JP2007314855A - Ultra-thin copper foil provided with carrier, copper-clad laminate and printed circuit board - Google Patents
Ultra-thin copper foil provided with carrier, copper-clad laminate and printed circuit board Download PDFInfo
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Abstract
Description
本発明はキャリア付き極薄銅箔並びに該キャリア付き極薄銅箔を用いた銅張積層板、プリント配線基板に関するもので、特に高密度極微細配線（ファインパターン）用途のプリント配線板、多層プリント配線板、チップオンフィルム用配線板に適したキャリア付き極薄銅箔に関するものである。 The present invention relates to an ultra-thin copper foil with a carrier, a copper-clad laminate using the ultra-thin copper foil with a carrier, and a printed wiring board, and in particular, a printed wiring board for use in high-density ultra-fine wiring (fine pattern), and multilayer printing. The present invention relates to an ultrathin copper foil with a carrier suitable for wiring boards and chip-on-film wiring boards.
通常、プリント配線板、多層プリント配線板、チップオンフィルム用配線板等の基礎となる銅張積層板、プリント配線基板に用いる銅箔は、樹脂基板等に熱圧着する側の表面を粗化面とし、この粗化面で該基板に対するアンカー効果を発揮させ、該基板と銅箔との接合強度を高めて銅張積層板、プリント配線基板としての信頼性を確保している。
さらに最近では、銅箔の粗化面をあらかじめエポキシ樹脂のような接着用樹脂で被覆し、該接着用樹脂を半硬化状態（Ｂステージ）の絶縁樹脂層にした樹脂付き銅箔を回路形成用の銅箔として用い、絶縁樹脂層の側を基板に熱圧着してプリント配線基板とし、該プリント配線基板を多層に積層してビルドアップ配線板を製造することが行われている。ビルドアップ配線基板とは、多層プリント配線板の一種で、絶縁基板上に１層ずつ絶縁層、導体パターンの順に形成し、レーザー法やフォト法により開口した穴（ビア）にめっきを施し、層間を導通させながら配線層を積み上げた配線板である。
Usually, copper-clad laminates that serve as the basis for printed wiring boards, multilayer printed wiring boards, chip-on-film wiring boards, and copper foils used for printed wiring boards are roughened on the surface that is thermocompression bonded to resin boards. In this roughened surface, the anchor effect on the substrate is exhibited, and the bonding strength between the substrate and the copper foil is increased to ensure the reliability as a copper-clad laminate and a printed wiring board.
More recently, a copper foil with resin, in which the roughened surface of the copper foil is previously coated with an adhesive resin such as an epoxy resin and the adhesive resin is used as an insulating resin layer in a semi-cured state (B stage), is used for circuit formation. As a copper foil, a printed wiring board is obtained by thermocompression bonding the insulating resin layer side to a substrate, and a build-up wiring board is manufactured by laminating the printed wiring board in multiple layers. A build-up wiring board is a type of multilayer printed wiring board, in which an insulating layer and a conductor pattern are formed in order on an insulating board in that order, and plating is performed on holes (vias) opened by the laser method or photo method. It is a wiring board which piled up wiring layers, making conduct.
この配線板は、各種電子部品の高度集積化に対応してビアが微細化できることから、配線パターンにも微細な線幅や線間ピッチの要求が高まってきており、例えば、半導体パッケージに使用されるプリント配線板の場合は、線幅や線間ピッチがそれぞれ３０μm前後という高密度極微細配線を有するプリント配線板の提供が要求されている。
このようなファインパターンプリント配線板用の銅箔として、厚い銅箔を用いると、エッチングによる配線回路形成時のエッチング時間が長くなり、その結果、形成される配線パターンの側壁の垂直性が崩れ、形成する配線パターンの配線線幅が狭い場合には断線に結びつくこともある。従って、ファインパターン用途に使われる銅箔としては、厚さ９μm以下の銅箔が要望され、現在では、厚さが５μｍ程度の銅箔が最も多く使用され、更に極薄銅箔化が求められている。
In this wiring board, vias can be miniaturized in response to high integration of various electronic components, and therefore, there is an increasing demand for fine line widths and line pitches in wiring patterns. For example, these wiring boards are used in semiconductor packages. In the case of a printed wiring board, it is required to provide a printed wiring board having high-density ultrafine wiring having a line width and a line pitch of about 30 μm.
As a copper foil for such a fine pattern printed wiring board, if a thick copper foil is used, the etching time at the time of wiring circuit formation by etching becomes long, and as a result, the verticality of the side wall of the formed wiring pattern is disrupted, When the wiring line width of the wiring pattern to be formed is narrow, it may lead to disconnection. Therefore, a copper foil having a thickness of 9 μm or less is demanded as a copper foil used for fine pattern applications. At present, a copper foil having a thickness of about 5 μm is most frequently used, and further ultrathin copper foil is required. ing.
しかし、このような薄い銅箔（以下、極薄銅箔ということがある）は機械的強度が弱く、プリント配線基板の製造時に皺や折れ目が発生しやすく、銅箔切れを起こすこともあるため、ファインパターン用途に使われる極薄銅箔としては、キャリアとしての金属箔（以下、キャリア箔という）の片面に剥離層を介して極薄銅箔層を直接電着させたキャリア付き極薄銅箔が使用されている。
上述したように、現在多用されている５μｍ厚さの銅箔はキャリア付き極薄銅箔として提供されている。
キャリア付き極薄銅箔は、キャリア箔の片面に、剥離層と電気銅めっきによる極薄銅箔がこの順序で形成されたものであり、該電気銅めっきからなる極薄銅箔の最外層表面が粗化面に仕上げられている。
キャリア箔の片面に形成する剥離層は、有機被膜、Ｃｒ金属、Ｃｒ合金、クロメートなどが常用されているが、近年ポリイミドなどの高温プラスチック等を絶縁基板とする配線基板においては、銅箔と基板とのプレス温度または硬化温度等の条件が高温のため、有機系の剥離層では剥がれなくなるため有機皮膜は使用できず、金属系の剥離層が用いられている。
However, such a thin copper foil (hereinafter, sometimes referred to as an ultrathin copper foil) has a low mechanical strength, easily causes wrinkles and creases during the production of a printed wiring board, and may cause the copper foil to break. Therefore, as an ultra-thin copper foil used for fine pattern applications, an ultra-thin copper with a carrier in which an ultra-thin copper foil layer is directly electrodeposited via a release layer on one side of a metal foil (hereinafter referred to as carrier foil) as a carrier. Copper foil is used.
As described above, the copper foil having a thickness of 5 μm that is widely used at present is provided as an ultrathin copper foil with a carrier.
The ultrathin copper foil with a carrier is formed by forming a peeling layer and an ultrathin copper foil by electrolytic copper plating in this order on one side of the carrier foil, and the outermost surface of the ultrathin copper foil made of the electrolytic copper plating Has a roughened surface.
For the release layer formed on one side of the carrier foil, organic coating, Cr metal, Cr alloy, chromate, etc. are commonly used. However, in recent years, in a wiring board using a high temperature plastic such as polyimide as an insulating substrate, a copper foil and a substrate are used. Since the conditions such as the pressing temperature or the curing temperature are high, the organic release layer cannot be peeled off and the organic coating cannot be used, and a metal release layer is used.
剥離層を形成する金属としては前記したようにＣｒ金属、Ｃｒ合金、クロメートが主流である。
また、Ｃｒ代替の新規剥離層として極薄銅箔の析出を容易にする金属種(Ｆｅ，Ｃｏ，Ｎｉ)と、極薄銅箔の剥離を容易にする金属種(Ｍｏ，Ｔａ，Ｖ，Ｗ)の合金を剥離層としたものも開発されている。
これらの剥離層により、高温での銅箔と基板とのプレス、または樹脂の硬化条件においても剥離可能なキャリア付き極薄銅箔が作製されている。
しかしながら、これらのめっきの比率・付着量等を制御することはかなりシビアな管理が要求されるのが現状である。
As described above, Cr metal, Cr alloy, and chromate are the mainstreams for forming the release layer.
