JPS6157911B2 - - Google Patents
Info
- Publication number
- JPS6157911B2 JPS6157911B2 JP3328782A JP3328782A JPS6157911B2 JP S6157911 B2 JPS6157911 B2 JP S6157911B2 JP 3328782 A JP3328782 A JP 3328782A JP 3328782 A JP3328782 A JP 3328782A JP S6157911 B2 JPS6157911 B2 JP S6157911B2
- Authority
- JP
- Japan
- Prior art keywords
- film
- etching
- minutes
- resin film
- water
- 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
- QAOWNCQODCNURD-UHFFFAOYSA-N Sulfuric acid Chemical compound OS(O)(=O)=O QAOWNCQODCNURD-UHFFFAOYSA-N 0.000 claims description 14
- 238000000034 method Methods 0.000 claims description 12
- 238000005530 etching Methods 0.000 claims description 10
- 239000011347 resin Substances 0.000 claims description 10
- 229920005989 resin Polymers 0.000 claims description 10
- 239000000203 mixture Substances 0.000 claims description 9
- KRVSOGSZCMJSLX-UHFFFAOYSA-L chromic acid Substances O[Cr](O)(=O)=O KRVSOGSZCMJSLX-UHFFFAOYSA-L 0.000 claims description 6
- 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 claims description 6
- 238000007772 electroless plating Methods 0.000 claims description 5
- 238000004381 surface treatment Methods 0.000 claims description 4
- 239000012670 alkaline solution Substances 0.000 claims description 2
- HEMHJVSKTPXQMS-UHFFFAOYSA-M Sodium hydroxide Chemical compound [OH-].[Na+] HEMHJVSKTPXQMS-UHFFFAOYSA-M 0.000 description 12
- 229910052751 metal Inorganic materials 0.000 description 10
- 239000002184 metal Substances 0.000 description 9
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 9
- 238000007747 plating Methods 0.000 description 6
- 229920006267 polyester film Polymers 0.000 description 6
- 239000000243 solution Substances 0.000 description 6
- KWYUFKZDYYNOTN-UHFFFAOYSA-M Potassium hydroxide Chemical compound [OH-].[K+] KWYUFKZDYYNOTN-UHFFFAOYSA-M 0.000 description 5
- 239000007788 liquid Substances 0.000 description 5
- VYZAMTAEIAYCRO-UHFFFAOYSA-N Chromium Chemical compound [Cr] VYZAMTAEIAYCRO-UHFFFAOYSA-N 0.000 description 4
- VEXZGXHMUGYJMC-UHFFFAOYSA-N Hydrochloric acid Chemical compound Cl VEXZGXHMUGYJMC-UHFFFAOYSA-N 0.000 description 4
- PXHVJJICTQNCMI-UHFFFAOYSA-N Nickel Chemical compound [Ni] PXHVJJICTQNCMI-UHFFFAOYSA-N 0.000 description 4
- KDLHZDBZIXYQEI-UHFFFAOYSA-N Palladium Chemical compound [Pd] KDLHZDBZIXYQEI-UHFFFAOYSA-N 0.000 description 4
- 239000002318 adhesion promoter Substances 0.000 description 4
- 239000007864 aqueous solution Substances 0.000 description 4
- 238000009713 electroplating Methods 0.000 description 4
- 150000007522 mineralic acids Chemical class 0.000 description 4
- 238000002791 soaking Methods 0.000 description 4
- 230000003746 surface roughness Effects 0.000 description 4
- 239000011324 bead Substances 0.000 description 3
- 230000007613 environmental effect Effects 0.000 description 3
- 239000011521 glass Substances 0.000 description 3
- 229920000728 polyester Polymers 0.000 description 3
- 239000000126 substance Substances 0.000 description 3
- 238000005406 washing Methods 0.000 description 3
- WMFOQBRAJBCJND-UHFFFAOYSA-M Lithium hydroxide Chemical compound [Li+].[OH-] WMFOQBRAJBCJND-UHFFFAOYSA-M 0.000 description 2
- 229910018104 Ni-P Inorganic materials 0.000 description 2
- 229910018536 Ni—P Inorganic materials 0.000 description 2
- ATJFFYVFTNAWJD-UHFFFAOYSA-N Tin Chemical compound [Sn] ATJFFYVFTNAWJD-UHFFFAOYSA-N 0.000 description 2
- WGLPBDUCMAPZCE-UHFFFAOYSA-N Trioxochromium Chemical compound O=[Cr](=O)=O WGLPBDUCMAPZCE-UHFFFAOYSA-N 0.000 description 2
