JPH0158266B2 - - Google Patents
Info
- Publication number
- JPH0158266B2 JPH0158266B2 JP55172499A JP17249980A JPH0158266B2 JP H0158266 B2 JPH0158266 B2 JP H0158266B2 JP 55172499 A JP55172499 A JP 55172499A JP 17249980 A JP17249980 A JP 17249980A JP H0158266 B2 JPH0158266 B2 JP H0158266B2
- Authority
- JP
- Japan
- Prior art keywords
- acid
- molded product
- polyacetal
- sputtering
- weight
- 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
Links
Classifications
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08J—WORKING-UP; GENERAL PROCESSES OF COMPOUNDING; AFTER-TREATMENT NOT COVERED BY SUBCLASSES C08B, C08C, C08F, C08G or C08H
- C08J7/00—Chemical treatment or coating of shaped articles made of macromolecular substances
- C08J7/12—Chemical modification
- C08J7/14—Chemical modification with acids, their salts or anhydrides
-
- C—CHEMISTRY; METALLURGY
- C23—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; CHEMICAL SURFACE TREATMENT; DIFFUSION TREATMENT OF METALLIC MATERIAL; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL; INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL
- C23C—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; SURFACE TREATMENT OF METALLIC MATERIAL BY DIFFUSION INTO THE SURFACE, BY CHEMICAL CONVERSION OR SUBSTITUTION; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL
- C23C14/00—Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material
- C23C14/22—Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material characterised by the process of coating
- C23C14/34—Sputtering
-
- C—CHEMISTRY; METALLURGY
- C23—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; CHEMICAL SURFACE TREATMENT; DIFFUSION TREATMENT OF METALLIC MATERIAL; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL; INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL
- C23C—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; SURFACE TREATMENT OF METALLIC MATERIAL BY DIFFUSION INTO THE SURFACE, BY CHEMICAL CONVERSION OR SUBSTITUTION; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL
- C23C14/00—Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material
- C23C14/02—Pretreatment of the material to be coated
- C23C14/021—Cleaning or etching treatments
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08J—WORKING-UP; GENERAL PROCESSES OF COMPOUNDING; AFTER-TREATMENT NOT COVERED BY SUBCLASSES C08B, C08C, C08F, C08G or C08H
- C08J2359/00—Characterised by the use of polyacetals containing polyoxymethylene sequences only
- C08J2359/02—Copolyoxymethylenes
Landscapes
- Chemical & Material Sciences (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Organic Chemistry (AREA)
- Materials Engineering (AREA)
- Mechanical Engineering (AREA)
- Metallurgy (AREA)
- Engineering & Computer Science (AREA)
- General Chemical & Material Sciences (AREA)
- Health & Medical Sciences (AREA)
- Medicinal Chemistry (AREA)
- Polymers & Plastics (AREA)
- Treatments Of Macromolecular Shaped Articles (AREA)
- Physical Vapour Deposition (AREA)
- Chemically Coating (AREA)
- Application Of Or Painting With Fluid Materials (AREA)
Description
【発明の詳細な説明】
本発明は、プラスチツクのメタライジングの一
方法としてのスパツタリングをポリアセタール成
形物に適通するための技術を提供するものであ
る。
一般にABS等で行われているスパツタリング
によるメタライズ化は、成形物を適当な溶剤で脱
脂した後、成形物にベースコート、例えばウレタ
ン塗料やポリエステル−ウレタン塗料、アクリル
−ウレタン塗料、アクリルエステル塗料等を塗
布・乾燥させた上、スパツタリング装置によりク
ロムSUS−304、クロム合金、アルミニウム等を
アルゴンガス圧５×10-3〜２×10-4Torrの圧力
下で、スパツタして300〜1000Å程度の金属薄膜
を生成させ、その上にトツプコート、例えばアク
リルエステル塗料やアクリルウレタン塗料等を塗
布乾燥させ、成形物に金属的光沢を与えるもので
ある。
