JP3417986B2 - Method for producing coated object with excellent adhesion - Google Patents
Method for producing coated object with excellent adhesionInfo
- Publication number
- JP3417986B2 JP3417986B2 JP27618293A JP27618293A JP3417986B2 JP 3417986 B2 JP3417986 B2 JP 3417986B2 JP 27618293 A JP27618293 A JP 27618293A JP 27618293 A JP27618293 A JP 27618293A JP 3417986 B2 JP3417986 B2 JP 3417986B2
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- Prior art keywords
- gas
- base material
- coating
- pretreatment
- nitride
- Prior art date
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Description
【０００１】[0001]
【産業上の利用分野】本発明は、窒化ケイ素系セラミッ
クス焼結体の基材の表面に、化学蒸着法（ＣＶＤ法）に
より被膜を被覆するための被覆物体の製造方法に関し、
具体的には、反応容器内で基材の表面にガスによる前処
理を施した後、被膜を被覆して切削工具および耐摩耗工
具等の工具として最適にするための付着性に優れた被覆
物体の製造方法に関する。BACKGROUND OF THE INVENTION 1. Field of the Invention The present invention relates to a method for producing a coated object for coating a surface of a base material of a silicon nitride ceramics sintered body with a chemical vapor deposition method (CVD method). ,
Specifically, after the surface of the base material is pretreated with gas in the reaction vessel, a coated object with excellent adhesion to cover the coating and optimize it as a tool such as a cutting tool and wear resistant tool. Manufacturing method.
【０００２】[0002]
【従来の技術】一般に、気相−気相反応により基材の表
面に被膜を被覆させる方法として知られている熱ＣＶＤ
法，プラズマＣＶＤ法またはレーザＣＶＤ法は、反応形
態により固相拡散反応，熱分解反応，水素還元反
応，複合反応，水素還元複合反応，置換反応等が
ある。2. Description of the Related Art Generally, thermal CVD is known as a method for coating a film on a surface of a substrate by a gas phase-gas phase reaction.
The method, plasma CVD method or laser CVD method includes solid phase diffusion reaction, thermal decomposition reaction, hydrogen reduction reaction, complex reaction, hydrogen reduction complex reaction, substitution reaction and the like depending on the reaction mode.
【０００３】これらの反応形態により行われる被覆工程
は、水や有機溶剤等で表面を洗浄した基材を反応容器内
に配置し、反応容器内を真空，水素ガスまたは不活性ガ
スの雰囲気とした後、昇温する第１工程と、被膜の構成
成分となる元素を含んだ気相またはその気相を励起させ
る励起ガスの添加や励起機構を備けて、加熱保持し、基
材の表面に被膜を被覆する第２工程と、反応容器内を冷
却する第３工程に大別できる。In the coating process performed by these reaction modes, a substrate whose surface has been washed with water, an organic solvent or the like is placed in a reaction vessel, and the inside of the reaction vessel is evacuated or filled with hydrogen gas or an inert gas atmosphere. After that, a first step of raising the temperature and a gas phase containing an element to be a constituent of the coating or an excitation gas addition for exciting the gas phase and an excitation mechanism are provided, and the material is heated and held, and the surface of the substrate is heated. It can be roughly divided into a second step of coating a film and a third step of cooling the inside of the reaction vessel.
【０００４】これらの工程を経て作製される被覆物体
は、被膜と基材との付着性が悪いこと、異質被膜間の付
着性が悪いことおよび付着強度のバラツキが大きいとい
う問題がある。The coated article produced through these steps has the problems of poor adhesion between the coating and the substrate, poor adhesion between different coatings, and large variations in adhesion strength.