- HCHKCACWOHOZIP-UHFFFAOYSA-N Zinc Chemical compound [Zn] HCHKCACWOHOZIP-UHFFFAOYSA-N 0.000 description 2
- 230000002378 acidificating effect Effects 0.000 description 2
- 239000012190 activator Substances 0.000 description 2
- 229910052878 cordierite Inorganic materials 0.000 description 2
- 238000000151 deposition Methods 0.000 description 2
- 229910052759 nickel Inorganic materials 0.000 description 2
- 239000007800 oxidant agent Substances 0.000 description 2
- 230000003647 oxidation Effects 0.000 description 2
- 238000007254 oxidation reaction Methods 0.000 description 2
- 230000001590 oxidative effect Effects 0.000 description 2
- 229910052763 palladium Inorganic materials 0.000 description 2
- -1 polyethylene Polymers 0.000 description 2
- 239000011135 tin Substances 0.000 description 2
- 229910052725 zinc Inorganic materials 0.000 description 2
- 239000011701 zinc Substances 0.000 description 2
- 241000694440 Colpidium aqueous Species 0.000 description 1
- RYGMFSIKBFXOCR-UHFFFAOYSA-N Copper Chemical compound [Cu] RYGMFSIKBFXOCR-UHFFFAOYSA-N 0.000 description 1
- XEEYBQQBJWHFJM-UHFFFAOYSA-N Iron Chemical compound [Fe] XEEYBQQBJWHFJM-UHFFFAOYSA-N 0.000 description 1
- 239000004698 Polyethylene Substances 0.000 description 1
- 239000004642 Polyimide Substances 0.000 description 1
- 239000003082 abrasive agent Substances 0.000 description 1
- 239000002253 acid Substances 0.000 description 1
- 230000004913 activation Effects 0.000 description 1
- 239000000853 adhesive Substances 0.000 description 1
- 230000001070 adhesive effect Effects 0.000 description 1
- 239000003513 alkali Substances 0.000 description 1
- 239000011248 coating agent Substances 0.000 description 1
- 238000000576 coating method Methods 0.000 description 1
- 238000004040 coloring Methods 0.000 description 1
- 230000000052 comparative effect Effects 0.000 description 1
- 229910052802 copper Inorganic materials 0.000 description 1
- 239000010949 copper Substances 0.000 description 1
- 229910052593 corundum Inorganic materials 0.000 description 1
- 239000010431 corundum Substances 0.000 description 1
- JSKIRARMQDRGJZ-UHFFFAOYSA-N dimagnesium dioxido-bis[(1-oxido-3-oxo-2,4,6,8,9-pentaoxa-1,3-disila-5,7-dialuminabicyclo[3.3.1]nonan-7-yl)oxy]silane Chemical compound [Mg++].[Mg++].[O-][Si]([O-])(O[Al]1O[Al]2O[Si](=O)O[Si]([O-])(O1)O2)O[Al]1O[Al]2O[Si](=O)O[Si]([O-])(O1)O2 JSKIRARMQDRGJZ-UHFFFAOYSA-N 0.000 description 1
- 239000011888 foil Substances 0.000 description 1
- CUILPNURFADTPE-UHFFFAOYSA-N hypobromous acid Chemical compound BrO CUILPNURFADTPE-UHFFFAOYSA-N 0.000 description 1
- 238000007654 immersion Methods 0.000 description 1
- 238000010030 laminating Methods 0.000 description 1
- 239000002932 luster Substances 0.000 description 1
- 239000000463 material Substances 0.000 description 1
- 229920000573 polyethylene Polymers 0.000 description 1
- 229920001721 polyimide Polymers 0.000 description 1
- 239000001044 red dye Substances 0.000 description 1
- 238000007788 roughening Methods 0.000 description 1
- 229910010271 silicon carbide Inorganic materials 0.000 description 1
- 239000000758 substrate Substances 0.000 description 1
- 230000002522 swelling effect Effects 0.000 description 1
Landscapes
- Treatments Of Macromolecular Shaped Articles (AREA)
- Chemically Coating (AREA)
Description
【発明の詳細な説明】
本発明はポリエステル等の樹脂フイルム上に金
属被膜を密着良く析出させるための表面処理方法
に関する。DETAILED DESCRIPTION OF THE INVENTION The present invention relates to a surface treatment method for depositing a metal film on a resin film such as polyester with good adhesion.
