evaporation Methods 0.000 description 1
- 238000010438 heat treatment Methods 0.000 description 1
- 239000002184 metal Substances 0.000 description 1
- 239000012495 reaction gas Substances 0.000 description 1
- 229910001220 stainless steel Inorganic materials 0.000 description 1
- 239000010935 stainless steel Substances 0.000 description 1
- 238000004381 surface treatment 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、切削工具や各種精密機械の耐摩耗性の向上
を目的として施工されるイオンプレーティングによる多
層膜の形成方法に関する。Description: TECHNICAL FIELD The present invention relates to a method for forming a multilayer film by ion plating for the purpose of improving the wear resistance of cutting tools and various precision machines.
［従来の技術及びその問題点］ 各種部材表面の耐摩耗性向上を目的としたセラミック
のイオンプレーティングは、切削工具に代表されるよう
に広く実用されており、更に高性能化（主に密着性）の
ために金属のアンダーコートを用いた多層膜のコーティ
ングが検討されている。その一つとして、従来、付着性
の優れたCrをアンダーコートとして多層膜を形成する方
法が知られている。しかしながら、Cr膜上にトップコー
トとしてTiN膜をイオンプレーティグすると、該TiN膜の
Cr膜に対する付着性及び耐摩耗性が不安定となる問題あ
った。[Prior art and its problems] Ion plating of ceramics for the purpose of improving the wear resistance of the surface of various members is widely used as represented by cutting tools, and further improved in performance (mainly adhesion The coating of a multi-layered film using a metal undercoat is being considered for this purpose. As one of them, conventionally, there is known a method of forming a multilayer film by using Cr, which has excellent adhesion, as an undercoat. However, when the TiN film is ion-plated as a top coat on the Cr film, the TiN film
There was a problem that the adhesion and wear resistance to the Cr film became unstable.
本発明は、上記従来の問題点を解決するためになされ
たもので、アンダーコートとしてCr膜及びトップコート
としてTiN膜を安定的にコーティングして密着性及び耐
摩耗性の優れた多層膜の形成方法を提供しようとするも
のである。The present invention has been made in order to solve the above-mentioned conventional problems, and stably forms a Cr film as an undercoat and a TiN film as a topcoat to form a multilayer film having excellent adhesion and wear resistance. It is intended to provide a method.
［問題点を解決するための手段］ 本発明は、基板上にアンダーコートとしてCr膜、トッ
プコートとしてTiN膜をイオンプレーティングによりコ
ーティングして多層膜を形成する方法において、前記基
板にバイアス電圧を印加せずにCr膜のコーティングを行
なった後、該基板にバイアス電圧を印加しつつTiN膜を
コーティングすることを特徴とする多層膜の形成方法で
ある。[Means for Solving Problems] The present invention provides a method of forming a multilayer film by coating a Cr film as an undercoat and a TiN film as a topcoat on a substrate by ion plating, and applying a bias voltage to the substrate. This is a method for forming a multilayer film, which comprises coating a Cr film without applying a voltage and then coating a TiN film while applying a bias voltage to the substrate.
［作用］ イオンプレーティングを、その装置の一形態を示す第
１図を参照して説明すると、真空容器１中を排気孔２よ
り真空排気し、ルツボ３内のコーティング材料４をプラ
ズマガン５から放出された電子線６によって加熱蒸発さ
せると共に、その蒸発原子を電子線６によってイオン化
し、このイオンをヒータ７で加熱された基板８の表面上
に堆積させる方法である。通常、基板８にはルツボ３対
して負の電圧が印加されており、これをバイアス電圧と
称している。なお、TiNのような化合物のコーティング
はTiを蒸発させると共に、導入口９より反応ガス（N2）
を供給してコーティングすることもある。[Operation] The ion plating will be described with reference to FIG. 1 showing one mode of the apparatus. The inside of the vacuum container 1 is evacuated through the exhaust hole 2, and the coating material 4 in the crucible 3 is removed from the plasma gun 5. This is a method of heating and evaporating by the emitted electron beam 6, ionizing the vaporized atoms by the electron beam 6, and depositing the ions on the surface of the substrate 8 heated by the heater 7. Usually, a negative voltage is applied to the crucible 3 on the substrate 8, and this is called a bias voltage. It should be noted that the coating of the compound such as TiN evaporates Ti and the reaction gas (N 2 ) is introduced from the inlet 9.