In addition, as a new release layer for replacing Cr, metal species (Fe, Co, Ni) that facilitate the deposition of ultrathin copper foil and metal species (Mo, Ta, V, W) that facilitate the exfoliation of ultrathin copper foil ) Alloys with a release layer have been developed.
With these release layers, an ultrathin copper foil with a carrier that can be peeled even under a press condition between a copper foil and a substrate at a high temperature or under resin curing conditions is produced.
However, the present situation is that severe control is required to control the ratio and the amount of adhesion of these platings.
前述したように、Ｃｒによる剥離層やＣｒ代替の新規剥離層により、高耐熱性のキャリア付き極薄銅箔が作製されているが、この合金めっきを制御することはかなりシビアな管理が要求されるため、より簡単に作製可能なキャリア付き極薄銅箔の出現が望まれている。 As described above, ultra-thin copper foil with a high heat resistance carrier is produced by a release layer made of Cr or a new release layer that replaces Cr. However, controlling this alloy plating requires a fairly severe management. Therefore, the appearance of an ultrathin copper foil with a carrier that can be more easily produced is desired.
本発明は、かかる現状に鑑み、キャリア付き極薄銅箔の製造条件における管理範囲を広げ、それによる製造品質の安定化を図り、高温下の環境に置かれてもキャリア箔と極薄銅箔とを容易に剥がすことができるキャリア付き極薄銅箔を提供することを目的とする。
また本発明は、前記キャリア付き極薄銅箔を使用したファインパターン用途のプリント配線板、多層プリント配線板、チップオンフィルム用配線板等の基材となる銅張積層板、プリント配線基板を提供することを目的とする。
In view of the present situation, the present invention expands the management range in the manufacturing conditions of the ultrathin copper foil with a carrier, thereby stabilizing the manufacturing quality, and the carrier foil and the ultrathin copper foil even when placed in a high temperature environment It is an object to provide an ultrathin copper foil with a carrier that can be easily peeled off.
The present invention also provides a copper-clad laminate and a printed wiring board as a base material for printed wiring boards for fine patterns, multilayer printed wiring boards, chip-on-film wiring boards, etc., using the ultrathin copper foil with carrier. The purpose is to do.
本発明の第１のキャリア付き極薄銅箔は、キャリア箔、剥離層、極薄銅箔からなるキャリア付き極薄銅箔において、剥離層と極薄銅箔間において、元素Ｐの酸化物又は／及び水酸化物、又は／及び元素Ｐを含有する合金がその界面に介在することを特徴とするキャリア付き極薄銅箔である。 The first ultra-thin copper foil with a carrier of the present invention is an ultra-thin copper foil with a carrier comprising a carrier foil, a release layer, and an ultra-thin copper foil. An ultrathin copper foil with a carrier, characterized in that an alloy containing / and hydroxide or / and element P is present at the interface.
本発明の第２のキャリア付き極薄銅箔は、キャリア箔、拡散防止層、剥離層、極薄銅箔からなるキャリア付き極薄銅箔において、剥離層と極薄銅箔間において、元素Ｐの酸化物又は／及び水酸化物、又は／及び元素Ｐを含有する合金がその界面に介在することを特徴とするキャリア付き極薄銅箔である。 The ultrathin copper foil with a carrier of the second carrier of the present invention is an ultrathin copper foil with a carrier comprising a carrier foil, a diffusion preventing layer, a release layer, and an ultrathin copper foil, and the element P between the release layer and the ultrathin copper foil. An ultrathin copper foil with a carrier, characterized in that an oxide or / and hydroxide, or an alloy containing element P is interposed at the interface.
本発明の前記元素Ｐの付着量は、０．００１ｍｇ／ｄｍ２〜１ｍｇ／ｄｍ２であることが好ましい。 Adhesion amount of the element P of the present invention is preferably 0.001mg / dm 2 ~1mg / dm 2 .
本発明の銅張積層板は、前記キャリア付き極薄銅箔の極薄銅箔を樹脂基板に積層してなる高密度極微細配線用途の銅張積層板である。
本発明のプリント配線基板は、前記キャリア付き極薄銅箔の極薄銅箔を樹脂基板に積層してなる高密度極微細配線用途のプリント配線基板である。
The copper-clad laminate of the present invention is a copper-clad laminate for use in high-density ultrafine wiring obtained by laminating the ultrathin copper foil of the ultrathin copper foil with carrier on a resin substrate.
The printed wiring board of the present invention is a printed wiring board for use in high-density ultrafine wiring obtained by laminating an ultrathin copper foil of the ultrathin copper foil with a carrier on a resin substrate.
本発明は、キャリア付き極薄銅箔の製造条件おける管理範囲が広いため製造品質が安定し、高温下の環境に置かれてもキャリア箔と極薄銅箔とを容易に剥がすことができるキャリア付き極薄銅箔を提供することができる。
また本発明は、前記キャリア付き極薄銅箔を使用したファインパターン用途のプリント配線板、多層プリント配線板、チップオンフィルム用配線板等の基材となる銅張積層板、プリント配線基板を提供することができる。
The present invention provides a carrier that can easily peel off the carrier foil and the ultrathin copper foil even when placed in a high temperature environment because the production range is stable because the management range of the ultrathin copper foil with the carrier is wide. An ultra-thin copper foil can be provided.
The present invention also provides a copper-clad laminate and a printed wiring board as a base material for printed wiring boards for fine patterns, multilayer printed wiring boards, chip-on-film wiring boards, etc., using the ultrathin copper foil with carrier. can do.
キャリア付き極薄銅箔用の金属キャリア箔としては一般に、アルミニウム箔、アルミニウム合金箔、ステンレス鋼箔、チタン箔、チタン合金箔、銅箔、銅合金箔等が使用可能であるが、極薄銅箔または極薄銅合金箔（以下これらを区別する必要がないときは総称して極薄銅箔という）に使用するキャリア箔としてはその取扱いの簡便さの点から、電解銅箔、電解銅合金箔、圧延銅箔または圧延銅合金箔が好ましい。また、その厚みは７μｍ〜２００μｍの厚さの箔を使用することが好ましい。 Generally, aluminum foil, aluminum alloy foil, stainless steel foil, titanium foil, titanium alloy foil, copper foil, copper alloy foil, etc. can be used as the metal carrier foil for ultrathin copper foil with carrier. As a carrier foil used for foil or ultra-thin copper alloy foil (hereinafter collectively referred to as ultra-thin copper foil when it is not necessary to distinguish between these), electrolytic copper foil, electrolytic copper alloy from the viewpoint of easy handling A foil, rolled copper foil or rolled copper alloy foil is preferred. Moreover, it is preferable to use the foil whose thickness is 7 micrometers-200 micrometers.
キャリア箔として、厚さが７μｍ以下の薄い銅箔を採用すると、このキャリア箔の機械的強度が弱いためにプリント配線基板等の製造時に皺や折れ目が発生しやすく、箔切れを起こす危険性がある。またキャリア箔の厚さが２００μｍ以上になると単位コイル当たりの重量（コイル単重）が増すことで生産性に大きく影響するとともに設備上もより大きな張力を要求され、設備が大がかりとなって好ましくない。従って、キャリア箔の厚さとしては７μｍ〜２００μｍのものが好適である。 If a thin copper foil with a thickness of 7 μm or less is used as the carrier foil, the mechanical strength of the carrier foil is weak, so that wrinkles and creases are likely to occur during the production of printed wiring boards, etc. There is. Further, when the thickness of the carrier foil is 200 μm or more, the weight per unit coil (coil single weight) increases, which greatly affects the productivity and requires a higher tension on the equipment, which is not preferable because the equipment becomes large. . Therefore, the thickness of the carrier foil is preferably 7 μm to 200 μm.