従来ポリエステルフイルムは耐酸化性が高く、
ポリエステルフイルム上に直接メツキする技術は
紹介されておらず、金属箔をラミネートするとき
の接着力向上のための手段が、幾つか紹介されて
いるのみである。例えば、
酸化性のある無機酸、あるいは無機酸とアル
カリとの混合液。その中で無機酸としては
KMnO4，NaCO3，K2CrO7等。又アルカリと
してはNaOH，KOH，LiOH，Na2CO3等。更に
酸化性のある無機酸の15〜95％溶液。それに
はHNO3，CrO3，HCO3，HBrO4等が紹介さ
れている。更に
火炎をあてて親水性にする方法。ホーニング
等により粗化する方法等も紹介されている。し
かし乍ら以上挙げた技術では金属被膜をメツキ
によつて１μ以上の厚さで密着良く析出させる
には不充分であつた。 Conventional polyester film has high oxidation resistance,
No technology for directly plating onto polyester film has been introduced, and only some methods for improving adhesive strength when laminating metal foil have been introduced. For example, oxidizing inorganic acids or mixtures of inorganic acids and alkalis. Among them, as an inorganic acid
KMnO 4 , NaCO 3 , K 2 CrO 7 etc. Also, examples of alkalis include NaOH, KOH, LiOH, Na 2 CO 3 , etc. Additionally 15-95% solutions of oxidizing inorganic acids. It introduces HNO 3 , CrO 3 , HCO 3 , HBrO 4 , etc. Another method is to apply flame to make it hydrophilic. A method of roughening by honing etc. is also introduced. However, the above-mentioned techniques were not sufficient to deposit a metal film with a thickness of 1 μm or more with good adhesion by plating.
本発明の目的は、ポリエステル等の樹脂フイル
ム上に金属被膜を密着良く析出させる表面処理方
法を提供することにある。 An object of the present invention is to provide a surface treatment method for depositing a metal film with good adhesion on a resin film such as polyester.
他の目的は、機械的強度、耐熱性の優れた金属
コート樹脂フイルムを提供することにある。 Another object is to provide a metal-coated resin film with excellent mechanical strength and heat resistance.
その特徴とするところは、樹脂フイルムをPH12
以上のアルカリ液でエツチングする工程と、クロ
ム酸硫酸混液でエツチングする工程と、メツキす
る工程とを有する樹脂フイルムの表面処理方法に
ある。 The feature is that the resin film is made of PH12
The method of surface treatment of a resin film includes the steps of etching with an alkaline solution, etching with a chromic acid/sulfuric acid mixture, and plating.
本発明方法においては、第１ステツプとしてア
ルカリエツチングによる膨潤作用と同時に低結晶
の分子質を溶出させる。次に第２ステツプとして
クロム酸硫酸混液によるエツチング処理により酸
化し、適当な表面凹凸を形成する。 In the method of the present invention, as a first step, low-crystalline molecular substances are eluted simultaneously with the swelling action of alkaline etching. Next, as a second step, oxidation is performed by etching with a chromic acid/sulfuric acid mixture to form appropriate surface irregularities.
