JPH01156496A - Formation of corrosion-resistant coating film on stainless steel member - Google Patents
Formation of corrosion-resistant coating film on stainless steel memberInfo
- Publication number
- JPH01156496A JPH01156496A JP31234487A JP31234487A JPH01156496A JP H01156496 A JPH01156496 A JP H01156496A JP 31234487 A JP31234487 A JP 31234487A JP 31234487 A JP31234487 A JP 31234487A JP H01156496 A JPH01156496 A JP H01156496A
- Authority
- JP
- Japan
- Prior art keywords
- stainless steel
- steel member
- film
- layer
- alumina
- 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.)
- Pending
Links
- 229910001220 stainless steel Inorganic materials 0.000 title claims abstract description 34
- 239000010935 stainless steel Substances 0.000 title claims abstract description 34
- 238000000576 coating method Methods 0.000 title claims abstract description 29
- 239000011248 coating agent Substances 0.000 title claims abstract description 28
- 238000005260 corrosion Methods 0.000 title claims abstract description 7
- 230000007797 corrosion Effects 0.000 title claims abstract description 7
- 230000015572 biosynthetic process Effects 0.000 title 1
- PNEYBMLMFCGWSK-UHFFFAOYSA-N aluminium oxide Inorganic materials [O-2].[O-2].[O-2].[Al+3].[Al+3] PNEYBMLMFCGWSK-UHFFFAOYSA-N 0.000 claims abstract description 29
- 239000010410 layer Substances 0.000 claims abstract description 26
- 230000002378 acidificating effect Effects 0.000 claims abstract description 10
- 239000002344 surface layer Substances 0.000 claims abstract description 8
- 238000007751 thermal spraying Methods 0.000 claims abstract description 6
- 229910052782 aluminium Inorganic materials 0.000 claims description 27
- XAGFODPZIPBFFR-UHFFFAOYSA-N aluminium Chemical compound [Al] XAGFODPZIPBFFR-UHFFFAOYSA-N 0.000 claims description 27
- 239000007864 aqueous solution Substances 0.000 claims description 9
- MUBZPKHOEPUJKR-UHFFFAOYSA-N Oxalic acid Chemical compound OC(=O)C(O)=O MUBZPKHOEPUJKR-UHFFFAOYSA-N 0.000 abstract description 9
- 238000005507 spraying Methods 0.000 abstract description 6
- 235000006408 oxalic acid Nutrition 0.000 abstract description 3
- 238000007743 anodising Methods 0.000 abstract description 2
- 230000035939 shock Effects 0.000 abstract description 2
- 238000005336 cracking Methods 0.000 abstract 2
- 238000007598 dipping method Methods 0.000 abstract 1
- 238000000034 method Methods 0.000 description 4
- 238000010586 diagram Methods 0.000 description 3
- OFOBLEOULBTSOW-UHFFFAOYSA-N Malonic acid Chemical compound OC(=O)CC(O)=O OFOBLEOULBTSOW-UHFFFAOYSA-N 0.000 description 2
- NBIIXXVUZAFLBC-UHFFFAOYSA-N Phosphoric acid Chemical compound OP(O)(O)=O NBIIXXVUZAFLBC-UHFFFAOYSA-N 0.000 description 2
- QAOWNCQODCNURD-UHFFFAOYSA-N Sulfuric acid Chemical compound OS(O)(=O)=O QAOWNCQODCNURD-UHFFFAOYSA-N 0.000 description 2
- 229910052736 halogen Inorganic materials 0.000 description 2
- 150000002367 halogens Chemical class 0.000 description 2
- 238000005268 plasma chemical vapour deposition Methods 0.000 description 2
- RYGMFSIKBFXOCR-UHFFFAOYSA-N Copper Chemical compound [Cu] RYGMFSIKBFXOCR-UHFFFAOYSA-N 0.000 description 1
- 229910000831 Steel Inorganic materials 0.000 description 1