【０００５】この問題を解決するための検討が多数行わ
れており、その１つの方法として、反応容器内に基材を
配置する前に、水や有機溶剤による基材表面の洗浄の他
に、超音波による基材表面の洗浄または酸やアルカリ溶
剤による基材表面のエッチング処理等があり、異質被膜
間の付着性の問題を解決しようとした代表的なものに、
特開昭５９−２１９４７７号公報がある。Many investigations have been made to solve this problem. One of the methods is to clean the surface of the substrate with water or an organic solvent before placing the substrate in the reaction vessel. Typical ones that have attempted to solve the problem of adhesion between different coatings, such as cleaning the substrate surface with ultrasonic waves or etching the substrate surface with an acid or alkaline solvent.
There is JP-A-59-219477.
【０００６】[0006]
【発明が解決しようとする課題】被覆物体における被膜
の接合または結合するための方法として提案されている
特開昭５９−２１９４７７号公報には、超硬合金に代表
される硬質金属製の切削植刃の基材表面を耐火金属の炭
化物，窒化物または炭窒化物の薄層で被覆し、該薄層を
酸化雰囲気に暴露して耐火金属の一酸化物より硬度の酸
化物を生成させ、該高度酸化物層をＴｉＣｌ4，ＨｆＣ
ｌ4，ＺｒＣｌ4の１種の化合物とＨ2との混合ガスで還
元してその表面に一酸化物を生成させ、次いで一酸化物
表面上に硬質の耐摩耗性酸化アルミニウムを被覆させる
ことを特徴とする硬質金属製切削工具植刃の製造方法に
ついて記載されている。SUMMARY OF THE INVENTION Japanese Patent Laid-Open No. 219477/1984 proposes a method for joining or joining coatings on a coated object, and a cutting plant made of hard metal represented by cemented carbide. Coating the substrate surface of the blade with a thin layer of a refractory metal carbide, nitride or carbonitride, and exposing the thin layer to an oxidizing atmosphere to form an oxide having a hardness higher than that of the refractory metal monoxide; Advanced oxide layer is TiCl 4 , HfC
l 4 , ZrCl 4 One compound of H 2 and a mixture gas of H 2 are reduced to form a monoxide on the surface, and then a hard wear-resistant aluminum oxide is coated on the surface of the monoxide. A method for manufacturing a characteristic hard metal cutting tool planting blade is described.
【０００７】同公報に記載されている製造方法は、耐火
金属の炭化物，窒化物または炭窒化物の薄層と酸化アル
ミニウムの硬質層との接合または結合を強固にするとい
う方法であるが、基材と薄層との付着性については改善
されてなく、特にセラミックス焼結体の基材の場合に
は、基材と薄層間における剥離でもって短寿命になると
いう問題がある。The manufacturing method described in the publication is a method of strengthening the bonding or bonding between a thin layer of a refractory metal carbide, nitride or carbonitride and a hard layer of aluminum oxide. The adhesion between the material and the thin layer has not been improved, and particularly in the case of the base material of the ceramics sintered body, there is a problem that the peeling between the base material and the thin layer shortens the service life.
【０００８】本発明は、上述のような問題点を解決した
もので、具体的には、ＣＶＤ法により基材の表面に被膜
を被覆する前に、フッ素ガスおよび／またはフッ素元素
を含むフッ素化合物ガスの存在する雰囲気中で基材を加
熱する前処理工程を施して、被膜と基材との付着強度、
耐剥離性を高めると共に、バラツキの小さい、信頼性の
高い被覆物体を得るための製造方法の提供を目的とす
る。The present invention has solved the above-mentioned problems. Specifically, the fluorine compound containing a fluorine gas and / or a fluorine element is formed before the surface of the substrate is coated with the film by the CVD method. By performing a pretreatment step of heating the base material in an atmosphere in which gas is present, the adhesion strength between the coating and the base material,
An object of the present invention is to provide a manufacturing method for enhancing the peeling resistance and obtaining a highly reliable coated object with less variation.