本発明に用いるPHが12以上のアルカリは
NaOH，KOHが良好で、液温度は20℃〜80℃、
浸漬時間は５分〜30分が適している。 The alkali with a pH of 12 or more used in the present invention is
NaOH, KOH are good, liquid temperature is 20℃~80℃,
A suitable soaking time is 5 to 30 minutes.
次に行なう、クロム酸硫酸混液はCrO3が50
ｇ／以上（好ましくは50〜300ｇ／）で硫酸
は18Nに換算して50c.c.／〜300c.c.／、液温度
は20〜80℃、浸漬時間は５分〜30分が適してい
る。 Next, the chromic acid/sulfuric acid mixture contains 50 % CrO3.
g/ or more (preferably 50 to 300 g/), sulfuric acid is 50 c.c./ to 300 c.c./ in terms of 18N, the liquid temperature is 20 to 80°C, and the immersion time is 5 to 30 minutes. There is.
本発明の方法は前述の２度のエツチング処理に
先立つてホーニング処理により表面が適当な凹凸
を有する事によりその効果はさらに向上する。こ
こで用いるホーニング処理としては、液体ホーニ
ング、ドライホーニング等が挙げられ、用いる研
磨材にはガラスビーズ、コランダム、鉄粉、カー
ボランダムがありその表面粗さは１μ以上が適し
ている。この粗さは、表面粗さ計で測定した時の
Rmax−minの値である。 The effectiveness of the method of the present invention is further improved by honing the surface to give it an appropriate roughness prior to the two etching steps described above. Examples of the honing treatment used here include liquid honing and dry honing, and the abrasive materials used include glass beads, corundum, iron powder, and carborundum, and a surface roughness of 1 μm or more is suitable. This roughness is measured using a surface roughness meter.
This is the value of Rmax−min.
本発明において金属皮膜を形成するには、無電
解メツキ液（例えば日本カニゼン社製のＳ−
653、ワールドメタル社製ニボロン等）であれ
ば、いかなるものでも良い。この時必要に応じ
て、該無電解メツキ処理後、電気メツキを析出さ
せる事により、種々の色調の金属光沢を有する、
金属ポリエステルフイルムが得られる。ここで用
いる電気メツキとしては、例えばサージエント型
装飾用クロムメツキ液、ブラツククロム液（例え
ば荏原コージライト(株)製：ネロスタープロセス、
酸性亜鉛メツキ浴）等が用いられる。 In the present invention, in order to form a metal film, an electroless plating solution (for example, S-
653, World Metal's Nibolon, etc.), any material may be used. At this time, if necessary, after the electroless plating treatment, electroplating is deposited to produce metallic luster in various tones.
A metallic polyester film is obtained. The electroplating used here includes, for example, sergeant type decorative chrome plating liquid, black chrome liquid (for example, Nerostar Process manufactured by Ebara Cordierite Co., Ltd.),
Acidic zinc plating bath) etc. are used.
以上によりポリエステル、ポリイミド、ポリパ
ラバン酸、ポリエチレン等の樹脂フイルム、特に
ポリエステルフイルムに密着性良好な金属被膜を
形成する事が出来、この結果樹脂フイルムの機械
的強度、耐熱性が向上する。 As described above, a metal coating with good adhesion can be formed on a resin film such as polyester, polyimide, polyparabanic acid, polyethylene, etc., especially a polyester film, and as a result, the mechanical strength and heat resistance of the resin film are improved.
無電解メツキの前に、必要に応じて活性化剤
（錫とパラジウムと塩酸の混合液等）、密着促進剤
（酸化剤等）等の処理を行なつても良い。 Before electroless plating, treatment with an activator (mixture of tin, palladium, hydrochloric acid, etc.), adhesion promoter (oxidizing agent, etc.) may be performed as necessary.
以下、本発明を実施例に従つて説明する。 Hereinafter, the present invention will be explained according to examples.