ところが、ポリアセタール樹脂は結晶性の樹脂
で化学的に安定であり、成形物を脱脂しただけで
成形物に実用に供する十分な密着性を与える有効
なベースコート塗料は未だに見つかつていない。
そのため一般のスパツタリング手法をそのまま適
用するわけにはいかない。
本発明者はポリアセタール成形物に上記の如き
一般のスパツタリング用ベースコート塗料を塗布
した場合、成形物に対して十分な密着性を持た
せ、かつ塗装後も塗膜の平滑性を失わず、スパツ
タリングによつてメタライズされた成形物が十分
実用に供する性能を持つことができるような方法
について研究の結果、ポリアセタール成形物を特
定の酸の混合水溶液で表面処理し、次いでベース
コート塗料を塗布することが非常に有効であるこ
とを見出して本発明に到つたものである。
即ち本発明は、ポリアセタール成形物を硫酸と
塩酸、リン酸、酢酸及びトルエンスルホン酸から
選ばれた１種又は２種以上の酸との混酸水溶液で
表面処理し、次いでベースコート塗料を塗布する
ことを特徴とするポリアセタール成形物をスパツ
タリングによりメタライズ化するためのポリアセ
タール成形物の表面処理法に係るものである。
本発明の方法によれば、特定の無機酸混合水溶
液又は無機酸と有機酸の混合水溶液を用いてポリ
アセタール成形物を表面処理することにより、ベ
ースコートの成形物に対する強力な接着を可能に
し、又かかる表面処理は表面の平滑性を損なわ
ず、更に金属をスパツタするに適した良好な表面
を提供し得る。
この場合、硫酸単独、塩酸単独、重クロム酸カ
リウムと硫酸との混合水溶液等の酸による処理で
も本発明の企画する上記効果は達成し得るが、処
理条件によつてはベース樹脂の分解を生ぜしめ、
ホルムアルデヒドの分解生成物が表面に付着した
り、また成形品の表面にクラツクが発生する等の
問題が生じ、好ましくない。即ち、上記酸化性の
酸を用いる場合、処理時間を25℃で180秒以内に
抑える必要があり、工業的にコントロールするの
が困難であるという欠点を有する。
これに対し本発明の酸の混合水溶液は、例えば
硫酸にリン酸を加えることにより表面処理をマイ
ルドにする効果があり、工業的に処理条件に幅が
あり、コントロールしやすいという利点がある。
本発明の酸の混合水溶液によるポリアセタール
成形物表面の処理条件は一般に０〜80℃で40分以
下が好ましい。特に好ましい条件を挙げれば、硫
酸と塩酸の混合水溶液の場合、硫酸濃度として30
〜60重量％、塩酸濃度として５〜30重量％、水濃
度65〜10重量％で０〜30℃で10分以下、硫酸とリ
ン酸の混酸系の場合、硫酸濃度20〜50重量％、リ
ン酸濃度30〜50重量％、水濃度50〜０重量％で０
〜30℃で15分以下である。
ポリアセタール成形物の酸による表面処理後、
成形物は中和剤溶液中に浸漬され、成形物の表面
上の酸性物質を中和する。次いで成形物にベース
コート塗料を塗布し、例えば120℃、30分間加熱
乾燥する。次いでその成形物表面にスパツタリン
グによりメタライズ化を行う。この様にして、ク
ラツクのない密着の良好な均一な厚さの金属層を
ベースコート上に作ることができる。
本発明に用いられるポリアセタールなる用語
は、ポリアセタールホモポリマー、各種のポリア
セタールコポリマー及び種々の化合物で変性され
たポリアセタールホモポリマー及びコポリマーを
包含する。樹脂組成物中には一般に使われる添加
物が含まれていても良い。例えば、炭酸カルシウ
ム、タルク等の充填物、ガラス繊維、ビーズ、ガ
ラスフレーク、雲母等の無機補強剤及び有機補強
剤、有機改質剤、安定剤等が含まれていてもよ
い。
本発明においてベースコート及びトツプコート
に用いる塗料及びその塗装法、並びにスパツタリ
ングによるメタライズ化の手法は、上記せる従来
の方法と同様に実施し得る。
以下実施例により本発明を詳細に説明する。
実施例１〜６、比較例１〜２
ポリアセタール樹脂ジユラコンM90（ポリプ
ラスチツクス(株)製）の成形平板50×70×3t（mm）
を有機溶剤で脱脂し、次いで表−１に示した種々
の表面処理条件で表面処理した後、50％の苛性ソ
ーダ水溶液中に板を浸漬して、板表面の残留酸を
中和した。その後スパツタリング用ベースコート
としてポリエステル−ウレタン系塗料（藤倉化成
(株)製商品名EXP1245）を塗布し、120℃で30分間
乾燥した。このベースコートを施した成形物を徳
田製作所製スパツタリング装置CFS−8ES中に置
き、クムロ合金を300〜400Åの厚さにスパツタし
た。スパツタした成形試験片の上に更にトツプコ
ートとしてアクリルウレタン系塗料（藤倉化成(株)
製商品名EXP1380）を塗布し、80℃で30分間乾
燥硬化させた。この工程を下記に示す。このよう
にしてメタライズ化した成形試験片に於けるメタ
ライズド被膜の密着性、即ち母材に対する（ベー
スコート＋スパツタ金属膜＋トツプコート）の密
着性を次の様に調べた。即ち被膜にナイフで１mm
間隔の線を11本罫書きし、100コマのマス目を１
cm2当りに作り、このゴバン目にセロハンテープを
密着させ、テープを板面に対して180゜の方向に剥
がした時のゴバン目の密着残存数をゴバン目総数
100個当りについて調べた。
メタライズド膜の光沢は外観からの目視により
判断した。
結果を表−１に示す。
ポリアセタールのスパツタリング手順
ポリアセタール成形品
↓
脱 脂
↓
酸 処 理* ＊必要に応じて成形品
↓ ひずみを除去するた
中 和 めのアニーリングを
↓ 行つてから酸処理す
ベースコート る。
↓
スパツタリング
↓
トツプコート
【表】DETAILED DESCRIPTION OF THE INVENTION The present invention provides a technique for applying sputtering as a method of metallizing plastics to polyacetal molded articles. Metallization by sputtering, which is generally done with ABS, involves degreasing the molded product with an appropriate solvent and then applying a base coat, such as urethane paint, polyester-urethane paint, acrylic-urethane paint, or acrylic ester paint, to the molded product.・After drying, chromium SUS-304, chromium alloy, aluminum, etc. are sputtered using a sputtering device under an argon gas pressure of 5×10 -3 to 2×10 -4 Torr to form a metal thin film of about 300 to 1000 Å. A top coat such as an acrylic ester paint or an acrylic urethane paint is applied thereon and dried to give the molded product a metallic luster. However, polyacetal resin is a crystalline resin and is chemically stable, and an effective base coat paint that provides sufficient adhesion for practical use on molded products simply by degreasing the molded products has not yet been found.