【０００９】[0009]
【課題を解決するための手段】本発明者らは、被覆物体
を切削工具として用いた場合、特に窒化ケイ素系セラミ
ックス焼結体の基材の表面に硬質被膜を被覆した被覆物
体における基材と被膜との付着強度を高めることについ
て検討していたところ、基材の表面に被膜を被覆する場
合、基材と被膜との付着性は、それぞれの材質の整合
性，被膜厚さ，基材の表面状態および被覆条件により大
きく影響を受けるが、被膜を被覆する前の基材表面状態
を調整すること、特に被膜を被覆するための反応容器内
に基材を設置してから被膜を被覆する直前における基材
表面状態により大きく影響を受けること、このとき基材
表面をフッ素ガスやフッ素元素を含むフッ素化合物ガス
の存在する雰囲気中で加熱するとより大きな効果がある
という知見を得て本発明を完成するに至ったものであ
る。The present inventors have found that when a coated object is used as a cutting tool, the surface of a substrate of a silicon nitride ceramics sintered body is coated with a hard coating. As a result of studying how to increase the adhesion strength between the base material and the coating on the object, when the surface of the base material is coated, the adhesion between the base material and the coating depends on the consistency of the respective materials and the film thickness. However, it is greatly affected by the surface condition of the base material and the coating conditions, but it is necessary to adjust the surface condition of the base material before coating the film, especially after installing the base material in the reaction vessel for coating the film. greatly influenced by the substrate surface condition immediately before coating the coating, obtained a finding that this time there is a greater effect when heated in an atmosphere in the presence of fluorine compound gas containing fluorine gas and fluorine element and the substrate surface Which has led to the completion of the present invention.
【００１０】すなわち、本発明の被覆物体の製造方法
は、窒化ケイ素系セラミックス焼結体の基材の表面にＣ
ＶＤ法により被膜を被覆する方法において、フッ素ガス
および／またはフッ素元素を含むフッ素化合物ガスでな
る前処理ガス中、もしくは該前処理ガスと希釈ガスとの
混合ガス（但し、基材の表面に被膜が形成されるような
処理ガスと希釈ガスとの組合わせは除く）中で該基材を
加熱する前処理工程を施した後、該基材の表面に該被膜
を被覆することを特徴とする方法である。That is, according to the method for producing a coated object of the present invention, C is formed on the surface of the base material of the silicon nitride ceramics sintered body.
In the method of coating a film by the VD method, in a pretreatment gas consisting of fluorine gas and / or a fluorine compound gas containing a fluorine element, or a mixed gas of the pretreatment gas and a diluting gas (however, the surface of the substrate is coated (Excluding a combination of a processing gas and a diluent gas so as to form) is subjected to a pretreatment step of heating the base material, and then the surface of the base material is coated with the coating film. Is the way.
【００１１】本発明の被覆物体の製造方法における基材
は、具体的には、窒化ケイ素系セラミックス焼結体を挙
げることができる。Specific examples of the base material in the method for producing a coated article of the present invention include silicon nitride ceramics sintered bodies.
【００１２】これらの基材の表面は、従来から行われて
いる水，有機溶剤，酸溶液，アルカリ溶液等で洗浄（超
音波洗浄も含む）処理を施すことは好ましいことであ
る。次いで、従来から実用されている各種のＣＶＤ法の
処理ができる装置の反応容器内に基材を設置し、基材の
表面に被膜を被覆する前に、フッ素ガスおよび／または
フッ素元素を含むフッ素化合物ガスでなる前処理ガス
中、もしくは該前処理ガスと希釈ガスとの混合ガス（但
し、基材の表面に被膜が形成されるような処理ガスと希
釈ガスとの組合わせは除く）中で基材を加熱する前処理
工程を施すことが本発明の製造方法の大きな特徴であ
る。It is preferable that the surface of these base materials is subjected to conventional cleaning treatment (including ultrasonic cleaning) with water, an organic solvent, an acid solution, an alkaline solution or the like. Next, the base material is placed in a reaction vessel of an apparatus capable of performing various types of conventional CVD methods, and fluorine gas and / or
In a pretreatment gas consisting of a fluorine compound gas containing elemental fluorine , or a mixed gas of the pretreatment gas and a diluent gas (however, a combination of the treatment gas and the diluent gas such that a film is formed on the surface of the base material) It is a major feature of the manufacturing method of the present invention that a pretreatment step of heating the base material is performed.
