JP2658701B2 - Metal surface treatment method - Google Patents
Metal surface treatment methodInfo
- Publication number
- JP2658701B2 JP2658701B2 JP34370791A JP34370791A JP2658701B2 JP 2658701 B2 JP2658701 B2 JP 2658701B2 JP 34370791 A JP34370791 A JP 34370791A JP 34370791 A JP34370791 A JP 34370791A JP 2658701 B2 JP2658701 B2 JP 2658701B2
- Authority
- JP
- Japan
- Prior art keywords
- metal
- copper foil
- foil
- resin
- copper
- 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 - Fee Related
Links
Classifications
-
- 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
- C23C2222/00—Aspects relating to chemical surface treatment of metallic material by reaction of the surface with a reactive medium
- C23C2222/20—Use of solutions containing silanes
-
- H—ELECTRICITY
- H05—ELECTRIC TECHNIQUES NOT OTHERWISE PROVIDED FOR
- H05K—PRINTED CIRCUITS; CASINGS OR CONSTRUCTIONAL DETAILS OF ELECTRIC APPARATUS; MANUFACTURE OF ASSEMBLAGES OF ELECTRICAL COMPONENTS
- H05K3/00—Apparatus or processes for manufacturing printed circuits
- H05K3/38—Improvement of the adhesion between the insulating substrate and the metal
- H05K3/382—Improvement of the adhesion between the insulating substrate and the metal by special treatment of the metal
Landscapes
- Chemical Treatment Of Metals (AREA)
Description
【０００１】[0001]
【産業上の利用分野】本発明は金属、特にプリント配線
板用金属はく表面の接着性を向上させる方法に関する。BACKGROUND OF THE INVENTION 1. Field of the Invention The present invention relates to a method for improving the adhesion of a metal, particularly a metal foil surface for a printed wiring board.
【０００２】[0002]
【従来の技術】プリント配線板用金属はく張り積層板
は、基材と樹脂からなる絶縁基材層に金属はくを接着し
たものである。基材としては、紙、ガラス繊維布、有機
繊維布などが用いられ、樹脂としては、フェノール、エ
ポキシ、ポリイミド、ポリエステルなどが用いられてい
る。金属はくとしてはほとんどの場合銅はくを用いる。
稀にニッケルはく、ステンレスはく、タングステンはく
を用いることもある。金属はくと絶縁基材層との接着を
保つために、粗化された面を絶縁基材層と接着される面
とし、この面をカップリング剤で処理している。さら
に、フェノール樹脂のような接着力の弱い樹脂を絶縁基
材層に用いる場合には接着剤を塗布している。2. Description of the Related Art A metal-clad laminate for a printed wiring board is obtained by bonding a metal foil to an insulating base material layer composed of a base material and a resin. Paper, glass fiber cloth, organic fiber cloth, or the like is used as the base material, and phenol, epoxy, polyimide, polyester, or the like is used as the resin. In most cases, copper foil is used as the metal foil.
Rarely, nickel foil, stainless steel foil, or tungsten foil may be used. In order to maintain the adhesion between the metal foil and the insulating substrate layer, the roughened surface is used as a surface to be bonded to the insulating substrate layer, and this surface is treated with a coupling agent. Further, when a resin having a low adhesive strength such as a phenol resin is used for the insulating base material layer, an adhesive is applied.
【０００３】フレキシブル配線板は、絶縁基材層とし
て、ポリイミドフィルム、ポリエステルフィルムなどを
ベースフィルムとした金属はく張り板であり、この場合
も金属はくの接着について同様な処理が施されている。A flexible wiring board is a metal-clad board using a polyimide film, a polyester film, or the like as a base film as an insulating base material layer. In this case, a similar treatment is applied to the adhesion of the metal foil. .