May be supplied for coating.
本発明者らは、上述したイオンプレーティングでCr膜
及びTiN膜をコーティングする際のTiN膜のCr膜に対する
付着性及び耐摩耗性の不安定化について検討したとこ
ろ、Crのコーティング条件によってその硬度やミクロ組
織等が大きく変化し、これがTiNの付着性不安定化等に
影響していることを究明した。The present inventors have studied the destabilization of the adhesion and abrasion resistance of the TiN film to the Cr film when coating the Cr film and the TiN film by the above-mentioned ion plating, and the hardness depending on the Cr coating conditions. It was clarified that the microstructure, microstructure, etc. changed significantly and that this affected the destabilization of the adhesion of TiN.
そこで、Crのイオンプレーティング時における上記硬
度やミクロ組織等の変化が起こる条件について更に検討
した結果、基板へのバイアス電圧の印加が最も大きな影
響要因であることを見出した。即ち、Crを基板上にイオ
ンプレーティングによりコーティングする際、基板にバ
イアス電圧を印加すると、Cr膜の硬度は低下し、結晶粒
が粗大化すると共に、その表面も凹凸が激しくなるのに
対し、バイアス電圧を印加しないと、Cr膜の高度は高
く、結晶粒も微細化し、表面も平滑になった。また、結
晶の配向性にも変化が見られ、バイアス電圧の印加の場
合には、ミラー指数表示で200）面が基板面に対して平
行に成長し易い（これを選択配向と称す）のに対し、バ
イアス電圧を印加しない場合には（110）面が選択配向
し易い。Therefore, as a result of further examination of the conditions under which the above-mentioned changes in hardness and microstructure occur during Cr ion plating, it was found that the application of a bias voltage to the substrate was the most influential factor. That is, when Cr is coated on the substrate by ion plating, if a bias voltage is applied to the substrate, the hardness of the Cr film is lowered, the crystal grains are coarsened, and the surface thereof is also roughened, whereas When the bias voltage was not applied, the Cr film had a high height, the crystal grains became fine, and the surface became smooth. Also, the crystal orientation changes, and when a bias voltage is applied, the (200) plane in the Miller index display tends to grow parallel to the substrate surface (this is called the selective orientation). On the other hand, when the bias voltage is not applied, the (110) plane is likely to be selectively oriented.
一方、TiNの場合にはバイアス電圧により（111）面が
選択配向し易くなる。また、バイアス電圧の印加はイオ
ンのエネルギーを増大させるため、基板のエッチング効
果を生じ、付着力が向上する。On the other hand, in the case of TiN, the bias voltage facilitates the selective orientation of the (111) plane. Further, the application of the bias voltage increases the energy of the ions, so that the etching effect of the substrate is produced and the adhesive force is improved.
以上のことより、基板にバイアス電圧を印加せずにCr
膜のコーティングを行なった後、該基板にバイアス電圧
を印加しつつTiN膜をコーティングすることによって、
次にのような良好な多層膜を形成できる。即ち、Crは結
晶面として最も密な（110）が選択配向し、更に結晶粒
も微細化し、硬度も高くなり、これにより耐摩耗性を向
上させるのに有効となる。また、TiNは同じく結晶面と
して最も密な（111）面が選択配向し、かつエッチング
効果により付着力も向上する。エッチング効果による付
着力の向上はCrにとって不利であるが、Crはもともと付
着性が良好な材料であるため、あまり影響されず、ミク
ロ組織の向上効果の方が大きいと思われる。From the above, Cr is applied without applying a bias voltage to the substrate.
After coating the film, by coating the TiN film while applying a bias voltage to the substrate,
The following good multilayer film can be formed. That is, Cr is the densest (110) as the crystal plane and is selectively oriented, and the crystal grains are further refined and the hardness is high, which is effective in improving the wear resistance. Similarly, TiN has the (111) plane, which is the densest as a crystal plane, selectively oriented, and the adhesion is improved by the etching effect. The improvement of the adhesive force due to the etching effect is disadvantageous to Cr, but since Cr is a material having a good adhesive property from the beginning, it is not so much affected and the effect of improving the microstructure seems to be greater.