キャリア箔としては、少なくとも片面の表面粗さがＲｚ：０．０１μｍ〜５．０μｍの金属箔を使用することが好ましく、特にチップオンフィルム用配線板における視認性などが要求される場合はＲｚ：０．０１μｍ〜２．０μｍであることが好ましい。そのため、チップオンフィルム配線基板用等視認性が要求される場合に表面粗さの範囲がＲｚ:２μｍ〜５．０μｍのキャリア箔を使用するときは、粗い表面に予め機械的研磨または電解研磨を施し、表面粗さをＲｚ：０．０１μｍ〜２μｍの範囲に平滑化して使用するとよい。なお、表面粗さＲｚ：５μｍ以上のキャリア箔についても予め機械的研磨・電気化学的溶解を施し、平滑化して使用することも可能である。 As the carrier foil, it is preferable to use a metal foil having a surface roughness of at least one surface of Rz: 0.01 μm to 5.0 μm, and particularly when visibility in a wiring board for chip-on-film is required. It is preferable that it is 0.01 micrometer-2.0 micrometers. Therefore, when using a carrier foil having a surface roughness range of Rz: 2 μm to 5.0 μm when visibility such as for a chip-on-film wiring board is required, mechanical polishing or electrolytic polishing is performed on the rough surface in advance. And the surface roughness is preferably smoothed to a range of Rz: 0.01 μm to 2 μm. Note that a carrier foil having a surface roughness Rz of 5 μm or more can be preliminarily mechanically polished and electrochemically dissolved and smoothed before use.
本発明において、キャリア箔上に設ける剥離層を形成する金属としては前記したようにＣｒ金属、Ｃｒ合金、クロメート皮膜又は／及びＣｒ代替の新規剥離層として極薄銅箔の析出を容易にする金属種(Ｆｅ，Ｃｏ，Ｎｉ)と極薄銅箔の剥離を容易にする金属種(Ｍｏ，Ｔａ，Ｖ，Ｗ)の合金を剥離層としたものであり、更に剥離層上にＰの酸化物又は／及び水酸化物、又は／及びＰを含有する合金で構成される。 In the present invention, as described above, the metal for forming the release layer provided on the carrier foil is a metal that facilitates the deposition of ultrathin copper foil as a new release layer of Cr metal, Cr alloy, chromate film or / and Cr as described above. An alloy of seeds (Fe, Co, Ni) and metal species (Mo, Ta, V, W) that facilitates peeling of the ultrathin copper foil is used as a peeling layer, and an oxide of P is further formed on the peeling layer. Alternatively, it is composed of an alloy containing hydroxide and / or P.
本発明において剥離層上に設ける元素Ｐの付着量をαとすると、
０．００１ｍｇ／ｄｍ２＜α＜１ｍｇ／ｄｍ２
とすることが好ましく、元素Ｐを剥離層上に介在させることにより、キャリア箔と極薄銅箔との剥離を容易にさせることが可能となる。
剥離層上にＰを設ける方法としては、Ｐを添加しためっき液で、剥離層上へ極薄いＰ含有銅めっき層を形成する。剥離層上のＰは、酸化物又は／及び水酸化物、又は／及びＰを含有する合金として形成する。Ｐの酸化物の例としてはＰ２Ｏ５等、Ｐ含有合金の例としてはＣｕ−Ｐ合金等が挙げられる。
In the present invention, when the adhesion amount of the element P provided on the release layer is α,
0.001 mg / dm 2 <α <1 mg / dm 2
It is preferable to interpose the element P on the release layer, and the carrier foil and the ultrathin copper foil can be easily peeled off.
As a method of providing P on the release layer, an extremely thin P-containing copper plating layer is formed on the release layer with a plating solution to which P is added. P on the release layer is formed as an oxide or / and hydroxide, or / and an alloy containing P. Examples of the P oxide include P 2 O 5 and the like, and examples of the P-containing alloy include a Cu—P alloy.
上記のような条件で剥離層及び剥離層上にＰを設けることで、目的とする効果は充分に達成されるが、剥離性に対する耐熱性をより安定させるために、キャリア箔と剥離層の間に拡散防止層を設けることで更に優れた効果が発揮される。拡散防止層はＮｉ又は／及びＣｏ、又は／及びその合金で形成することが好ましい。なお、ＣｒまたはＣｒ合金での形成も効果がある。 By providing P on the release layer and the release layer under the conditions as described above, the intended effect is sufficiently achieved, but in order to further stabilize the heat resistance against the release property, between the carrier foil and the release layer. A further excellent effect is exhibited by providing a diffusion preventing layer on the surface. The diffusion prevention layer is preferably formed of Ni or / and Co, or / and alloys thereof. In addition, formation with Cr or Cr alloy is also effective.
極薄銅箔の形成は、硫酸銅浴、ホウフッ化銅浴、スルファミン酸銅浴、ピロリン酸銅浴、シアン化銅浴などを使用し、剥離層上に電解めっきで形成する。なお、めっき浴は、ｐＨ１〜１２の間にある銅めっき浴を使用することが好ましい。
極薄銅箔の形成は、剥離層がめっき液に溶解し易い金属で形成されている場合には、めっき液中のディップ時間・電流値、めっき仕上げのめっき液切り・水洗、金属めっき直後のめっき液ｐＨなどが剥離層の残存状態を決定するため、浴種は剥離層表面との関係で選択する必要がある。
The ultrathin copper foil is formed by electrolytic plating on the release layer using a copper sulfate bath, a copper borofluoride bath, a copper sulfamate bath, a copper pyrophosphate bath, a copper cyanide bath, or the like. The plating bath is preferably a copper plating bath having a pH between 1 and 12.
Ultra-thin copper foil is formed when the release layer is made of a metal that is easily dissolved in the plating solution, dipping time / current value in the plating solution, cutting of the plating solution for plating finish, washing with water, immediately after metal plating. Since the plating solution pH determines the remaining state of the release layer, the bath type must be selected in relation to the release layer surface.
なお、極薄銅箔表面における絶縁基板とのより強い密着性を得るためには極薄銅箔表面に粗化処理を行い、表面の粗度をＲｚ：０．２〜３．０（μｍ）にするとよい。粗化処理は、粗さが０．２（μｍ）以下では、密着性にあまり影響を与えないため粗化を行っても意味がなく、粗さが３（μｍ）あれば、充分な密着性を得られることからそれ以上の粗化は必要としないためである。
最後に、粗化処理した表面上に防錆及び耐熱性に効果があるＮｉ、Ｚｎ、或いは場合によりＣｒを付着させる。またピール強度を向上させるためシランを塗布することも効果的である。
In order to obtain stronger adhesion to the insulating substrate on the surface of the ultrathin copper foil, the surface of the ultrathin copper foil is subjected to a roughening treatment, and the surface roughness is Rz: 0.2 to 3.0 (μm). It is good to. As for the roughening treatment, if the roughness is 0.2 (μm) or less, there is no effect on the adhesion, so it is meaningless to roughen. If the roughness is 3 (μm), sufficient adhesion is achieved. This is because no further roughening is required.
Finally, Ni, Zn, or, in some cases, Cr, which has an effect on rust prevention and heat resistance, is deposited on the roughened surface. It is also effective to apply silane in order to improve the peel strength.
以下、本発明を実施例により具体的に説明する。
各実施例のめっき条件は次のとおりである。
Hereinafter, the present invention will be specifically described by way of examples.
The plating conditions in each example are as follows.