【０００４】[0004]
【発明が解決しようとする課題】近年プリント配線板の
高密度化に伴い、形成される回路の幅が細くなってきて
いる。そのため、エッチング精度もよくなければならな
い。ところが、金属はくの粗化度が大であると、絶縁基
材層に食い込んだ金属はくをエッチングによって除去す
るため強いエッチングをすることとなり、垂直方向のエ
ッチングのほか水平方向にもエッチングが進行し（サイ
ドエッチングという）、エッチング精度が悪くなる。ま
た粗化度が小さいとサイドエッチングによるエッチング
精度の低下はなくなるが、接着強度が低下する。そこ
で、金属はくの粗化度が小さくても、なお絶縁基材層と
の接着強度の良い接着方法が望まれていた。本発明は、
このような事情に鑑みてなされたもので、金属はく表面
の接着性を高める方法を提供することを目的とするもの
である。In recent years, as the density of printed wiring boards has increased, the width of circuits formed has been reduced. Therefore, the etching accuracy must be good. However, if the degree of roughness of the metal foil is large, the metal foil that has penetrated the insulating base layer is removed by etching, so that strong etching is performed. The etching proceeds (called side etching), and the etching accuracy deteriorates. When the degree of roughness is small, the etching accuracy is not reduced by the side etching, but the bonding strength is reduced. Therefore, there has been a demand for a bonding method having a good bonding strength to the insulating base material layer even though the metal foil has a low degree of roughness. The present invention
The present invention has been made in view of such circumstances, and has as its object to provide a method for improving the adhesion of a metal foil surface.
【０００５】[0005]
【課題を解決するための手段】本発明は、金属はくの表
面にカップリング剤を付着させた後、紫外線を照射する
ことを特徴とする。The present invention is characterized in that a coupling agent is attached to the surface of a metal foil and then irradiated with ultraviolet light.
【０００６】金属はくとしては銅、アルミニウム、鉄、
ニッケル、亜鉛などの単体又は合金のはくがあり、必要
に応じて防錆のためにクロム、モリブデンなどの金属で
表面処理がほどこされたものでもよい。これらの金属は
くについては電解法、圧延法など、公知の技術によって
製造されたものを使用することができる。[0006] Metal foils include copper, aluminum, iron,
There is a simple substance such as nickel, zinc or the like, or an alloy, and if necessary, a surface treatment with a metal such as chromium or molybdenum for rust prevention may be used. As these metal foils, those manufactured by a known technique such as an electrolytic method and a rolling method can be used.
【０００７】カップリング剤としては従来公知のカップ
リング剤が適宜使用できる。主なものとしては、ビニル
トリクロロシラン、ビニルトリス（２−メトキシ）シラ
ン、γ−グリドキシプロピルトリメトキシシラン、γ−
メタクリロキシプロピルトリメトキシシラン、γ−アミ
ノプロピルトリメトキシシラン、γ−アミノプロピルト
リエトキシシラン、γ−（２−アミノエチル）アミノプ
ロピルトリメトキシシラン、Ｎ−β−（Ｎ−ビニルベン
ジルアミノエチル）−γ−アミノプロピルトリメトキシ
シラン、γ−クロロプロピルトリメトキシシラン、ビニ
ルトリエトキシシラン、β−（３，４エポキシシクロヘ
キシル）エチルトリメトキシシランなどのシラン系カッ
プリング剤、アセトアルコキシアルミニウムジイソプロ
ピレートなどのアルミニウム系カップリング剤などがあ
る。このほかチタネート系カップリング剤も使用可能で
ある。これらは接着される樹脂との反応性を考慮して適
宜選定される。カップリング剤は濃度０．０１〜５重量
％の溶液として使用される。溶媒としては水、アルコー
ル類、ケトン類、グリコールエーテル類を単独で又は混
合して使用する。As the coupling agent, conventionally known coupling agents can be appropriately used. The main ones are vinyltrichlorosilane, vinyltris (2-methoxy) silane, γ-glycoxypropyltrimethoxysilane, γ-
Methacryloxypropyltrimethoxysilane, γ-aminopropyltrimethoxysilane, γ-aminopropyltriethoxysilane, γ- (2-aminoethyl) aminopropyltrimethoxysilane, N-β- (N-vinylbenzylaminoethyl)- silane coupling agents such as γ-aminopropyltrimethoxysilane, γ-chloropropyltrimethoxysilane, vinyltriethoxysilane, β- (3,4 epoxycyclohexyl) ethyltrimethoxysilane, acetoalkoxyaluminum diisopropylate, etc. Aluminum-based coupling agents and the like. In addition, titanate-based coupling agents can be used. These are appropriately selected in consideration of the reactivity with the resin to be bonded. The coupling agent is used as a solution having a concentration of 0.01 to 5% by weight. As the solvent, water, alcohols, ketones, and glycol ethers are used alone or as a mixture.