【００１３】本発明の被覆物体の製造方法における前処
理ガスは、具体的には、例えばフッ素ガス、ＣＦ4，Ｃ2
Ｆ6，Ｃ3Ｆ8，ＣＣｌ2Ｆ2，ＣＢｒＦ3，ＨＦ，ＣＨ
Ｆ3，ＷＦ6，ＭｏＦ6，ＳｉＦ4のフッ化炭素ガス，フッ
化水素ガス，フッ化炭化水素ガス，フッ化ケイ素ガス，
金属フッ化ガスを挙げることができる。The pretreatment gas in the method for producing a coated article according to the present invention is, for example, fluorine gas, CF 4 , C 2
F 6 , C 3 F 8 , CCl 2 F 2 , CBrF 3 , HF, CH
F 3, WF 6, MoF 6 , SiF 4 fluorocarbon gas, fluoride <br/> hydrogen gas, fluorocarbon gas, silicon fluoride gas,
Metal fluoride gas may be mentioned.
【００１４】これらの前処理ガスの中の少なくとも１種
のガス雰囲気中または前処理ガスと例えば水素，酸素，
一酸化炭素，不活性ガスの中の少なくとも１種の希釈ガ
スとの混合ガス中で基材を約４００℃以上に加熱すると
いう前処理工程を施して、基材表面を改造した後、基材
表面に被膜を被覆する方法である。In a gas atmosphere of at least one of these pretreatment gases or with the pretreatment gas such as hydrogen, oxygen,
After modifying the surface of the base material by subjecting the base material surface to a pretreatment step of heating the base material to about 400 ° C. or higher in a mixed gas of carbon monoxide and at least one diluent gas among inert gases, the base material This is a method of coating a film on the surface.
【００１５】この前処理工程の前後に別の工程を付加す
ることも好ましいことであり、特に、反応容器内に基材
を設置し、次いで反応容器内を真空雰囲気中または非酸
化性ガス雰囲気中にして基材を昇温し、次いで前処理工
程を施した後、基材表面に被膜を被覆することは、基材
と被膜の付着強度から好ましいことである。また、以上
のような工程の後に、さらに物理蒸着法（ＰＶＤ法）で
もって被膜を被覆し、多層膜とすることも好ましいこと
である。It is also preferable to add another step before and after this pretreatment step. In particular, a base material is placed in a reaction vessel, and then the reaction vessel is subjected to a vacuum atmosphere or a non-oxidizing gas atmosphere. It is preferable from the standpoint of adhesion strength between the base material and the coating film to raise the temperature of the base material and then perform the pretreatment step and then coat the surface of the base material with the coating film. It is also preferable that after the above steps, the coating film is further coated by a physical vapor deposition method (PVD method) to form a multilayer film.
【００１６】本発明の被覆物体の製造方法における被膜
は、周期律表の４ａ，５ａ，６ａ族の炭化物，窒化物，
炭酸化物，窒酸化物，硫化物，ホウ化物，Ａｌの酸化
物，窒化物，Ｓｉの炭化物，窒化物およびこれらの相互
固溶体の中の少なくとも１種の単層あるいは多層を挙げ
ることができる。The coating used in the method for producing a coated article according to the present invention comprises a carbide, a nitride, or a group 4a, 5a or 6a of the periodic table.
Mention may be made of at least one monolayer or multilayer of carbon oxides, nitrogen oxides, sulfides, borides, Al oxides, nitrides, Si carbides, nitrides and mutual solid solutions thereof.