Therefore, general sputtering methods cannot be applied as is. The present inventor has found that when a general base coat paint for sputtering as described above is applied to a polyacetal molded product, it has sufficient adhesion to the molded product and does not lose the smoothness of the coating even after painting, preventing sputtering. As a result of research on a method for making metallized moldings have sufficient performance for practical use, it was found that it is extremely important to surface treat polyacetal moldings with a mixed aqueous solution of a specific acid, and then apply a base coat paint. The present invention was developed based on the discovery that this method is effective for the following purposes. That is, the present invention involves surface-treating a polyacetal molded article with a mixed acid aqueous solution of sulfuric acid and one or more acids selected from hydrochloric acid, phosphoric acid, acetic acid, and toluenesulfonic acid, and then applying a base coat paint. The present invention relates to a surface treatment method for a polyacetal molded product for metalizing the polyacetal molded product by sputtering. According to the method of the present invention, strong adhesion of the base coat to the molded product is made possible by surface-treating the polyacetal molded product using a specific inorganic acid mixed aqueous solution or a mixed inorganic acid and organic acid mixed aqueous solution, and The surface treatment does not impair the smoothness of the surface and may further provide a good surface suitable for sputtering metal. In this case, the above effects planned by the present invention can be achieved by treatment with acids such as sulfuric acid alone, hydrochloric acid alone, or a mixed aqueous solution of potassium dichromate and sulfuric acid, but depending on the treatment conditions, the base resin may decompose. Close,
Problems such as formaldehyde decomposition products adhering to the surface and cracks occurring on the surface of the molded article are undesirable. That is, when using the above-mentioned oxidizing acid, it is necessary to limit the treatment time to 180 seconds or less at 25° C., which has the drawback that it is difficult to control it industrially. On the other hand, the mixed aqueous acid solution of the present invention has the effect of milder surface treatment by adding phosphoric acid to sulfuric acid, for example, and has the advantage of having a wide range of industrial treatment conditions and being easy to control. The conditions for treating the surface of a polyacetal molded product with the mixed aqueous solution of the acid of the present invention are generally preferably 0 to 80°C for 40 minutes or less. Particularly preferable conditions include a mixed aqueous solution of sulfuric acid and hydrochloric acid with a sulfuric acid concentration of 30
~60% by weight, hydrochloric acid concentration of 5 to 30% by weight, water concentration of 65 to 10% by weight at 0 to 30℃ for 10 minutes or less, in the case of a mixed acid system of sulfuric acid and phosphoric acid, sulfuric acid concentration of 20 to 50% by weight, phosphorus 0 at acid concentration 30-50% by weight and water concentration 50-0% by weight
No more than 15 minutes at ~30°C. After surface treatment of polyacetal moldings with acid,