【０００８】カップリング剤を金属はく表面に付着させ
た後、紫外線を照射する。紫外線の光源に制限はなく、
低圧水銀灯、中圧水銀灯、高圧水銀灯が使用できる。ま
た波長も２００〜４００ｎｍの範囲であればよい。紫外
線の照射量は、２００ｍＪ／ｃｍ2〜２５００ｍＪ／ｃ
ｍ2が適当である。２００ｍＪ／ｃｍ2より少ないと効果
が小さく、２５００ｍＪ／ｃｍ2以上の照射をしても効
果が飽和して変わらない。照射時間は５分以下が望まし
い。少ない光量で長時間処理するのは効果が少なく好ま
しくない。紫外線照射の効果は室温空気中保管で、照射
後、少なくとも１カ月以上持続する。紫外線の照射は、
金属はくを製造する際の製はく、カップリング剤処理と
一連に実施しても、また、全く別個でも何れでもよい。
また、プリント配線板材料を製造する際にその工程の中
に紫外線照射工程を組み込んでもよく、特に不飽和ポリ
エステル樹脂、ビニルエステル樹脂などを用いる樹脂含
浸、積層、硬化を一連に行う連続製造方法においてはそ
の方が効率よく製造できる。After attaching the coupling agent to the surface of the metal foil, it is irradiated with ultraviolet light. There is no limitation on the source of ultraviolet light,
Low-pressure, medium-pressure, and high-pressure mercury lamps can be used. The wavelength may be in the range of 200 to 400 nm. The irradiation amount of ultraviolet rays is 200 mJ / cm 2 to 2500 mJ / c.
m 2 is appropriate. If it is less than 200 mJ / cm 2 , the effect is small, and even if irradiation is performed at 2500 mJ / cm 2 or more, the effect is saturated and does not change. The irradiation time is desirably 5 minutes or less. It is not preferable to perform processing for a long time with a small amount of light because the effect is small. The effect of UV irradiation is stored in air at room temperature and lasts for at least one month after irradiation. UV irradiation
It may be carried out in series with the production of the metal foil and the treatment with the coupling agent, or may be carried out completely separately.
In addition, when manufacturing a printed wiring board material, an ultraviolet irradiation step may be incorporated in the process, particularly in a continuous manufacturing method in which resin impregnation using an unsaturated polyester resin, vinyl ester resin, and the like, lamination, and curing are performed in series. Can be manufactured more efficiently.
【０００９】プリント配線板材料としては、フェノール
樹脂、エポキシ樹脂、ポリエステル樹脂、ビニルエステ
ル樹脂、メラミン樹脂、ポリブタジエン樹脂、ポリイミ
ド樹脂、ポリエチレン樹脂、ポリブチレンテレフタレー
ト樹脂、ポリフェニレンオキシド樹脂、ポリエーテルイ
ミド樹脂、ポリアミドイミド樹脂など単独、変性又は複
合した樹脂組成物を使用して紙基材、有機繊維基材、無
機繊維基材などに含浸して得られたプリプレグを使用し
て金属はくと一体化された金属はく積層板あるいは樹脂
単独を板状、フィルム状として一体化した金属はく付き
フィルム、あるいは金属ベース基板など従来公知のもの
全般があげられる。Printed wiring board materials include phenolic resins, epoxy resins, polyester resins, vinyl ester resins, melamine resins, polybutadiene resins, polyimide resins, polyethylene resins, polybutylene terephthalate resins, polyphenylene oxide resins, polyetherimide resins, and polyamides. Independently such as imide resin, integrated with metal foil using prepreg obtained by impregnating paper base, organic fiber base, inorganic fiber base, etc. using a modified or composite resin composition Conventionally known general products such as a metal-laminated film, a metal-laminated film in which a resin alone is integrated into a plate shape or a film shape, or a metal base substrate are exemplified.