（１）拡散防止層作製めっき条件
〈Ｎｉめっき〉
硫酸ニッケル（Ｎｉとして） ：１〜1２０ｇ／ｄｍ３
ホウ酸 ：１０〜５０ｇ／ｄｍ３
電流密度 ：１〜６０Ａ／ｄｍ２
通電時間 ：１〜１２０秒
浴温 ：１０〜７０℃
(1) Diffusion prevention layer fabrication plating conditions <Ni plating>
Nickel sulfate (as Ni): 1-120 g / dm 3
Boric acid: 10-50 g / dm 3
Current density: 1 to 60 A / dm 2
Energizing time: 1 to 120 seconds Bath temperature: 10 to 70 ° C
（２）剥離層作製めっき条件１
〈Ｃｒめっき〉
Ｃｒ量 ：１〜５００ｇ／ｄｍ３
硫酸 ：０．０１〜５ｇ／ｄｍ３
電流密度 ：１〜６０Ａ／ｄｍ２
通電時間 ：１〜１２０秒
浴温 ：１０℃〜６０℃
(2) Release layer preparation plating condition 1
<Cr plating>
Cr amount: 1 to 500 g / dm 3
Sulfuric acid: 0.01-5 g / dm 3
Current density: 1 to 60 A / dm 2
Energizing time: 1 to 120 seconds Bath temperature: 10 ° C to 60 ° C
（２）剥離層作製めっき条件２
〈Ｍｏ−Ｃｏめっき〉
Ｃｏ量 ：０．１〜２０ｇ／ｄｍ３
Ｍｏ量 ：０．０５〜２０ｇ／ｄｍ３
クエン酸 ：５〜２４０ｇ／ｄｍ３
電流密度 ：０．１〜６０Ａ／ｄｍ２
通電時間 ：１〜３００秒
浴温 ：１０℃〜７０℃
(2) Peeling layer preparation plating condition 2
<Mo-Co plating>
Co amount: 0.1 to 20 g / dm 3
Mo amount: 0.05 to 20 g / dm 3
Citric acid: 5-240 g / dm 3
Current density: 0.1 to 60 A / dm 2
Energizing time: 1 to 300 seconds Bath temperature: 10 ° C to 70 ° C
（３）剥離層作製めっき条件３
〈Ｍｏ−Ｎｉめっき〉
硫酸Ｎｉ六水和物 ：１０〜１００ｇ／ｄｍ３
モリブデン酸ナトリウム二水和物 ：１０〜１００ｇ／ｄｍ３
クエン酸ナトリウム ：３０〜２００ｇ／ｄｍ３
浴温 ：１０〜５０℃
電流密度 ：０．５〜１５Ａ／ｄｍ２
(3) Peeling layer preparation plating condition 3
<Mo-Ni plating>
Ni sulfate hexahydrate: 10 to 100 g / dm 3
Sodium molybdate dihydrate: 10 to 100 g / dm 3
Sodium citrate: 30 to 200 g / dm 3
Bath temperature: 10-50 ° C
Current density: 0.5 to 15 A / dm 2
（４）剥離層作製めっき条件４
〈Ｗ−Ｎｉめっき〉
硫酸Ｎｉ六水和物 ：１０〜１００ｇ／ｄｍ３
タングステン酸ナトリウム二水和物 ：１０〜１００ｇ／ｄｍ３
クエン酸ナトリウム ：３０〜２００ｇ／ｄｍ３
浴温 ：３０〜９０℃
電流密度 ：０．５〜１５Ａ／ｄｍ２
(4) Release layer preparation plating condition 4
<W-Ni plating>
Ni sulfate hexahydrate: 10 to 100 g / dm 3
Sodium tungstate dihydrate: 10 to 100 g / dm 3
Sodium citrate: 30 to 200 g / dm 3
Bath temperature: 30-90 ° C
Current density: 0.5 to 15 A / dm 2
（５）剥離層作製めっき条件５
〈Ｗ−Ｃｏめっき〉
Ｃｏ量 ：０．１〜２０ｇ／ｄｍ３
タングステン酸ナトリウム二水和物 ：１０〜１００ｇ／ｄｍ３
クエン酸ナトリウム ：３０〜２００ｇ／ｄｍ３
浴温 ：３０〜９０℃
電流密度 ：０．５〜１５Ａ／ｄｍ２
(5) Peeling layer preparation plating condition 5
<W-Co plating>
Co amount: 0.1 to 20 g / dm 3
Sodium tungstate dihydrate: 10 to 100 g / dm 3
Sodium citrate: 30 to 200 g / dm 3
Bath temperature: 30-90 ° C
Current density: 0.5 to 15 A / dm 2
（６）極薄銅箔作製めっき条件１
〈硫酸銅めっき〉
硫酸銅（Ｃｕ金属として） ：１０〜７０ｇ／ｄｍ３
硫酸 ：３０〜１２０ｇ／ｄｍ３
電流密度 ：１〜６０Ａ／ｄｍ２
浴温 ：１０〜７０℃
(6) Ultra-thin copper foil production plating condition 1
<Copper sulfate plating>
Copper sulfate (as Cu metal): 10-70 g / dm 3
Sulfuric acid: 30-120 g / dm 3
Current density: 1 to 60 A / dm 2
Bath temperature: 10-70 ° C
（７）Ｐ含有極薄銅層作製めっき条件１
〈ピロリン酸銅めっき１〉
Ｃｕ２Ｐ２Ｏ７・３Ｈ２Ｏ ：１０〜1５０ｇ／ｌ
Ｋ４Ｐ２Ｏ７ ：５０〜４００ｇ／ｌ
ＮａＰＨ２Ｏ２ ：１〜１６０ｇ／ｌ
ＮＨ３ＯＨ（２８％） ：１〜１０ｍｌ／ｌ
ｐＨ ：８〜１２
電流密度 ：０.１〜５Ａ／ｄｍ２
浴温 ：２０〜６０℃
(7) P-containing ultrathin copper layer production plating condition 1
<Copper pyrophosphate plating 1>
Cu 2 P 2 O 7 · 3H 2 O: 10~150g / l
K 4 P 2 O 7: 50~400g / l
NaPH 2 O 2 : 1 to 160 g / l
NH 3 OH (28%): 1-10 ml / l
pH: 8-12
Current density: 0.1 to 5 A / dm 2
Bath temperature: 20-60 ° C
（８）Ｐ含有極薄銅層作製めっき条件２
〈ピロリン酸銅めっき２〉
Ｃｕ２Ｐ２Ｏ７・３Ｈ２Ｏ ：３〜５０ｇ／ｌ
Ｋ４Ｐ２Ｏ７ ：５０〜３５０ｇ／ｌ
ＮａＰＨ２Ｏ２ ：１〜１６０ｇ／ｌ
ｐＨ ：８〜１１
電流密度 ：０.１〜５Ａ／ｄｍ２
浴温 ：２０〜６０℃
(8) P-containing ultrathin copper layer production plating condition 2
<Copper pyrophosphate plating 2>
Cu 2 P 2 O 7 · 3H 2 O: 3~50g / l
K 4 P 2 O 7: 50~350g / l
NaPH 2 O 2 : 1 to 160 g / l
pH: 8-11
Current density: 0.1 to 5 A / dm 2
Bath temperature: 20-60 ° C
（９）Ｐ含有極薄銅層作製めっき条件３
〈硫酸銅めっき(Ｐ含有)〉
硫酸銅（Ｃｕ金属として） ：１０〜７０ｇ／ｄｍ３
硫酸 ：３０〜１２０ｇ／ｄｍ３
Ｎａ２ＨＰＯ４ ：1〜１５０ｇ／ｄｍ３
電流密度 ：１〜６０Ａ／ｄｍ２
浴温 ：１０〜７０℃
(9) P-containing ultrathin copper layer production plating condition 3
<Copper sulfate plating (containing P)>
Copper sulfate (as Cu metal): 10-70 g / dm 3
Sulfuric acid: 30-120 g / dm 3
Na 2 HPO 4 : 1 to 150 g / dm 3
Current density: 1 to 60 A / dm 2
Bath temperature: 10-70 ° C
＜実施例１＞
→拡散防止層作製めっき条件〈Ｎｉめっき〉
→剥離層作製めっき条件１〈Ｃｒめっき〉
→Ｐ含有極薄銅層作製めっき条件１〈ピロリン酸銅めっき１〉
→極薄銅箔めっき条件１〈硫酸銅めっき〉
によるめっきを順次行ったキャリア付き極薄銅箔の製造。
片面がＲｚ：０．８μｍの銅箔（厚さ：３１μｍ）をキャリア箔とし、該キャリア箔上に前記Ｎｉめっき条件下において拡散防止層を施した後、下記条件にてＣｒめっきにより剥離層を形成した。
Ｃｒ量 ：２５０ｇ／ｄｍ３
硫酸 ：２．５ｇ／ｄｍ３
電流密度 ：１０Ａ／ｄｍ２
通電時間 ：６０秒
浴温 ：５０℃
形成した剥離層の付着量は０．０１ｍｇ/ｄｍ２であった。
該剥離層上に前記Ｐ含有極薄銅層作製めっき条件１〈ピロリン酸銅めっき１〉で０．２μｍ厚さに銅めっきを施した。この層のＰ付着量は０．０１３ｍｇ／ｄｍ２であった。次いでその上に前記極薄銅箔めっき条件１〈硫酸銅めっき〉により電流密度４．５Ａ／ｄｍ２で３μｍ厚さの極薄銅箔を形成し、キャリア付き極薄銅箔とした。
更に、Ｎｉ：０．５ｍｇ/dm2、Ｚｎ：０．０５ｍｇ／ｄｍ２、Ｃｒ：０．３ｍｇ／ｄｍ２の表面処理後、シランカップリング剤処理（後処理）を行い、キャリア付き極薄銅箔を得た。
<Example 1>
→ Diffusion prevention layer plating conditions <Ni plating>
→ Peeling layer preparation plating condition 1 <Cr plating>
→ P-containing ultrathin copper layer preparation plating condition 1 <copper pyrophosphate copper plating 1>
→ Ultra-thin copper foil plating condition 1 <Copper sulfate plating>
Manufacturing of ultra-thin copper foil with carrier, which was sequentially plated by the above.