- 229910000147 aluminium phosphate Inorganic materials 0.000 description 1
- KGBXLFKZBHKPEV-UHFFFAOYSA-N boric acid Chemical compound OB(O)O KGBXLFKZBHKPEV-UHFFFAOYSA-N 0.000 description 1
- 239000004327 boric acid Substances 0.000 description 1
- 238000005524 ceramic coating Methods 0.000 description 1
- KRVSOGSZCMJSLX-UHFFFAOYSA-L chromic acid Substances O[Cr](O)(=O)=O KRVSOGSZCMJSLX-UHFFFAOYSA-L 0.000 description 1
- 150000001875 compounds Chemical class 0.000 description 1
- 229910052802 copper Inorganic materials 0.000 description 1
- 239000010949 copper Substances 0.000 description 1
- 238000001035 drying Methods 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 230000005611 electricity Effects 0.000 description 1
- AWJWCTOOIBYHON-UHFFFAOYSA-N furo[3,4-b]pyrazine-5,7-dione Chemical compound C1=CN=C2C(=O)OC(=O)C2=N1 AWJWCTOOIBYHON-UHFFFAOYSA-N 0.000 description 1
- 229910052751 metal Inorganic materials 0.000 description 1
- 239000002184 metal Substances 0.000 description 1
- LNOPIUAQISRISI-UHFFFAOYSA-N n'-hydroxy-2-propan-2-ylsulfonylethanimidamide Chemical compound CC(C)S(=O)(=O)CC(N)=NO LNOPIUAQISRISI-UHFFFAOYSA-N 0.000 description 1
- 239000000843 powder Substances 0.000 description 1
- 238000006748 scratching Methods 0.000 description 1
- 230000002393 scratching effect Effects 0.000 description 1
- 239000010959 steel Substances 0.000 description 1
- 238000007738 vacuum evaporation Methods 0.000 description 1
- 238000005406 washing Methods 0.000 description 1
Landscapes
- Other Surface Treatments For Metallic Materials (AREA)
- Coating By Spraying Or Casting (AREA)
Abstract
Description
【発明の詳細な説明】
（産業上の利用分野）
本発明は腐蝕性ガスが使用される真空蒸着装置やプラズ
マＣＶＤ装置等に用いられるステンレス部材の耐蝕被覆
方法に関する。DETAILED DESCRIPTION OF THE INVENTION (Field of Industrial Application) The present invention relates to a method for corrosion-resistant coating of stainless steel members used in vacuum evaporation equipment, plasma CVD equipment, etc. in which corrosive gas is used.
（従来の技術）
従来、ステンレス部材はハロゲンやその化合物により腐
蝕され易いので、アルミナの粉末をプラズマ溶射し、第
１図示のようにステンレス部材ａの表面をアルミナ溶射
被膜すで覆うことが行なわれている。またアルミナの被
膜すを形成するに先立ち、第２図示のように、アルミニ
ウムの被膜Ｃを溶射により形成することも行なわれてい
る。(Prior Art) Conventionally, since stainless steel members are easily corroded by halogens and their compounds, alumina powder is plasma sprayed to cover the surface of stainless steel member a with an alumina spray coating as shown in Figure 1. ing. Furthermore, prior to forming the alumina coating, an aluminum coating C is formed by thermal spraying as shown in the second figure.
（発明が解決しようとする問題点）
前記第１図示のようにステンレス部材ａに直接アルミナ
の被膜すを形成したものは、金属にセラミックスの被膜
を形成することになるので、密着性が悪く、しかも両者
の熱膨張率の差があるので、アルミナ被膜すにクラック
が入り、ハロゲン等がクラックを介して侵入し、ステン
レス部材ａを腐蝕させる欠点がある。(Problems to be Solved by the Invention) In the case where the alumina coating is directly formed on the stainless steel member a as shown in the first drawing, since a ceramic coating is formed on the metal, the adhesion is poor. Furthermore, since there is a difference in the coefficient of thermal expansion between the two, cracks occur in the alumina coating, and halogen and the like enter through the cracks, causing corrosion of the stainless steel member a.