【００１０】[0010]
【作用】紫外線を照射することにより、金属はく表面上
に存在するカップリング剤の有機官能基が活性化され、
樹脂との反応が促進され、密着性が向上するものと考え
られる。The organic functional group of the coupling agent present on the surface of the metal foil is activated by irradiating ultraviolet rays,
It is considered that the reaction with the resin is promoted, and the adhesion is improved.
【００１１】[0011]
実施例１ 厚み１８μｍ、粗化面の表面粗さ１．３μｍ（Ｒａ）の
電解銅はくに、γ−グリシドキシプロピルトリメトキシ
シランを付着させた。次に８０Ｗの高圧水銀灯３本の下
を４ｍ／分で通過させ銅はく１を得た。累積照射量は、
１２００ｍＪ／ｃｍ2 であった。Example 1 γ-glycidoxypropyltrimethoxysilane was attached to electrolytic copper foil having a thickness of 18 μm and a roughened surface having a surface roughness of 1.3 μm (Ra). Next, the copper foil was passed under three 80 W high-pressure mercury lamps at 4 m / min to obtain copper foil 1. The cumulative dose is
It was 1200 mJ / cm 2 .
【００１２】エポキシ樹脂１００部（重量部、以下同
じ）、ジシアンジアミド４部、ベンジルジメチルアミン
０．２部、メチルセルソルブ５０部からなるエポキシ樹
脂ワニスを厚み０．２ｍｍのガラス布に含浸、乾燥して
プリプレグとした。得られたプリプレグを８枚積層し、
その両側に前記銅はく１を配置して温度１７０℃、圧力
６ＭＰＡで７０分間、加熱加圧し、厚み１．６ｍｍの銅
張積層板を得た。この積層板の銅はくのピール強度は、
１．６ｋＮ／ｍであった。なおピール強度の測定は、Ｊ
ＩＳＣ６４８１に準拠した（以下の各実施例及び比較例
においても同じである）。A glass cloth having a thickness of 0.2 mm is impregnated with an epoxy resin varnish consisting of 100 parts (parts by weight, hereinafter the same), 4 parts of dicyandiamide, 0.2 parts of benzyldimethylamine and 50 parts of methylcellosolve, and dried. Prepreg. Eight prepregs obtained are laminated,
The copper foil 1 was placed on both sides and heated and pressed at a temperature of 170 ° C. and a pressure of 6 MPa for 70 minutes to obtain a copper-clad laminate having a thickness of 1.6 mm. The peel strength of the copper foil of this laminate is
It was 1.6 kN / m. The peel strength was measured by J
It complies with ISC6481 (the same applies to the following examples and comparative examples).
【００１３】比較例１ 紫外線を照射しない銅はくを用いたほかは実施例１と同
様にして厚み１．６ｍｍの銅張積層板を得た。この積層
板の銅はくのピール強度は、１．３ｋＮ／ｍであった。Comparative Example 1 A copper-clad laminate having a thickness of 1.6 mm was obtained in the same manner as in Example 1 except that a copper foil not irradiated with ultraviolet rays was used. The peel strength of the copper foil of this laminate was 1.3 kN / m.