【００１７】[0017]
【作用】本発明の被覆物体の製造方法は、前処理ガス、
または前処理ガスと希釈ガスとの混合ガスが基材表面の
付着または酸化した酸化物や不純物を除去し、面粗さを
大きくし、大きな面粗さの中に被膜がクサビ状に付着さ
れることにより、基材と被膜との付着強度を高める作用
をしていること、または基材表面の実質的表面積を広く
し、広い表面積に被膜が付着されることにより、基材と
被膜との付着強度を高める作用となっていること、さら
には、基材表面が研摩されている場合には、研摩により
生じた基材表面の微小クラックを減少または消滅させる
作用をし、その結果微小クラックから発生する被膜の剥
離を抑制するという間接的作用をしているものである。The method for producing a coated object according to the present invention comprises a pretreatment gas,
Alternatively, the mixed gas of the pretreatment gas and the diluent gas removes the oxides or impurities that have adhered or oxidized on the surface of the base material to increase the surface roughness, and the film is attached like wedges in the large surface roughness. This has the effect of increasing the adhesive strength between the base material and the coating film, or widens the substantial surface area of the base material surface and allows the coating material to adhere to a large surface area, thereby adhering the base material to the coating film. It has the effect of increasing the strength, and further, when the base material surface is polished, it acts to reduce or eliminate microcracks on the base material surface caused by polishing, resulting in the generation of microcracks. It has an indirect effect of suppressing peeling of the coating film.
【００１８】[0018]
【実施例１】９２％Ｓｉ3Ｎ4−５％Ｙ2Ｏ3−３％Ａｌ2
Ｏ3（重量％）組成の市販窒化ケイ素系焼結体をＪＩＳ
規格による形状ＳＮＭＮ１２０４１２に成形し、その表
面を鏡面研摩し、ＪＩＳ規格Ｂ０６０１による表面粗さ
Ｒａ＝０．００５μｍ以下にした基材を準備した。この
基材の表面を洗浄および乾燥した後、化学蒸着装置の反
応容器内に装着し、表１の昇温工程の条件でもって１１
００℃まで昇温し、次いで表１に示した前処理工程、第
１被膜工程、第２被膜工程、第３被膜工程および冷却工
程を順次行って、本発明の方法による被覆物体を得た。
このとき、工程から次の工程に移る際には、必ずガスの
供給を止め、反応容器内に残ったガスは、エジェクター
ポンプにより５Ｔｏｒｒ以上の真空にして行った。Example 1 92% Si 3 N 4 -5% Y 2 O 3 -3% Al 2
A commercially available silicon nitride-based sintered body having an O 3 (wt%) composition is JIS
A base material having a standard shape SNMN120412 and having its surface mirror-polished to have a surface roughness Ra of 0.005 μm or less according to JIS standard B0601 was prepared. After cleaning and drying the surface of the base material, the base material was mounted in a reaction vessel of a chemical vapor deposition apparatus, and the temperature of the heating step in Table 1
The temperature was raised to 00 ° C., and then the pretreatment step, the first coating step, the second coating step, the third coating step and the cooling step shown in Table 1 were sequentially performed to obtain a coated object by the method of the present invention.
At this time, when moving from one step to the next step, the supply of gas was always stopped, and the gas remaining in the reaction vessel was evacuated to 5 Torr or more by an ejector pump.
【００１９】比較として、表１に示した前処理工程のみ
行わず、その他をすべて上述と同様の工程で行って、比
較の方法による被覆物体を得た。For comparison, only the pretreatment steps shown in Table 1 were not carried out, and the other steps were all carried out in the same steps as described above to obtain coated objects by the method of comparison.
【００２０】こうして得た本発明の方法による被覆物体
と比較の方法による被覆物体の被膜の付着強度を評価す
るために、ロックウエルダイヤモンド圧子を用いたスク
ラッチ試験を行った結果、本発明の方法による被覆物体
は、１０Ｋｇｆの荷重においても被膜の剥離が生じない
のに対し、比較の方法による被覆物体は、１Ｋｇｆの荷
重で被膜の剥離が生じた。In order to evaluate the adhesion strength of the coating of the coated article obtained by the method of the present invention and the coated article obtained by the comparative method, a scratch test using a Rockwell diamond indenter was carried out. As a result, the coating produced by the method of the present invention was used. The object did not peel off the coating even under a load of 10 Kgf, whereas the coated article according to the comparative method caused peeling of the film under a load of 1 Kgf.