第２図示のものは、中間にアルミニウムの被膜Ｃが形成
されているので熱膨張率の差によるクラックの発生は少
ないが、溶射ではアルミニウムの被膜Ｃの厚さが最低１
００μ以上、その上のアルミナの被膜すが１００μ以上
となり、どうしても２００μ以上の厚さになるので、被
膜すが剥離し易く、またアルミニウムの溶射面とアルミ
ナの溶射面との結合が十分でないことも剥離の原因にな
っている。In the case shown in the second figure, since an aluminum coating C is formed in the middle, cracks are less likely to occur due to differences in thermal expansion coefficients, but in thermal spraying, the thickness of the aluminum coating C is at least 1.
00μ or more, the alumina coating on it is 100μ or more, and the thickness is inevitably 200μ or more, so the coating is likely to peel off, and the bond between the aluminum sprayed surface and the alumina sprayed surface may not be sufficient. It causes peeling.
本発明は、上記のような問題点を解決し、密着性が良く
しかもクラックの入らないアルミナ被膜をステンレス部
材に形成する方法を提案することを目的とするものであ
る。It is an object of the present invention to solve the above-mentioned problems and to propose a method for forming an alumina coating with good adhesion and no cracks on a stainless steel member.
（問題点を解決するための手段）
本発明では、前記問題点を解決するために、ステンレス
部材の表面にアルミニウムを溶射してアルミニウムの被
膜を形成したのち、該ステンレス部材を酸性水溶液中に
浸し、該アルミニウム被膜の表層を陽極酸化させアルミ
ナ層を形成するようにした。(Means for Solving the Problems) In order to solve the above-mentioned problems, in the present invention, aluminum is thermally sprayed onto the surface of a stainless steel member to form an aluminum film, and then the stainless steel member is immersed in an acidic aqueous solution. The surface layer of the aluminum coating was anodized to form an alumina layer.
（作 用）
ステンレス部材の表面に例えばアルミニウムワイヤを使
用したガス溶射によりアルミニウムの被膜を形成する。(Function) An aluminum coating is formed on the surface of a stainless steel member by gas spraying using, for example, an aluminum wire.
次にこれをシュウ酸等の酸性水溶液中に浸し、前記の溶
射で形成された被膜の表層例えば該被膜の厚さで１７５
〜４７５程度の表層を陽極酸化させる。Next, this is immersed in an acidic aqueous solution such as oxalic acid, and the surface of the coating formed by the above thermal spraying is, for example, 175 mm thick.
~475 surface layer is anodized.
これにより、第３図示のように、ステンレス部材（１）
を覆うアルミニウム被膜（２）の表層が陽極酸化によっ
てアルミナ層（３）となり、下層がアルミニウムのまま
残る。このアルミニウムの下層は、表層のアルミナ層（
３）と強固に密着すると共にステンレス部材（１）とも
強固に密着するので、アルミナ層（３）はステンレス部
材（１）に強く密着し、アルミナ層（３）とステンレス
部材（１）との熱膨張率の差は、中間のアルミニウムの
層により吸収され、アルミナ層■のクラックの発生を防
げる。As a result, as shown in the third diagram, the stainless steel member (1)
The surface layer of the aluminum film (2) covering the aluminum film becomes an alumina layer (3) by anodizing, and the lower layer remains aluminum. The lower layer of aluminum is the surface alumina layer (
3) and also firmly adheres to the stainless steel member (1), the alumina layer (3) strongly adheres to the stainless steel member (1) and the heat between the alumina layer (3) and the stainless steel member (1) is The difference in expansion coefficient is absorbed by the intermediate aluminum layer, preventing cracks from forming in the alumina layer.