【００１４】実施例２ 厚み１８μｍ（Ｒａ）の電解銅はくにγ−（２−アミノ
エチル）アミノプロピルトリメトキシシランを粗化面に
付着させた。次に８０Ｗの高圧水銀灯３本の下を３．７
ｍ／分で通過させ銅はく２を得た。累積照射量は１５０
０ｍＪ／ｃｍ2であった。Example 2 An electrolytic copper foil having a thickness of 18 μm (Ra), particularly γ- (2-aminoethyl) aminopropyltrimethoxysilane, was adhered to a roughened surface. Next, 3.7 under three 80W high-pressure mercury lamps.
It was passed at m / min to obtain copper foil 2. Cumulative irradiation dose is 150
It was 0 mJ / cm 2 .
【００１５】Ｎ，Ｎ’−４，４’ジフェニルメタンビス
マレイミドとジアミンとを原料とするアミノビスマレイ
ミド樹脂（ローヌプーラン社製、ケルイミド６０１）を
加熱しながらＮ−メチル−２−ピロリドンに溶解して６
０重量％の溶液とした。この溶液１００部に、ジメチル
ホルムアミド１０部に溶解したＮ−トリブロムフェニル
モノマレイミド６部を加えた。この樹脂組成物を、厚み
０．２ｍｍのガラスクロスに含浸、乾燥して溶剤を除
き、プリプレグとした。このプリプレグ８枚を積層し、
その両側に前記銅はく２を配置して温度２００℃、圧力
６ＭＰａで３時間加熱加圧し、厚み１．６ｍｍの銅張積
層板を得た。この積層板の銅はくのピール強度は、１．
４ｋＮ／ｍであった。An aminobismaleimide resin (Kerimide 601 manufactured by Rhone Poulin Co., Ltd.) made from N, N'-4,4'diphenylmethanebismaleimide and diamine is dissolved in N-methyl-2-pyrrolidone while heating. 6
A 0% by weight solution was obtained. To 100 parts of this solution was added 6 parts of N-tribromophenylmonomaleimide dissolved in 10 parts of dimethylformamide. This resin composition was impregnated into a glass cloth having a thickness of 0.2 mm and dried to remove the solvent, thereby obtaining a prepreg. 8 prepregs are laminated,
The copper foil 2 was placed on both sides and heated and pressed at a temperature of 200 ° C. and a pressure of 6 MPa for 3 hours to obtain a copper-clad laminate having a thickness of 1.6 mm. The peel strength of the copper foil of this laminate was 1.
It was 4 kN / m.
【００１６】比較例２ 紫外線を照射しない銅はくを用いたほかは実施例２と同
様にして銅張積層板を得た。この積層板の銅はくのピー
ル強度は、１．１ｋＮ／ｍであった。Comparative Example 2 A copper-clad laminate was obtained in the same manner as in Example 2 except that a copper foil not irradiated with ultraviolet rays was used. The peel strength of the copper foil of this laminate was 1.1 kN / m.
【００１７】実施例３ 厚み１８μｍ、粗化面の表面粗さを１．３μｍ（Ｒａ）
の電解銅はくにγ−メタクリロキシプロピルトリメトキ
シシランを付着させ、次に８０Ｗの高圧水銀灯３本の下
を４ｍ／分で通過させ銅はく３を得た。累積照射量は１
２００ｍＪ／ｃｍ2 であった。Example 3 A thickness of 18 μm and a roughened surface having a surface roughness of 1.3 μm (Ra)
Γ-methacryloxypropyltrimethoxysilane was adhered to the electrolytic copper foil, and then passed under three 80 W high-pressure mercury lamps at 4 m / min to obtain copper foil 3. The cumulative dose is 1
It was 200 mJ / cm 2 .
【００１８】次にビニルエステル樹脂１００部にクメン
ハイドロパーオキサイド１部を添加し樹脂組成物を厚み
０．２ｍｍのガラス布基材に含浸し、これをそのまま７
枚積層し、その両面に前記銅はく３を配置し１１０℃で
２０分さらに１６０℃で３０分加熱し厚み１．６ｍｍの
両面銅張積層板を得た。この積層板の銅はくのピール強
度は、１．５ｋＮ／ｍであった。Next, 1 part of cumene hydroperoxide was added to 100 parts of the vinyl ester resin, and the resin composition was impregnated into a glass cloth substrate having a thickness of 0.2 mm.