本発明方法におけるバイアス電圧は、10V以上で効果
があり、それ以上高くてもよいが、あまり高くし過ぎる
と、エッチング効果が増大して成膜速度が低下する。こ
のため、工業的には上限を300V程度に設定することが望
ましい。The bias voltage in the method of the present invention is effective when it is 10 V or higher, and may be higher than that. However, if it is too high, the etching effect increases and the film formation rate decreases. Therefore, it is industrially desirable to set the upper limit to about 300V.
［発明の実施例］ 以下、本発明の実施例を詳細に説明する。[Examples of the Invention] Examples of the present invention will be described in detail below.
前述した第１図のイオンプレーティング装置の真空容
器１内に基板８として13Crステンレス鋼を配置し、下記
表に示す４つの条件で基板８上に暑さ８μｍのCr膜、更
に該Cr膜上に暑さ３μｍのTiN膜をコーティングして４
種の多層膜を夫々形成した。13Cr stainless steel is placed as the substrate 8 in the vacuum container 1 of the ion plating apparatus shown in FIG. 1, and a Cr film having a heat of 8 μm and further on the Cr film are placed on the substrate 8 under the four conditions shown in the table below. Coating with a TiN film with a heat of 3 μm
Seed multilayers were formed respectively.
しかして、サンプルNo.1〜No.4の多層膜を構成するCr
及びTiNについてＸ線回折法による結晶構造解析を行な
った結果、第２図に示すスペクトル特性図を得た。この
第２図より、本発明方法であるサンプルNo.2ではCrが
（110）面、TiNが（111）面に選択配向していることが
明らかになった。 Then, the Cr that constitutes the multilayer film of samples No. 1 to No. 4
As a result of crystal structure analysis of TiN and TiN by the X-ray diffraction method, the spectrum characteristic diagram shown in FIG. 2 was obtained. It is clear from FIG. 2 that in sample No. 2 which is the method of the present invention, Cr is selectively oriented on the (110) plane and TiN is oriented on the (111) plane.
また、サンプルNo.1〜No.4の多層膜についてスクラッ
チ試験を行なったところ、第３図に示す結果を得た。な
お、スクラッチ試験はダイヤモンド針に荷重を掛けて多
層膜表面を引掻き、荷重を増大していって多層膜が剥離
した時の荷重（臨界荷重）をAE信号により測定して評価
した。この場合、臨界荷重が大きい程、多層膜の付着力
が大きいことを意味する。この第３図から本発明方法で
あるサンプルNo.2が最も良好な付着性を有していること
が明らかとなった。When a scratch test was conducted on the multilayer films of Samples No. 1 to No. 4, the results shown in FIG. 3 were obtained. In the scratch test, a diamond needle was applied with a load to scratch the surface of the multilayer film, and the load (critical load) when the load was increased and the multilayer film was peeled off was evaluated by measuring the AE signal. In this case, the greater the critical load, the greater the adhesive force of the multilayer film. It is clear from FIG. 3 that sample No. 2 which is the method of the present invention has the best adhesion.
更に、サンプルNo.1〜No.4の多層膜について耐摩耗性
評価としてキャビテーションエロージョン試験（超音波
エロージョン試験、振動数:18.3kHz、振巾:25μｍ）を
行なったところ、第４図に示す結果を得た。この第４図
から本発明方法であるサンプルNo.2が最も良好な耐キャ
ビテーションエロージョン性を有していることが明らか
となった。Further, a cavitation erosion test (ultrasonic erosion test, frequency: 18.3 kHz, amplitude: 25 μm) was performed on the multilayer films of Samples No. 1 to No. 4 as an evaluation of wear resistance, and the results shown in FIG. 4 were obtained. Got It is clear from FIG. 4 that sample No. 2 which is the method of the present invention has the best cavitation erosion resistance.