A copper foil (thickness: 31 μm) having a Rz of 0.8 μm on one side was used as a carrier foil, and a diffusion prevention layer was applied on the carrier foil under the Ni plating conditions, followed by Cr plating under the following conditions. Formed.
Cr amount: 250 g / dm 3
Sulfuric acid: 2.5 g / dm 3
Current density: 10 A / dm 2
Energizing time: 60 seconds Bath temperature: 50 ° C
The adhesion amount of the formed release layer was 0.01 mg / dm 2 .
The P-containing ultrathin copper layer production plating condition 1 <copper pyrophosphate plating 1> was subjected to copper plating to a thickness of 0.2 μm on the release layer. The P adhesion amount of this layer was 0.013 mg / dm 2 . Then, an ultrathin copper foil having a carrier density of 3 μm was formed at a current density of 4.5 A / dm 2 under the above ultrathin copper foil plating condition 1 (copper sulfate plating) to obtain an ultrathin copper foil with a carrier.
Furthermore, after surface treatment of Ni: 0.5 mg / dm 2 , Zn: 0.05 mg / dm 2 , Cr: 0.3 mg / dm 2 , silane coupling agent treatment (post treatment) was performed, and ultrathin copper with a carrier A foil was obtained.
＜実施例２＞
→拡散防止層作製めっき条件〈Ｎｉめっき〉
→剥離層作製めっき条件１〈Ｃｒめっき〉
→Ｐ含有極薄銅層作製めっき条件２〈ピロリン酸銅めっき２〉
→極薄銅箔めっき条件１〈硫酸銅めっき〉
によるめっきを順次行ったキャリア付き極薄銅箔の製造。
片面がＲｚ：０．８μｍの銅箔（厚さ：３１μｍ）をキャリア箔とし、該キャリア箔上に前記Ｎｉめっき条件下において拡散防止層を施した後、下記条件にてＣｒめっきにより剥離層を形成した。
Ｃｒ量 ：２５０ｇ／ｄｍ３
硫酸 ：２．５ｇ／ｄｍ３
電流密度 ：１０Ａ／ｄｍ２
通電時間 ：６０秒
浴温 ：５０℃
形成した剥離層の付着量は０．０１ｍｇ/ｄｍ２であった。
該剥離層上に前記Ｐ含有極薄銅層作製めっき条件２〈ピロリン酸銅めっき２〉で０．２μｍ厚さに銅めっきを施した。この層のＰ付着量は０．０１２ｍｇ／ｄｍ２であった。次いでその上に前記極薄銅箔めっき条件１〈硫酸銅めっき〉により電流密度４．５Ａ／ｄｍ２で３μｍ厚さの極薄銅箔を形成し、キャリア付き極薄銅箔とした。
更に、Ｎｉ：０．５ｍｇ/dm2、Ｚｎ：０．０５ｍｇ／ｄｍ２、Ｃｒ：０．３ｍｇ／ｄｍ２の表面処理後、シランカップリング剤処理（後処理）を行い、キャリア付き極薄銅箔を得た。
<Example 2>
→ Diffusion prevention layer plating conditions <Ni plating>
→ Peeling layer preparation plating condition 1 <Cr plating>
→ P-containing ultrathin copper layer preparation plating condition 2 <copper pyrophosphate copper plating 2>
→ Ultra-thin copper foil plating condition 1 <Copper sulfate plating>
Manufacturing of ultra-thin copper foil with carrier, which was sequentially plated by the above.
A copper foil (thickness: 31 μm) having a Rz of 0.8 μm on one side was used as a carrier foil, and a diffusion prevention layer was applied on the carrier foil under the Ni plating conditions, followed by Cr plating under the following conditions. Formed.
Cr amount: 250 g / dm 3
Sulfuric acid: 2.5 g / dm 3
Current density: 10 A / dm 2
Energizing time: 60 seconds Bath temperature: 50 ° C
The adhesion amount of the formed release layer was 0.01 mg / dm 2 .
On the release layer, copper plating was performed to a thickness of 0.2 μm under the P-containing ultrathin copper layer preparation plating condition 2 <copper pyrophosphate plating 2>. The P adhesion amount of this layer was 0.012 mg / dm 2 . Then, an ultrathin copper foil having a carrier density of 3 μm was formed at a current density of 4.5 A / dm 2 under the above ultrathin copper foil plating condition 1 (copper sulfate plating) to obtain an ultrathin copper foil with a carrier.
Furthermore, after surface treatment of Ni: 0.5 mg / dm 2 , Zn: 0.05 mg / dm 2 , Cr: 0.3 mg / dm 2 , silane coupling agent treatment (post treatment) was performed, and ultrathin copper with a carrier A foil was obtained.
＜実施例３＞
→拡散防止層作製めっき条件〈Ｎｉめっき〉
→剥離層作製めっき条件１〈Ｃｒめっき〉
→Ｐ含有極薄銅層作製めっき条件３〈硫酸銅めっき(Ｐ含有)〉
→極薄銅箔めっき条件１〈硫酸銅めっき〉
によるめっきを順次行ったキャリア付き極薄銅箔の製造。
片面がＲｚ：０．８μｍの銅箔（厚さ：３１μｍ）をキャリア箔とし、該キャリア箔上に前記Ｎｉめっき条件下において拡散防止層を施した後、下記条件にてＣｒめっきにより剥離層を形成した。
Ｃｒ量 ：２５０ｇ／ｄｍ３
硫酸 ：２．５ｇ／ｄｍ３
電流密度 ：１０Ａ／ｄｍ２
通電時間 ：６０秒
浴温 ：５０℃
形成した剥離層の付着量は０．０１ｍｇ/ｄｍ２であった。
該剥離層上にＰ含有極薄銅層作製めっき条件３〈硫酸銅めっき(Ｐ含有)〉で０．２μｍ厚さに銅めっきを施した。この層のＰ付着量は０．０１３ｍｇ／ｄｍ２であった。次いでその上に前記極薄銅箔めっき条件１〈硫酸銅めっき〉により電流密度４．５Ａ／ｄｍ２で３μｍ厚さの極薄銅箔を形成し、キャリア付き極薄銅箔とした。
更に、Ｎｉ：０．５ｍｇ/dm2、Ｚｎ：０．０５ｍｇ／ｄｍ２、Ｃｒ：０．３ｍｇ／ｄｍ２の表面処理後、シランカップリング剤処理（後処理）を行い、キャリア付き極薄銅箔を得た。
<Example 3>
→ Diffusion prevention layer plating conditions <Ni plating>
→ Peeling layer preparation plating condition 1 <Cr plating>
→ P-containing ultra-thin copper layer production plating condition 3 <copper sulfate plating (P-containing)>
→ Ultra-thin copper foil plating condition 1 <Copper sulfate plating>
Manufacturing of ultra-thin copper foil with carrier, which was sequentially plated by the above.
A copper foil (thickness: 31 μm) having a Rz of 0.8 μm on one side was used as a carrier foil, and a diffusion prevention layer was applied on the carrier foil under the Ni plating conditions, followed by Cr plating under the following conditions. Formed.