The copper foil 3 was placed on both sides of the laminate, and heated at 110 ° C. for 20 minutes and at 160 ° C. for 30 minutes to obtain a 1.6 mm-thick double-sided copper-clad laminate. The peel strength of the copper foil of this laminate was 1.5 kN / m.
【００１９】比較例３ 紫外線を照射しない銅はくを用いたほか、実施例３と同
様にして銅張積層板を得た。この積層板の銅はくのピー
ル強度は、１．１ｋＮ／ｍであった。Comparative Example 3 A copper-clad laminate was obtained in the same manner as in Example 3 except that a copper foil not irradiated with ultraviolet rays was used. The peel strength of the copper foil of this laminate was 1.1 kN / m.
【００２０】比較例４ 紫外線を照射しない表面粗さ１．５μｍ（Ｒａ）の銅は
くを用いたほか実施例３と同様にして銅張積層板を得
た。この積層板の銅はくのピール強度は、１．３ｋＮ／
ｍであった。Comparative Example 4 A copper-clad laminate was obtained in the same manner as in Example 3 except that a copper foil not irradiated with ultraviolet rays and having a surface roughness of 1.5 μm (Ra) was used. The peel strength of the copper foil of this laminate was 1.3 kN /
m.
【００２１】[0021]
【発明の効果】本発明によれば、金属はくにカップリン
グ剤を付着し、その後紫外線を照射することにより、金
属はくと樹脂との接着強度を高めることができる。以上
金属はくの場合について説明したが、本発明は金属板と
樹脂との接着、多層プリント配線板の内層回路板と接着
用プリプレグとの接着にも応用できる。According to the present invention, the bonding strength between the metal foil and the resin can be increased by adhering the coupling agent to the metal foil and then irradiating it with ultraviolet rays. Although the case of metal foil has been described above, the present invention can also be applied to bonding between a metal plate and a resin, and bonding between an inner layer circuit board of a multilayer printed wiring board and a bonding prepreg.
Claims (2)
た後、紫外線を照射することを特徴とする金属表面の処
理方法。1. A method for treating a metal surface, comprising applying a coupling agent to the surface of the metal and irradiating the surface with ultraviolet light.
ことを特徴とする金属表面の処理方法。2. A method for treating a metal surface, wherein the metal is metal foil for a printed wiring board.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| JP34370791A JP2658701B2 (en) | 1991-12-26 | 1991-12-26 | Metal surface treatment method |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| JP34370791A JP2658701B2 (en) | 1991-12-26 | 1991-12-26 | Metal surface treatment method |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| JPH05171458A JPH05171458A (en) | 1993-07-09 |
| JP2658701B2 true JP2658701B2 (en) | 1997-09-30 |
Family
ID=18363630
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| JP34370791A Expired - Fee Related JP2658701B2 (en) | 1991-12-26 | 1991-12-26 | Metal surface treatment method |
Country Status (1)
| Country | Link |
|---|---|
| JP (1) | JP2658701B2 (en) |
Families Citing this family (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| KR100442563B1 (en) * | 2001-10-23 | 2004-07-30 | 엘지전선 주식회사 | Surface treatment of copper foil with silane coupling agent |
| JP2006245303A (en) * | 2005-03-03 | 2006-09-14 | Nikko Kinzoku Kk | Surface treatment method of copper foil |
| JP5429375B2 (en) * | 2011-04-15 | 2014-02-26 | 東洋紡株式会社 | LAMINATE, MANUFACTURING METHOD THEREOF, AND METHOD FOR CREATING DEVICE STRUCTURE USING THIS LAMINATE |
-
1991
- 1991-12-26 JP JP34370791A patent/JP2658701B2/en not_active Expired - Fee Related
Also Published As
| Publication number | Publication date |
|---|---|
| JPH05171458A (en) | 1993-07-09 |
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