〔実施例 １〕
＃120のガラスビーズによるホーニング処理を
施し１μの表面粗さとなつた。50μのポリエステ
ルフイルムを、PH13のNaOH、50℃の水溶液に10
分間浸漬してエツチング後、水洗した。次いで
CnO3100ｇ／・18NH2SO4100c.c.／を混合し
た50℃の水溶液に10分間浸漬してエツチング後水
洗した。その後錫とパラジウムと塩酸の混合液で
ある活性化剤（日立化成社製HS−101B）に20℃
５分間浸漬した後、水洗した。その後密着促進剤
としての酸化剤（室町化学工業社製MK−330）
に20℃３分間浸漬した後水洗した。その後無電解
ニツケルメツキ（日本カニゼンKK社製Ｓ−
753）の90℃に60分間浸漬し、15μのNi−Ｐ皮膜
を得た。この皮膜は60℃−90％240時間の環境テ
スト前後において良好な密着力を示した。[Example 1] Honing treatment was performed using #120 glass beads to obtain a surface roughness of 1μ. A 50μ polyester film was placed in an aqueous solution of PH13 NaOH at 50℃ for 10 minutes.
After soaking for a minute and etching, it was washed with water. then
It was etched by immersing it in an aqueous solution at 50° C. containing 100 g of CnO 3 /100 c.c. of 18NH 2 SO 4 for 10 minutes, and then washing with water. After that, it was added to an activator (HS-101B manufactured by Hitachi Chemical Co., Ltd.), which is a mixture of tin, palladium, and hydrochloric acid, at 20°C.
After soaking for 5 minutes, it was washed with water. After that, an oxidizing agent (MK-330 manufactured by Muromachi Chemical Industry Co., Ltd.) as an adhesion promoter
After soaking at 20°C for 3 minutes, it was washed with water. After that, electroless nickel metal fittings (S- made by Nippon Kanizen KK Co., Ltd.)
753) at 90°C for 60 minutes to obtain a 15μ Ni-P film. This film showed good adhesion before and after an environmental test at 60°C and 90% for 240 hours.
〔実施例 ２〕
実施例−１において、アルカリ浴をPH12.5の
KOH液（60℃）とし、クロム酸200ｇ／・18N
硫酸200c.c.／の混液でエツチングした。密着促
進剤にて処理したフイルムを10分間無電解銅メツ
キ（日立化成CUST−201）し水洗した。その
後、ブラツククローム電気メツキ液（荏原コージ
ライト製ネロスタープロセス）にて0.2μのブラ
ツククローム皮膜を得た。この皮膜は60℃−90％
240時間の環境テスト前後において良好な密着力
を示した。[Example 2] In Example-1, the alkaline bath was adjusted to pH 12.5.
KOH solution (60℃), chromic acid 200g/・18N
Etching was performed with a mixture of 200 c.c. of sulfuric acid. The film treated with the adhesion promoter was electroless copper plated (Hitachi Chemical CUST-201) for 10 minutes and washed with water. Thereafter, a black chrome film of 0.2μ was obtained using a black chrome electroplating solution (Nerostar Process manufactured by Ebara Cordierite). This film is 60℃-90%
It showed good adhesion before and after a 240 hour environmental test.
〔実施例 ３〕
実施例−１において、アルカリ浴と、クロム酸
硫酸混液をいずれも70℃とした。密着促進剤にて
処理したフイルムを10分間無電解ニツケルメツキ
（ワールドメタル社製、ニボロンMNP）し水洗し
た。その後酸性亜鉛電気メツキ液（ドイツシユー
リング社製、エクセルツクス）にて10μ析出さ
せ、その後クロメード処理を行ない水洗し、赤色
の染料液に浸漬し、着色した。この皮膜は60℃−
90％240時間の環境テスト前後において良好な密
着力を示した。[Example 3] In Example-1, the temperature of both the alkaline bath and the chromic acid/sulfuric acid mixture was 70°C. The film treated with the adhesion promoter was subjected to electroless nickel plating (Niboron MNP manufactured by World Metal Co., Ltd.) for 10 minutes and washed with water. Thereafter, 10μ of acidic zinc electroplating solution (manufactured by Schüring AG, Germany, Excelx) was deposited, followed by chromade treatment, washing with water, and coloring by immersing in a red dye solution. This film is 60℃−
90% showed good adhesion before and after the 240 hour environmental test.