Cr amount: 250 g / dm 3
Sulfuric acid: 2.5 g / dm 3
Current density: 10 A / dm 2
Energizing time: 60 seconds Bath temperature: 50 ° C
The adhesion amount of the formed release layer was 0.01 mg / dm 2 .
Copper plating was performed on the release layer to a thickness of 0.2 μm under P-containing ultrathin copper layer production plating condition 3 <copper sulfate plating (P-containing)>. The P adhesion amount of this layer was 0.013 mg / dm 2 . Then, an ultrathin copper foil having a carrier density of 3 μm was formed at a current density of 4.5 A / dm 2 under the above ultrathin copper foil plating condition 1 (copper sulfate plating) to obtain an ultrathin copper foil with a carrier.
Furthermore, after surface treatment of Ni: 0.5 mg / dm 2 , Zn: 0.05 mg / dm 2 , Cr: 0.3 mg / dm 2 , silane coupling agent treatment (post treatment) was performed, and ultrathin copper with a carrier A foil was obtained.
＜実施例４＞
→拡散防止層作製めっき条件〈Ｎｉめっき〉
→剥離層作製めっき条件２〈Ｍｏ−Ｃｏめっき〉
→Ｐ含有極薄銅層作製めっき条件１〈ピロリン酸銅めっき１〉
→極薄銅箔めっき条件１〈硫酸銅めっき〉
によるめっきを順次行ったキャリア付き極薄銅箔の製造。
片面がＲｚ：０．８μｍの銅箔（厚さ：３１μｍ）をキャリア箔とし、該キャリア箔上に前記Ｎｉめっき条件下において拡散防止層を施した後、下記条件にてＭｏ−Ｃｏめっきにより剥離層を形成した。
Ｃｏ量 ：４．０ｇ／ｄｍ３
Ｍｏ量 ：２.０ｇ／ｄｍ３
クエン酸 ：８０ｇ／ｄｍ３
電流密度 ：２Ａ／ｄｍ２
通電時間 ：１５秒
浴温 ：５０℃
形成した剥離層の付着量は１．５ｍｇ/ｄｍ２であった。
該剥離層上にＰ含有極薄銅層作製めっき条件１〈ピロリン酸銅めっき１〉で０．２μｍ厚さに銅めっきを施した。この層のＰ付着量は０．０１５ｍｇ／ｄｍ２であった。次いでその上に前記極薄銅箔めっき条件１〈硫酸銅めっき〉により電流密度４．５Ａ／ｄｍ２で３μｍ厚さの極薄銅箔を形成し、キャリア付き極薄銅箔とした。
次いで、Ｎｉ：０．５ｍｇ/dm2、Ｚｎ：０．０５ｍｇ／ｄｍ２、Ｃｒ：０．３ｍｇ／ｄｍ２の表面処理後、シランカップリング剤処理（後処理）を行い、キャリア付き極薄銅箔を得た。
<Example 4>
→ Diffusion prevention layer plating conditions <Ni plating>
→ Peeling layer preparation plating condition 2 <Mo-Co plating>
→ P-containing ultrathin copper layer preparation plating condition 1 <copper pyrophosphate copper plating 1>
→ Ultra-thin copper foil plating condition 1 <Copper sulfate plating>
Manufacturing of ultra-thin copper foil with carrier, which was sequentially plated by the above.
A copper foil (thickness: 31 μm) with Rz: 0.8 μm on one side was used as a carrier foil, and a diffusion prevention layer was applied on the carrier foil under the Ni plating conditions, and then peeled off by Mo-Co plating under the following conditions: A layer was formed.
Co amount: 4.0 g / dm 3
Mo amount: 2.0 g / dm 3
Citric acid: 80 g / dm 3
Current density: 2 A / dm 2
Energizing time: 15 seconds Bath temperature: 50 ° C
The adhesion amount of the formed release layer was 1.5 mg / dm 2 .
On the release layer, copper plating was performed to a thickness of 0.2 μm under P-containing ultrathin copper layer production plating condition 1 <copper pyrophosphate plating 1>. The P adhesion amount of this layer was 0.015 mg / dm 2 . Then, an ultrathin copper foil having a carrier density of 3 μm was formed at a current density of 4.5 A / dm 2 under the above ultrathin copper foil plating condition 1 (copper sulfate plating) to obtain an ultrathin copper foil with a carrier.
Next, after surface treatment of Ni: 0.5 mg / dm 2 , Zn: 0.05 mg / dm 2 , Cr: 0.3 mg / dm 2 , silane coupling agent treatment (post treatment) is performed, and ultrathin copper with a carrier A foil was obtained.
＜実施例５＞
→拡散防止層作製めっき条件〈Ｎｉめっき〉
→剥離層作製めっき条件２〈Ｍｏ−Ｃｏめっき〉
→Ｐ含有極薄銅層作製めっき条件２〈ピロリン酸銅めっき２〉
→極薄銅箔めっき条件１〈硫酸銅めっき〉
によるめっきを順次行ったキャリア付き極薄銅箔の製造。
片面がＲｚ：０．８μｍの銅箔（厚さ：３１μｍ）をキャリア箔とし、該キャリア箔上に前記Ｎｉめっき条件下において拡散防止層を施した後、下記条件にてＭｏ−Ｃｏめっきにより剥離層を形成した。
Ｃｏ量 ：４．０ｇ／ｄｍ３
Ｍｏ量 ：２.０ｇ／ｄｍ３
クエン酸 ：８０ｇ／ｄｍ３
電流密度 ：２Ａ／ｄｍ２
通電時間 ：１５秒
浴温 ：５０℃
形成した剥離層の付着量は１．５ｍｇ/ｄｍ２であった。
該剥離層上にＰ含有極薄銅層作製めっき条件２〈ピロリン酸銅めっき２〉で０．２μｍ厚さに銅めっきを施した。この層のＰ付着量は０．０１４ｍｇ／ｄｍ２であった。次いでその上に前記極薄銅箔めっき条件１〈硫酸銅めっき〉により電流密度４．５Ａ／ｄｍ２で３μｍ厚さの極薄銅箔を形成し、キャリア付き極薄銅箔とした。
更に、Ｎｉ：０．５ｍｇ/dm2、Ｚｎ：０．０５ｍｇ／ｄｍ２、Ｃｒ：０．３ｍｇ／ｄｍ２の表面処理後、シランカップリング剤処理（後処理）を行い、キャリア付き極薄銅箔を得た。
<Example 5>
→ Diffusion prevention layer plating conditions <Ni plating>
→ Peeling layer preparation plating condition 2 <Mo-Co plating>
→ P-containing ultrathin copper layer preparation plating condition 2 <copper pyrophosphate copper plating 2>
→ Ultra-thin copper foil plating condition 1 <Copper sulfate plating>
Manufacturing of ultra-thin copper foil with carrier, which was sequentially plated by the above.
A copper foil (thickness: 31 μm) with Rz: 0.8 μm on one side was used as a carrier foil, and a diffusion prevention layer was applied on the carrier foil under the Ni plating conditions, and then peeled off by Mo-Co plating under the following conditions: A layer was formed.
Co amount: 4.0 g / dm 3
Mo amount: 2.0 g / dm 3
Citric acid: 80 g / dm 3
Current density: 2 A / dm 2
Energizing time: 15 seconds Bath temperature: 50 ° C
The adhesion amount of the formed release layer was 1.5 mg / dm 2 .
On the release layer, copper plating was applied to a thickness of 0.2 μm under P-containing ultrathin copper layer production plating condition 2 <copper pyrophosphate plating 2>. The P adhesion amount of this layer was 0.014 mg / dm 2 . Then, an ultrathin copper foil having a carrier density of 3 μm was formed at a current density of 4.5 A / dm 2 under the above ultrathin copper foil plating condition 1 (copper sulfate plating) to obtain an ultrathin copper foil with a carrier.
Furthermore, after surface treatment of Ni: 0.5 mg / dm 2 , Zn: 0.05 mg / dm 2 , Cr: 0.3 mg / dm 2 , silane coupling agent treatment (post treatment) was performed, and ultrathin copper with a carrier A foil was obtained.