［発明の効果］ 以上詳述した如く、本発明によればアンダーコートと
してCr膜及びトップコートとしてTiN膜を安定的にコー
ティングして密着性及び耐摩耗性の優れた多層膜を形成
でき、ひいては切削工具や各種精密機械の耐摩耗性付与
のための表面処理技術として有効に利用できる等顕著な
効果を有する。[Effects of the Invention] As described in detail above, according to the present invention, a Cr film as an undercoat and a TiN film as a topcoat can be stably coated to form a multilayer film having excellent adhesion and wear resistance. It has remarkable effects such as effective use as a surface treatment technology for imparting wear resistance to cutting tools and various precision machines.
第１図は本発明方法で用いたイオンプレーティング装置
の一形態を示す概略図、第２図は多層膜を構成するCr、
TiNのコーティング膜のＸ線分析結果を示すスペクトル
図、第３図はスクラッチ試験結果を示す線図、第４図は
キャビティーエロージョン試験結果を示す線図である。 １…真空容器、３…ルツボ、５…プラズマガン、６…電
子線、８…基板。FIG. 1 is a schematic view showing an embodiment of an ion plating apparatus used in the method of the present invention, and FIG. 2 is Cr constituting a multilayer film,
FIG. 4 is a spectrum diagram showing an X-ray analysis result of the TiN coating film, FIG. 3 is a diagram showing a scratch test result, and FIG. 4 is a diagram showing a cavity erosion test result. 1 ... Vacuum container, 3 ... Crucible, 5 ... Plasma gun, 6 ... Electron beam, 8 ... Substrate.
───────────────────────────────────────────────────── フロントページの続き (72)発明者 江原 隆一郎 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53−33777（ＪＰ，Ａ) 特開 昭54−139891（ＪＰ，Ａ) 特開 昭61−37960（ＪＰ，Ａ) ─────────────────────────────────────────────────── ─── Continuation of the front page (72) Inventor Ryuichiro Ehara 4-6-22 Kannon Shinmachi, Nishi-ku, Hiroshima City, Hiroshima Prefecture Mitsubishi Heavy Industries, Ltd. Hiroshima Research Laboratory (56) Reference JP-A-53-33777 (JP, A) JP-A-54-139891 (JP, A) JP-A-61-37960 (JP, A)
Claims (1)
プコートとしてTiN膜をイオンプレーティングによりコ
ーティングして多層膜を形成する方法において、前記基
板にバイアス電圧を印加せずにCr膜のコーティングを行
なった後、該基板にバイアス電圧を印加しつつTiN膜を
コーティングすることを特徴とする多層膜の形成方法。1. A method for forming a multilayer film by coating a Cr film as an undercoat and a TiN film as a topcoat on a substrate by ion plating to form a multilayer film without applying a bias voltage to the substrate. After that, a TiN film is coated on the substrate while applying a bias voltage to the substrate.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| JP5136887A JPH0830264B2 (en) | 1987-03-06 | 1987-03-06 | Method for forming multilayer film |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| JP5136887A JPH0830264B2 (en) | 1987-03-06 | 1987-03-06 | Method for forming multilayer film |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| JPS63219566A JPS63219566A (en) | 1988-09-13 |
| JPH0830264B2 true JPH0830264B2 (en) | 1996-03-27 |
Family
ID=12884997
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| JP5136887A Expired - Lifetime JPH0830264B2 (en) | 1987-03-06 | 1987-03-06 | Method for forming multilayer film |
Country Status (1)
| Country | Link |
|---|---|
| JP (1) | JPH0830264B2 (en) |
Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| WO2010016282A1 (en) | 2008-08-06 | 2010-02-11 | 三菱重工業株式会社 | Component for rotary machine |
-
1987
- 1987-03-06 JP JP5136887A patent/JPH0830264B2/en not_active Expired - Lifetime
Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| WO2010016282A1 (en) | 2008-08-06 | 2010-02-11 | 三菱重工業株式会社 | Component for rotary machine |
Also Published As
| Publication number | Publication date |
|---|---|
| JPS63219566A (en) | 1988-09-13 |
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Legal Events
| Date | Code | Title | Description |
|---|---|---|---|
| EXPY | Cancellation because of completion of term |