〔比較例 １〕
＃120のガラスビーズによるホーニング処理を
施し１μの表面粗さとなつた50μのポリエステル
フイルムをPH11のNaOH50℃の水溶液に10分間浸
漬してエツチング後水洗した。次いでCnO3100
ｇ／・H2SO4100c.c.／を混合した50℃の水溶
液に３分間浸漬してエツチング後水洗した。その
後活性化処理、密着促進処理、実施例−１と同じ
無電解メツキを施し15μのNi−Ｐ皮膜を得た。
この皮膜は析出後皮膜のフクレを生じ、テープイ
ングによる密着試験にて剥れを生じた。[Comparative Example 1] A 50 μm polyester film that had been honed with #120 glass beads to have a surface roughness of 1 μm was immersed in a pH 11 NaOH aqueous solution at 50° C. for 10 minutes, etched, and then washed with water. Then CnO 3 100
After etching, the substrate was immersed in a 50° C. aqueous solution containing 100 c.c./g/·H 2 SO 4 of 100 c.c./cm, followed by washing with water. Thereafter, activation treatment, adhesion promotion treatment, and electroless plating as in Example 1 were performed to obtain a 15 μm Ni-P film.
This film blistered after being deposited, and peeled off in an adhesion test using taping.
Claims (1)
チングする工程と、クロム酸硫酸混液でエツチン
グする工程と、無電解メツキする工程とを有する
樹脂フイルムの表面処理方法。1. A method for surface treatment of a resin film, comprising the steps of etching the resin film with an alkaline solution having a pH of 12 or higher, etching the resin film with a chromic acid/sulfuric acid mixture, and electroless plating.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| JP3328782A JPS58149924A (en) | 1982-03-03 | 1982-03-03 | Surface treatment of resin film |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| JP3328782A JPS58149924A (en) | 1982-03-03 | 1982-03-03 | Surface treatment of resin film |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| JPS58149924A JPS58149924A (en) | 1983-09-06 |
| JPS6157911B2 true JPS6157911B2 (en) | 1986-12-09 |
Family
ID=12382313
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| JP3328782A Granted JPS58149924A (en) | 1982-03-03 | 1982-03-03 | Surface treatment of resin film |
Country Status (1)
| Country | Link |
|---|---|
| JP (1) | JPS58149924A (en) |
Families Citing this family (7)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JPH0639712B2 (en) * | 1984-11-21 | 1994-05-25 | 東レ株式会社 | Method for producing surface metallized thermoplastic polyester resin molded article |
| JPH0647740B2 (en) * | 1984-12-03 | 1994-06-22 | 東レ株式会社 | Method for producing surface metallized thermoplastic polyester resin molded article |
| JPH0639713B2 (en) * | 1985-05-02 | 1994-05-25 | 東レ株式会社 | Method for producing surface metallized thermoplastic polyester resin molded article |
| JPH03202477A (en) * | 1989-12-28 | 1991-09-04 | Mitsubishi Rayon Co Ltd | Plated article |
| FR2823214B1 (en) * | 2001-04-09 | 2007-05-11 | Jean Claude Portner | PRE-TREATMENT OF PLASTIC MATERIAL |
| FR2957715B1 (en) * | 2010-03-18 | 2012-04-20 | Centre Nat Rech Scient | METHOD OF FORMING A PATTERN ON A SURFACE OF A SUPPORT |
| CN103483614A (en) * | 2013-09-26 | 2014-01-01 | 张家港市锦丰润尔发五金塑料厂 | Plastic surface treatment method |
-
1982
- 1982-03-03 JP JP3328782A patent/JPS58149924A/en active Granted
Also Published As
| Publication number | Publication date |
|---|---|
| JPS58149924A (en) | 1983-09-06 |
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