＜実施例６＞
→拡散防止層作製めっき条件〈Ｎｉめっき〉
→剥離層作製めっき条件２〈Ｍｏ−Ｃｏめっき〉
→Ｐ含有極薄銅層作製めっき条件３〈硫酸銅めっき(Ｐ含有)〉
→極薄銅箔めっき条件１〈硫酸銅めっき〉
によるめっきを順次行ったキャリア付き極薄銅箔の製造。
片面がＲｚ：０．８μｍの銅箔（厚さ：３１μｍ）をキャリア箔とし、該キャリア箔上に前記Ｎｉめっき条件下において拡散防止層を施した後、下記条件にてＭｏ−Ｃｏめっきにより剥離層を形成した。
Ｃｏ量 ：４．０ｇ／ｄｍ３
Ｍｏ量 ：２.０ｇ／ｄｍ３
クエン酸 ：８０ｇ／ｄｍ３
電流密度 ：２Ａ／ｄｍ２
通電時間 ：１５秒
浴温 ：５０℃
形成した剥離層の付着量は１．５ｍｇ/ｄｍ２であった。
該剥離層上にＰ含有極薄銅層作製めっき条件３〈硫酸銅めっき(Ｐ含有)〉で０．２μｍ厚さに銅めっきを施した。この層のＰ付着量は０．０１４ｍｇ／ｄｍ２であった。次いで、その上に前記極薄銅箔めっき条件１〈硫酸銅めっき〉により電流密度４．５Ａ／ｄｍ２で３μｍ厚さの極薄銅箔を形成し、キャリア付き極薄銅箔とした。
更に、Ｎｉ：０．５ｍｇ/dm2、Ｚｎ：０．０５ｍｇ／ｄｍ２、Ｃｒ：０．３ｍｇ／ｄｍ２の表面処理後、シランカップリング剤処理（後処理）を行い、キャリア付き極薄銅箔を得た。
<Example 6>
→ Diffusion prevention layer plating conditions <Ni plating>
→ Peeling layer preparation plating condition 2 <Mo-Co plating>
→ P-containing ultra-thin copper layer production plating condition 3 <copper sulfate plating (P-containing)>
→ Ultra-thin copper foil plating condition 1 <Copper sulfate plating>
Manufacturing of ultra-thin copper foil with carrier, which was sequentially plated by the above.
A copper foil (thickness: 31 μm) with Rz: 0.8 μm on one side was used as a carrier foil, and a diffusion prevention layer was applied on the carrier foil under the Ni plating conditions, and then peeled off by Mo-Co plating under the following conditions: A layer was formed.
Co amount: 4.0 g / dm 3
Mo amount: 2.0 g / dm 3
Citric acid: 80 g / dm 3
Current density: 2 A / dm 2
Energizing time: 15 seconds Bath temperature: 50 ° C
The adhesion amount of the formed release layer was 1.5 mg / dm 2 .
Copper plating was performed on the release layer to a thickness of 0.2 μm under P-containing ultrathin copper layer production plating condition 3 <copper sulfate plating (P-containing)>. The P adhesion amount of this layer was 0.014 mg / dm 2 . Subsequently, an ultrathin copper foil having a current density of 4.5 A / dm 2 and a thickness of 3 μm was formed on the ultrathin copper foil plating condition 1 (copper sulfate plating) thereon to obtain an ultrathin copper foil with a carrier.
Furthermore, after surface treatment of Ni: 0.5 mg / dm 2 , Zn: 0.05 mg / dm 2 , Cr: 0.3 mg / dm 2 , silane coupling agent treatment (post treatment) was performed, and ultrathin copper with a carrier A foil was obtained.
＜実施例７＞
→拡散防止層作製めっき条件〈Ｎｉめっき〉
→剥離層作製めっき条件３〈Ｍｏ−Ｎｉめっき〉
→Ｐ含有極薄銅層作製めっき条件１〈ピロリン酸銅めっき１〉
→極薄銅箔めっき条件１〈硫酸銅めっき〉
によるめっきを順次行ったキャリア付き極薄銅箔の製造。
片面がＲｚ：０．８μｍの銅箔（厚さ：３１μｍ）をキャリア箔とし、該キャリア箔上に前記Ｎｉめっき条件下において拡散防止層を施した後、下記条件にてＭｏ−Ｎｉめっきにより剥離層を形成した。
硫酸Ｎｉ六水和物 ：５０ｇ／ｄｍ３
モリブデン酸ナトリウム二水和物 ：６０ｇ／ｄｍ３
クエン酸ナトリウム ：９０ｇ／ｄｍ３
浴温 ：３０℃
電流密度 ：３Ａ／ｄｍ２
通電時間 ：２０秒
作製した剥離層の付着量は：２．４ｍｇ／ｄｍ２であった。
該剥離層上にＰ含有極薄銅層作製めっき条件１〈ピロリン酸銅めっき１〉で０．２μｍ厚さに銅めっきを施した。この層のＰ付着量は０．０１３ｍｇ／ｄｍ２であった。次いで、その上に前記極薄銅箔めっき条件１〈硫酸銅めっき〉により電流密度４．５Ａ／ｄｍ２で３μｍ厚さの極薄銅箔を形成し、キャリア付き極薄銅箔とした。
更に、Ｎｉ：０．５ｍｇ／ｄｍ２、Ｚｎ：０．０５ｍｇ／ｄｍ２、Ｃｒ：０．３ｍｇ／ｄｍ２の表面処理後、シランカップリング剤処理（後処理）を行い、キャリア付き極薄銅箔を得た。
<Example 7>
→ Diffusion prevention layer plating conditions <Ni plating>
→ Peeling layer preparation plating condition 3 <Mo-Ni plating>
→ P-containing ultrathin copper layer preparation plating condition 1 <copper pyrophosphate copper plating 1>
→ Ultra-thin copper foil plating condition 1 <Copper sulfate plating>
Manufacturing of ultra-thin copper foil with carrier, which was sequentially plated by the above.
A copper foil (thickness: 31 μm) with Rz: 0.8 μm on one side was used as a carrier foil, and after applying a diffusion prevention layer on the carrier foil under the Ni plating conditions, peeling was performed by Mo-Ni plating under the following conditions: A layer was formed.
Ni sulfate sulfate: 50 g / dm 3
Sodium molybdate dihydrate: 60 g / dm 3
Sodium citrate: 90 g / dm 3
Bath temperature: 30 ° C
Current density: 3 A / dm 2
Energization time: 20 seconds The adhesion amount of the produced release layer was: 2.4 mg / dm 2 .
On the release layer, copper plating was performed to a thickness of 0.2 μm under P-containing ultrathin copper layer production plating condition 1 <copper pyrophosphate plating 1>. The P adhesion amount of this layer was 0.013 mg / dm 2 . Subsequently, an ultrathin copper foil having a current density of 4.5 A / dm 2 and a thickness of 3 μm was formed on the ultrathin copper foil plating condition 1 (copper sulfate plating) thereon to obtain an ultrathin copper foil with a carrier.
Furthermore, after surface treatment of Ni: 0.5 mg / dm 2 , Zn: 0.05 mg / dm 2 , Cr: 0.3 mg / dm 2 , silane coupling agent treatment (post treatment) was performed, and ultrathin copper with a carrier A foil was obtained.