The molded article is immersed in a neutralizing agent solution to neutralize acidic substances on the surface of the molded article. Next, a base coat paint is applied to the molded product, and the molded product is heated and dried at, for example, 120° C. for 30 minutes. Next, metallization is performed on the surface of the molded product by sputtering. In this way, a metal layer of uniform thickness with good adhesion and no cracks can be produced on the base coat. The term polyacetal as used in the present invention includes polyacetal homopolymers, various polyacetal copolymers, and polyacetal homopolymers and copolymers modified with various compounds. The resin composition may contain commonly used additives. For example, fillers such as calcium carbonate and talc, inorganic and organic reinforcing agents such as glass fibers, beads, glass flakes, and mica, organic modifiers, stabilizers, and the like may be included. In the present invention, the paint used for the base coat and top coat, the coating method thereof, and the metallization method by sputtering can be carried out in the same manner as the above-mentioned conventional method. The present invention will be explained in detail below with reference to Examples. Examples 1 to 6, Comparative Examples 1 to 2 Molded flat plate of polyacetal resin Diuracon M90 (manufactured by Polyplastics Co., Ltd.) 50 x 70 x 3t (mm)
After degreasing with an organic solvent and then surface treating under various surface treatment conditions shown in Table 1, the plate was immersed in a 50% caustic soda aqueous solution to neutralize residual acid on the plate surface. After that, polyester-urethane paint (Fujikura Kasei Co., Ltd.) was used as a base coat for sputtering.
Co., Ltd. (trade name: EXP1245) was applied and dried at 120°C for 30 minutes. The base coated molded product was placed in a CFS-8ES sputtering device manufactured by Tokuda Seisakusho, and Kumuro alloy was sputtered to a thickness of 300 to 400 Å. Acrylic urethane paint (Fujikura Kasei Co., Ltd.) was applied as a top coat on the spattered molded test piece.
(trade name: EXP1380) was applied and dried and cured at 80°C for 30 minutes. This process is shown below. The adhesion of the metallized coating on the thus metallized molded test piece, that is, the adhesion of (base coat + sputtered metal film + top coat) to the base material, was investigated as follows. That is, 1 mm into the film with a knife.
Draw 11 lines at intervals and draw 1 square of 100 frames.
Make cellophane tape per cm 2 , stick cellophane tape tightly to these goblets, and when the tape is peeled off in a direction of 180° to the board surface, calculate the number of sticks remaining that are the total number of goblins.
I looked into the per 100 pieces. The gloss of the metallized film was judged visually from its appearance. The results are shown in Table-1. Polyacetal sputtering procedure Polyacetal molded product ↓ Degreasing ↓ Acid treatment * *If necessary, molded product ↓ Neutralizing annealing to remove distortion ↓ After that, perform acid treatment Base coat. ↓ Sputtering ↓ Top coat [front]
Claims (1)
酸、酢酸及びトルエンスルホン酸から選ばれた１
種又は２種以上の酸との混酸水溶液で表面処理
し、次いでベースコート塗料を塗布することを特
徴とするポリアセタール成形物をスパツタリング
によりメタライズ化するためのポリアセタール成
形物の表面処理法。 ２ 混酸水溶液が (1) 30〜60重量％の硫酸及び５〜30重量％の塩酸
を含有する水溶液、又は (2) 20〜50重量％の硫酸及び30〜50重量％のリン
酸を含有する水溶液 である特許請求の範囲第１項記載の表面処理法。[Claims] 1. The polyacetal molded product is made of 1 selected from sulfuric acid, hydrochloric acid, phosphoric acid, acetic acid, and toluenesulfonic acid.