（実施例）
本発明の実施例を図面第３図及び第４図に基づき乍ら説
明すると、符号（１）はステンレス部材、（２）は該ス
テンレス部材（１）の表面にアルミニウムワイヤを使用
してガス溶射により厚さ２００μに均一に形成したアル
ミニウム被膜を示す。該アルミニウム被膜（２）を形成
したステンレス部材（１）には、第４図示のように直流
電源（４）を介して陰極板（５）が接続され、電解槽（
６）内の５〜３０％に調整したシュウ酸の酸性水溶液（
７）中に浸漬される。そして直流電源（４）により該ス
テンレス部材（１）１１００ Ｖ 〜４００ Ｖ（ｒ）
電圧を８０分間カケ、アルミニウム被膜（２）の厚さの
約３／４即ち約１５０μまで陽極酸化させ、第３図示の
ようにアルミナ層（３）に変化させた。このあと該ステ
ンレス部材（１）を電解槽（６）から取出し、３〜５回
の洗浄にて付着した酸性水溶液（７）を除去し、１００
℃の熱風により乾燥してアルミナ層（３）で耐蝕被覆さ
れたステンレス部材を得た。(Example) An example of the present invention will be explained based on FIGS. 3 and 4. Reference numeral (1) is a stainless steel member, and (2) is an aluminum wire on the surface of the stainless steel member (1). The figure shows an aluminum coating uniformly formed to a thickness of 200 μm by gas spraying. As shown in the fourth diagram, a cathode plate (5) is connected to the stainless steel member (1) on which the aluminum coating (2) is formed via a DC power source (4), and an electrolytic cell (
6) Acidic aqueous solution of oxalic acid adjusted to 5 to 30% (
7) Immersed in. Then, the stainless steel member (1) is heated at 1100 V to 400 V (r) by the DC power source (4).
The voltage was applied for 80 minutes to anodize the aluminum film (2) to about 3/4 of the thickness, or about 150 μm, and transform it into an alumina layer (3) as shown in Figure 3. After that, the stainless steel member (1) was taken out from the electrolytic bath (6), and the attached acidic aqueous solution (7) was removed by washing 3 to 5 times.
A stainless steel member coated with a corrosion-resistant alumina layer (3) was obtained by drying with hot air at a temperature of .degree.
この実施例で得゛たステンレス部材のアルミナ層（３）
の表面に、太さ０．５ｍｍφ、先端角度が３０℃の先の
とがった針を当て、波計に１ｋｇの荷重を加え乍ら１ｃ
ＩＩＩ／ｓｅｃで動かし、ひっかき試験を行なったとこ
ろ、アルミナ層（３）の表面に傷がつかなかった。これ
に対しステンレス部材に２００μのアルミナ層を形成し
たものは、前記と同様のひっかき試験によりアルミナ層
の表面に傷がつき部分的に剥れた。Alumina layer (3) of stainless steel member obtained in this example
A pointed needle with a thickness of 0.5 mmφ and a tip angle of 30°C is applied to the surface of the wave meter, and a load of 1 kg is applied to the wave meter.
When a scratch test was performed by moving at a speed of 3/sec, the surface of the alumina layer (3) was not scratched. On the other hand, when a 200 μm thick alumina layer was formed on a stainless steel member, the surface of the alumina layer was scratched and partially peeled off in the same scratching test as above.
溶射により形成されたアルミニウムの被膜（２）は微小
孔を多数備えており、酸性水溶液中に於ては該微小孔内
に酸性水溶液が浸透し、その浸透領域が通電により陽極
酸化されてアルミナ層（３）になるものと考えられ、ア
ルミニウムの被膜（２）の全体がアルミナ層（３）にな
らないように通電時間が制御される。The aluminum coating (2) formed by thermal spraying has many micropores, and in an acidic aqueous solution, the acidic aqueous solution penetrates into the micropores, and the permeated area is anodized by electricity, forming an alumina layer. (3), and the current application time is controlled so that the entire aluminum coating (2) does not become the alumina layer (3).