【００２１】上述の本発明の方法および比較の方法の
内、基材の表面のみ、＃４００砥石で研削した面とし、
その他をそれぞれ同様に行って得た被覆物体を用いて、
被削材：ＦＣ３５０（ＨＢ２０８），切削時間：２０
分，切削速度：２００ｍ／ｍｉｎ，送り：０．３ｍｍ／
ｒｅｖ，切込み：１．５ｍｍ，乾式による切削試験を行
った結果、本発明の方法による被覆物体は、平均逃げ面
摩耗量（ＶＢ）＝０．１９で被膜の剥離が生じていなか
ったのに対し、比較の方法による被覆物体は、平均逃げ
面摩耗量（ＶＢ）＝０．５２で被膜の剥離が生じた。Among the above-described method of the present invention and the comparative method, only the surface of the substrate is a surface ground with a # 400 grindstone,
Using coated objects obtained by performing the other respectively in the same manner,
Work Material: FC350 (HB208), Cutting Time: 20
Min, cutting speed: 200 m / min, feed: 0.3 mm /
rev, depth of cut: 1.5 mm, as a result of a cutting test by a dry method, it was found that the coated article produced by the method of the present invention had an average flank wear amount (V B ) = 0.19 and no peeling of the coating. On the other hand, in the case of the coated article prepared by the comparative method, the peeling of the coating occurred at the average flank wear amount (V B ) = 0.52.
【００２２】[0022]
【表１】 [Table 1]
【００２３】[0023]
【発明の効果】本発明の被覆物体の製造方法は、従来の
ＣＶＤ法による被覆物体の製造方法に比べて、基材と被
膜との付着強度が約５〜１０倍も優れているという顕著
な効果がある。EFFECTS OF THE INVENTION The method for producing a coated article according to the present invention is remarkably superior in adhesion strength between the substrate and the coating by about 5 to 10 times as compared with the conventional method for producing a coated article by the CVD method. effective.
───────────────────────────────────────────────────── フロントページの続き (56)参考文献 特開 平４−104982（ＪＰ，Ａ) 特開 平４−104983（ＪＰ，Ａ) 特開 平４−136174（ＪＰ，Ａ) 特開 平５−132777（ＪＰ，Ａ) 特開 昭51−146177（ＪＰ，Ａ) 特開 昭62−67174（ＪＰ，Ａ) 特開 昭63−40786（ＪＰ，Ａ) (58)調査した分野(Int.Cl.7，ＤＢ名) C23C 16/00 - 16/56 C04B 35/56 - 35/58 ─────────────────────────────────────────────────── ─── Continuation of the front page (56) Reference JP-A-4-104982 (JP, A) JP-A-4-104983 (JP, A) JP-A-4-136174 (JP, A) JP-A-5- 132777 (JP, A) JP-A-51-146177 (JP, A) JP-A-62-67174 (JP, A) JP-A-63-40786 (JP, A) (58) Fields investigated (Int.Cl. 7 , DB name) C23C 16/00-16/56 C04B 35/56-35/58
Claims (2)
の表面に化学蒸着法により周期律表の４ａ，５ａ，６ａ
族の炭化物，窒化物，炭窒化物，窒酸化物，硫化物，ホ
ウ化物，Ａｌの酸化物，窒化物，Ｓｉの炭化物，窒化物
およびこれらの相互固溶体のなかの少なくとも１種の単
層あるいは多層からなる被膜を被覆する方法において、
フッ素ガスおよび／またはフッ素元素を含むフッ素化合
物ガスでなる前処理ガス中、もしくは該前処理ガスと希
釈ガスとの混合ガス（但し、基材の表面に被膜が形成さ
れるような処理ガスと希釈ガスとの組合わせは除く）中
で該基材を加熱する前処理工程を施した後、該基材の表
面に該被膜を被覆することを特徴とする付着性に優れた
被覆物体の製造方法。1. A periodic table of 4a, 5a, 6a formed on a surface of a base material of a silicon nitride ceramics sintered body by a chemical vapor deposition method.