1. A method for surface treatment of a polyacetal molded product for metalizing the polyacetal molded product by sputtering, the method comprising treating the surface with an aqueous solution of a mixed acid with a seed or two or more acids, and then applying a base coat paint. 2. The mixed acid aqueous solution contains (1) 30 to 60% by weight of sulfuric acid and 5 to 30% by weight of hydrochloric acid, or (2) 20 to 50% by weight of sulfuric acid and 30 to 50% by weight of phosphoric acid. The surface treatment method according to claim 1, which is an aqueous solution.
Priority Applications (4)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| JP55172499A JPS5796026A (en) | 1980-12-05 | 1980-12-05 | Surface treatment for sputtering |
| GB8136306A GB2091274B (en) | 1980-12-05 | 1981-12-02 | A process for the treatment of polyacetal articles |
| KR1019810004736A KR870001091B1 (en) | 1980-12-05 | 1981-12-04 | Surface treatment method of poliacetal resin for spattering |
| HK163/86A HK16386A (en) | 1980-12-05 | 1986-03-06 | A process for the treatment of polyacetal articles |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| JP55172499A JPS5796026A (en) | 1980-12-05 | 1980-12-05 | Surface treatment for sputtering |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| JPS5796026A JPS5796026A (en) | 1982-06-15 |
| JPH0158266B2 true JPH0158266B2 (en) | 1989-12-11 |
Family
ID=15943101
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| JP55172499A Granted JPS5796026A (en) | 1980-12-05 | 1980-12-05 | Surface treatment for sputtering |
Country Status (4)
| Country | Link |
|---|---|
| JP (1) | JPS5796026A (en) |
| KR (1) | KR870001091B1 (en) |
| GB (1) | GB2091274B (en) |
| HK (1) | HK16386A (en) |
Families Citing this family (8)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JPH0765154B2 (en) * | 1985-09-02 | 1995-07-12 | ポリプラスチックス株式会社 | Resin molded product with surface metal treatment |
| JPH062836B2 (en) * | 1986-08-06 | 1994-01-12 | ポリプラスチックス株式会社 | Surface treatment method for polyacetal resin moldings |
| JPH0649179B2 (en) * | 1986-09-01 | 1994-06-29 | ポリプラスチックス株式会社 | Painted polyacetal resin molding |
| US5094713A (en) * | 1988-02-16 | 1992-03-10 | Hoechst Celanese Corporation | Process for improving the adhesion to polyacetal articles |
| FR2703074B1 (en) * | 1990-11-27 | 1996-01-05 | Eumail | Process for treating chromable polyacetals with a mixture of acids. |
| JP4414346B2 (en) * | 2002-12-20 | 2010-02-10 | イー・アイ・デュポン・ドウ・ヌムール・アンド・カンパニー | Surface treatment of polyacetal articles |
| ES2288426B1 (en) * | 2006-06-26 | 2008-12-16 | Albert Sanahuja Julibert | PRE-TREATMENT PROCEDURE FOR A PART OR SURFACE OF PLASTIC MATERIAL, IN PARTICULAR OF METHYLENE POLYOXIDE. |
| CN103757677B (en) * | 2013-11-29 | 2017-01-25 | 云南云天化股份有限公司 | Polyformaldehyde product surface processing method |
-
1980
- 1980-12-05 JP JP55172499A patent/JPS5796026A/en active Granted
-
1981
- 1981-12-02 GB GB8136306A patent/GB2091274B/en not_active Expired
- 1981-12-04 KR KR1019810004736A patent/KR870001091B1/en not_active Expired
-
1986
- 1986-03-06 HK HK163/86A patent/HK16386A/en not_active IP Right Cessation
Also Published As
| Publication number | Publication date |
|---|---|
| KR830007879A (en) | 1983-11-07 |
| GB2091274B (en) | 1985-08-21 |
| KR870001091B1 (en) | 1987-06-04 |
| JPS5796026A (en) | 1982-06-15 |
| HK16386A (en) | 1986-03-14 |
| GB2091274A (en) | 1982-07-28 |
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