酸性水溶液（７）として硫酸、クロム酸、マロン酸、ス
ルファミン酸、ホウ酸、リン酸等を使用してもよく、ス
テンレス部材（１）に代え鋼鉄、銅、アルミニウム等の
溶射被膜を形成し得る部材を使用できる。Sulfuric acid, chromic acid, malonic acid, sulfamic acid, boric acid, phosphoric acid, etc. may be used as the acidic aqueous solution (7), and a thermal spray coating of steel, copper, aluminum, etc. can be formed in place of the stainless steel member (1). parts can be used.
（発明の効果）
以上のように本発明に於ては、ステンレス部材の表面に
アルミニウムの溶射被膜を形成したのち該被膜の表層を
酸性水溶液中に於て陽極酸化させてアルミナ層とするよ
うにしたので、アルミナ層はその下層に残存するアルミ
ニウムの被膜を介してステンレス部材に強固に密着し、
溶射被膜を薄く形成することが出来るので該被膜の剥離
を防げ、中間にアルミニウムの層が介在するので熱ショ
ックやクラックの発生が少なくなり、ステンレス部材の
耐蝕性を向上させ得、プラズマＣＶＤ装置等の部材とし
て好都合である等の効果がある。(Effects of the Invention) As described above, in the present invention, after forming a sprayed aluminum coating on the surface of a stainless steel member, the surface layer of the coating is anodized in an acidic aqueous solution to form an alumina layer. As a result, the alumina layer firmly adheres to the stainless steel member through the aluminum coating remaining below it,
Since the thermal spray coating can be formed thinly, peeling of the coating can be prevented, and since there is an aluminum layer in the middle, thermal shock and cracks are less likely to occur, improving the corrosion resistance of stainless steel parts, and is useful for plasma CVD equipment, etc. It has advantages such as being convenient as a member.
第１図及び第２図は従来例の拡大断面図、第３図は本発
明の方法により製作させたステンレス部材の拡大断面図
、第４図は本発明の方法の実施に使用した装置の概略断
面図である。
（１）・・・ステンレス部材
（２）・・・アルミニウム被膜
（３）・・・アルミナ層
第１図
第２図
第３図Figures 1 and 2 are enlarged cross-sectional views of the conventional example, Figure 3 is an enlarged cross-sectional view of a stainless steel member manufactured by the method of the present invention, and Figure 4 is a schematic diagram of the apparatus used to carry out the method of the present invention. FIG. (1) Stainless steel member (2) Aluminum coating (3) Alumina layer Figure 1 Figure 2 Figure 3
Claims (1)
ニウム被膜を形成したのち、該ステンレス部材を酸性水
溶液中に浸し、該アルミニウム被膜の表層を陽極酸化さ
せアルミナ層を形成することを特徴とするステンレス部
材の耐蝕被覆方法。Corrosion resistance of a stainless steel member, characterized in that an aluminum coating is formed on the surface of the stainless steel member by thermal spraying, and then the stainless steel member is immersed in an acidic aqueous solution, and the surface layer of the aluminum coating is anodized to form an alumina layer. Coating method.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| JP31234487A JPH01156496A (en) | 1987-12-11 | 1987-12-11 | Formation of corrosion-resistant coating film on stainless steel member |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| JP31234487A JPH01156496A (en) | 1987-12-11 | 1987-12-11 | Formation of corrosion-resistant coating film on stainless steel member |
Publications (1)
| Publication Number | Publication Date |
|---|---|
| JPH01156496A true JPH01156496A (en) | 1989-06-20 |
Family
ID=18028113
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| JP31234487A Pending JPH01156496A (en) | 1987-12-11 | 1987-12-11 | Formation of corrosion-resistant coating film on stainless steel member |
Country Status (1)
| Country | Link |
|---|---|
| JP (1) | JPH01156496A (en) |