Group Carbides, Nitride, Carbonitride, Nitroxide, Sulfide, Ho
Uride, Al oxide, nitride, Si carbide, nitride
And at least one of these mutual solid solutions.
Oite the method for coating a coating comprising a layer or multi-layer,
Fluorine gas and / or pre-treatment gas comprising a fluorine compound <br/> compound gas containing fluorine element, or pretreatment gas and mixed gas of diluent gas (however, as the film is formed on the surface of the substrate (Excluding a combination of a processing gas and a diluting gas) is subjected to a pretreatment step of heating the base material, and then the surface of the base material is coated with the film, which is excellent in adhesion. A method of manufacturing a coated object.
の表面に化学蒸着法により周期律表の４ａ，５ａ，６ａ
族の炭化物，窒化物，炭窒化物，窒酸化物，硫化物，ホ
ウ化物，Ａｌの酸化物，窒化物，Ｓｉの炭化物，窒化物
およびこれらの相互固溶体のなかの少なくとも１種の単
層あるいは多層からなる被膜を被覆する方法において、
真空もしくは非酸化性ガスの雰囲気中で該基材を昇温す
る工程と、フッ素ガスおよび／またはフッ素元素を含む
フッ素化合物ガスでなる前処理ガス中、あるいは該前処
理ガスと希釈ガスとの混合ガス（但し、基材の表面に被
膜が形成されるような処理ガスと希釈ガスとの組合わせ
は除く）中で該基材を加熱する前処理工程とを施した
後、該基材の表面に該被膜を被覆することを特徴とする
付着性に優れた被覆物体の製造方法。2. A periodic table of 4a, 5a, 6a formed on a surface of a base material of a silicon nitride ceramics sintered body by a chemical vapor deposition method.
Group Carbides, Nitride, Carbonitride, Nitroxide, Sulfide, Ho
Uride, Al oxide, nitride, Si carbide, nitride
And at least one of these mutual solid solutions.
Oite the method for coating a coating comprising a layer or multi-layer,
And a step of a base material to heating in an atmosphere of vacuum or non-oxidizing gas, fluorine gas and / or fluorine element
In a pretreatment gas consisting of a fluorine compound gas, or a mixed gas of the pretreatment gas and a diluting gas (excluding the combination of the treatment gas and the diluting gas such that a film is formed on the surface of the base material) And a pretreatment step of heating the base material, and then coating the coating on the surface of the base material.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| JP27618293A JP3417986B2 (en) | 1993-10-07 | 1993-10-07 | Method for producing coated object with excellent adhesion |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| JP27618293A JP3417986B2 (en) | 1993-10-07 | 1993-10-07 | Method for producing coated object with excellent adhesion |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| JPH07109572A JPH07109572A (en) | 1995-04-25 |
| JP3417986B2 true JP3417986B2 (en) | 2003-06-16 |
Family
ID=17565862
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| JP27618293A Expired - Fee Related JP3417986B2 (en) | 1993-10-07 | 1993-10-07 | Method for producing coated object with excellent adhesion |
Country Status (1)
| Country | Link |
|---|---|
| JP (1) | JP3417986B2 (en) |
Families Citing this family (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1186213C (en) * | 1999-06-16 | 2005-01-26 | Tdy工业公司 | Substrate treatment method |
-
1993
- 1993-10-07 JP JP27618293A patent/JP3417986B2/en not_active Expired - Fee Related
Also Published As
| Publication number | Publication date |
|---|---|
| JPH07109572A (en) | 1995-04-25 |
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