Cited By (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103374694A (en) * | 2012-04-24 | 2013-10-30 | 中国石油天然气股份有限公司 | Preparation method for anti-corrosion composite coating of oil pipe |
| CN103451662A (en) * | 2012-06-01 | 2013-12-18 | 广东欧珀移动通信有限公司 | Stainless steel surface treatment method |
| DE102014116335A1 (en) | 2014-11-10 | 2016-05-12 | Thyssenkrupp Ag | Composite material, composite product, process for its manufacture and uses therefor |
| JP2016514213A (en) * | 2013-03-14 | 2016-05-19 | アプライド マテリアルズ インコーポレイテッドＡｐｐｌｉｅｄ Ｍａｔｅｒｉａｌｓ，Ｉｎｃｏｒｐｏｒａｔｅｄ | High purity aluminum topcoat on substrate |
| CN107400888A (en) * | 2016-05-19 | 2017-11-28 | 南京理工大学 | A kind of stainless steel resistance to high temperature oxidation and seawater corrosion resistance Na2SiO3/Al2O3Preparation method of composite coating |
| US10260160B2 (en) | 2013-11-13 | 2019-04-16 | Applied Materials, Inc. | High purity metallic top coat for semiconductor manufacturing components |
Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JPS531648A (en) * | 1976-06-26 | 1978-01-09 | Yamazaki Keiichiro | Production process for metal products |
| JPS556105A (en) * | 1978-06-27 | 1980-01-17 | Toshiba Corp | Heat-exchange sound-insulation ventilating fan |
| JPS6187861A (en) * | 1984-10-08 | 1986-05-06 | Canon Inc | Surface treatment of structural material for vacuum apparatus |
-
1987
- 1987-12-11 JP JP31234487A patent/JPH01156496A/en active Pending
Patent Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JPS531648A (en) * | 1976-06-26 | 1978-01-09 | Yamazaki Keiichiro | Production process for metal products |
| JPS556105A (en) * | 1978-06-27 | 1980-01-17 | Toshiba Corp | Heat-exchange sound-insulation ventilating fan |
| JPS6187861A (en) * | 1984-10-08 | 1986-05-06 | Canon Inc | Surface treatment of structural material for vacuum apparatus |
Cited By (8)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103374694A (en) * | 2012-04-24 | 2013-10-30 | 中国石油天然气股份有限公司 | Preparation method for anti-corrosion composite coating of oil pipe |
| CN103451662A (en) * | 2012-06-01 | 2013-12-18 | 广东欧珀移动通信有限公司 | Stainless steel surface treatment method |
| JP2016514213A (en) * | 2013-03-14 | 2016-05-19 | アプライド マテリアルズ インコーポレイテッドＡｐｐｌｉｅｄ Ｍａｔｅｒｉａｌｓ，Ｉｎｃｏｒｐｏｒａｔｅｄ | High purity aluminum topcoat on substrate |
| US10260160B2 (en) | 2013-11-13 | 2019-04-16 | Applied Materials, Inc. | High purity metallic top coat for semiconductor manufacturing components |
| DE102014116335A1 (en) | 2014-11-10 | 2016-05-12 | Thyssenkrupp Ag | Composite material, composite product, process for its manufacture and uses therefor |
| WO2016074915A1 (en) | 2014-11-10 | 2016-05-19 | Thyssenkrupp Ag | Composite material, composite material product, methods for producing said composite material and composite material product, and uses therefor |
| CN107400888A (en) * | 2016-05-19 | 2017-11-28 | 南京理工大学 | A kind of stainless steel resistance to high temperature oxidation and seawater corrosion resistance Na2SiO3/Al2O3Preparation method of composite coating |
| CN107400888B (en) * | 2016-05-19 | 2019-08-30 | 南京理工大学 | A kind of stainless steel resistance to high temperature oxidation and seawater corrosion resistance Na2SiO3/Al2O3Preparation method of composite coating |
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