＜実施例８＞
キャリア箔
→拡散防止層作製めっき条件〈Ｎｉめっき〉
→剥離層作製めっき条件４〈Ｗ−Ｎｉめっき〉
→Ｐ含有極薄銅層作製めっき条件１〈ピロリン酸銅めっき１〉
→極薄銅箔めっき条件１〈硫酸銅めっき〉
によるめっきを順次行ったキャリア付き極薄銅箔の製造。
片面がＲｚ：０．８μｍの銅箔（厚さ：３１μｍ）をキャリア箔とし、該キャリア箔上に前記Ｎｉめっき条件下において拡散防止層を施した後、下記条件にてＷ−Ｎｉめっきにより剥離層を形成した。
硫酸Ｎｉ六水和物 ：５０ｇ／ｄｍ３
タングステン酸ナトリウム二水和物 ：６０ｇ／ｄｍ３
クエン酸ナトリウム ：９０ｇ／ｄｍ３
浴温 ：７０℃
電流密度 ：２．５Ａ／ｄｍ２
通電時間 ：１８秒
作製した剥離層の付着量は：２．１ｍｇ／ｄｍ２であった。
該剥離層上にＰ含有極薄銅層作製めっき条件１〈ピロリン酸銅めっき１〉で０．２μｍ厚さに銅めっきを施した。この層のＰ付着量は０．０１１ｍｇ／ｄｍ２であった。次いで、その上に前記極薄銅箔めっき条件１〈硫酸銅めっき〉により電流密度４．５Ａ／ｄｍ２で３μｍ厚さの極薄銅箔を形成し、キャリア付き極薄銅箔とした。
該剥離層上に厚さ０．２μmの銅めっき層を形成した後、更に＜銅めっき条件３＞を使用し銅めっき層を、電流密度４．５Ａ／ｄｍ２のめっきで形成し、３μｍ厚さの極薄銅箔を形成させ、キャリア付き極薄銅箔とした。
更に、Ｎｉ：０．５ｍｇ／ｄｍ２、Ｚｎ：０．０５ｍｇ／ｄｍ２、Ｃｒ：０．３ｍｇ／ｄｍ２の表面処理後、シランカップリング剤処理（後処理）を行い、キャリア付き極薄銅箔を得た。
<Example 8>
Carrier foil → Diffusion prevention layer preparation plating conditions <Ni plating>
→ Peeling layer preparation plating condition 4 <W-Ni plating>
→ P-containing ultrathin copper layer preparation plating condition 1 <copper pyrophosphate copper plating 1>
→ Ultra-thin copper foil plating condition 1 <Copper sulfate plating>
Manufacturing of ultra-thin copper foil with carrier, which was sequentially plated by the above.
A copper foil (thickness: 31 μm) with Rz: 0.8 μm on one side was used as a carrier foil, and a diffusion prevention layer was applied on the carrier foil under the Ni plating conditions, and then peeled off by W-Ni plating under the following conditions: A layer was formed.
Ni sulfate sulfate: 50 g / dm 3
Sodium tungstate dihydrate: 60 g / dm 3
Sodium citrate: 90 g / dm 3
Bath temperature: 70 ° C
Current density: 2.5 A / dm 2
Energizing time: 18 seconds The adhesion amount of the produced release layer was: 2.1 mg / dm 2 .
On the release layer, copper plating was performed to a thickness of 0.2 μm under P-containing ultrathin copper layer production plating condition 1 <copper pyrophosphate plating 1>. The P adhesion amount of this layer was 0.011 mg / dm 2 . Subsequently, an ultrathin copper foil having a current density of 4.5 A / dm 2 and a thickness of 3 μm was formed on the ultrathin copper foil plating condition 1 (copper sulfate plating) thereon to obtain an ultrathin copper foil with a carrier.
After forming a copper plating layer having a thickness of 0.2 μm on the release layer, a copper plating layer is further formed by plating with a current density of 4.5 A / dm 2 using <copper plating condition 3>, and a thickness of 3 μm. A very thin copper foil was formed to obtain an ultrathin copper foil with a carrier.
Furthermore, after surface treatment of Ni: 0.5 mg / dm 2 , Zn: 0.05 mg / dm 2 , Cr: 0.3 mg / dm 2 , silane coupling agent treatment (post treatment) was performed, and ultrathin copper with a carrier A foil was obtained.
＜実施例９＞
→拡散防止層作製めっき条件〈Ｎｉめっき〉
→剥離層作製めっき条件４〈Ｗ−Ｃｏめっき〉
→Ｐ含有極薄銅層作製めっき条件１〈ピロリン酸銅めっき１〉
→極薄銅箔めっき条件１〈硫酸銅めっき〉
によるめっきを順次行ったキャリア付き極薄銅箔の製造。
片面がＲｚ：０．８μｍの銅箔（厚さ：３１μｍ）をキャリア箔とし、該キャリア箔上に前記Ｎｉめっき条件下において拡散防止層を施した後、下記条件にてＷ−Ｃｏめっきにより剥離層を形成した。
Ｃｏ量 ：４．０ｇ／ｄｍ３
タングステン酸ナトリウム二水和物 ：６０ｇ／ｄｍ３
クエン酸ナトリウム ：９０ｇ／ｄｍ３
浴温 ：７０℃
電流密度 ：２．５Ａ／ｄｍ２
通電時間 ：１８秒
作製した剥離層の付着量は：２．１ｍｇ／ｄｍ２であった。
該剥離層上にＰ含有極薄銅層作製めっき条件１〈ピロリン酸銅めっき１〉で０．２μｍ厚さに銅めっきを施した。この層のＰ付着量は０．０１２ｍｇ／ｄｍ２であった。次いで、その上に前記極薄銅箔めっき条件１〈硫酸銅めっき〉により電流密度４．５Ａ／ｄｍ２で３μｍ厚さの極薄銅箔を形成し、キャリア付き極薄銅箔とした。
更に、Ｎｉ：０．５ｍｇ／ｄｍ２、Ｚｎ：０．０５ｍｇ／ｄｍ２、Ｃｒ：０．３ｍｇ／ｄｍ２の表面処理後、シランカップリング剤処理（後処理）を行い、キャリア付き極薄銅箔を得た。
<Example 9>
→ Diffusion prevention layer plating conditions <Ni plating>
→ Peeling layer preparation plating condition 4 <W-Co plating>
→ P-containing ultrathin copper layer preparation plating condition 1 <copper pyrophosphate copper plating 1>
→ Ultra-thin copper foil plating condition 1 <Copper sulfate plating>
Manufacturing of ultra-thin copper foil with carrier, which was sequentially plated by the above.
A copper foil (thickness: 31 μm) with Rz: 0.8 μm on one side was used as a carrier foil, and a diffusion prevention layer was applied on the carrier foil under the Ni plating conditions, followed by peeling by W-Co plating under the following conditions: A layer was formed.
Co amount: 4.0 g / dm 3
Sodium tungstate dihydrate: 60 g / dm 3
Sodium citrate: 90 g / dm 3
Bath temperature: 70 ° C
Current density: 2.5 A / dm 2
Energizing time: 18 seconds The adhesion amount of the produced release layer was: 2.1 mg / dm 2 .
On the release layer, copper plating was performed to a thickness of 0.2 μm under P-containing ultrathin copper layer production plating condition 1 <copper pyrophosphate plating 1>. The P adhesion amount of this layer was 0.012 mg / dm 2 . Subsequently, an ultrathin copper foil having a current density of 4.5 A / dm 2 and a thickness of 3 μm was formed on the ultrathin copper foil plating condition 1 (copper sulfate plating) thereon to obtain an ultrathin copper foil with a carrier.
Furthermore, after surface treatment of Ni: 0.5 mg / dm 2 , Zn: 0.05 mg / dm 2 , Cr: 0.3 mg / dm 2 , silane coupling agent treatment (post treatment) was performed, and ultrathin copper with a carrier A foil was obtained.
＜比較例１＞
キャリア箔
→拡散防止層作製めっき条件〈Ｎｉめっき〉
→剥離層作製めっき条件１〈Ｃｒめっき〉
→極薄銅箔めっき条件１〈硫酸銅めっき〉
によるめっきを順次行ったキャリア付き極薄銅箔の製造。
片面がＲｚ：０．８μｍの銅箔（厚さ：３１μｍ）をキャリア箔とし、該キャリア箔上に前記Ｎｉめっき条件下において拡散防止層を施した後、下記条件にてＣｒめっきにより剥離層を形成した。
Ｃｒ量 ：２５０ｇ／ｄｍ３
硫酸 ：２．５ｇ／ｄｍ３
電流密度 ：１０Ａ／ｄｍ２
通電時間 ：６０秒
浴温 ：５０℃
形成した剥離層の付着量は０．０１ｍｇ/ｄｍ２であった。
該剥離層上に前記極薄銅箔めっき条件１〈硫酸銅めっき〉により電流密度４．５Ａ／ｄｍ２で３μｍ厚さの極薄銅箔を形成し、キャリア付き極薄銅箔とした。
次いで、Ｎｉ：０．５ｍｇ/dm2、Ｚｎ：０．０５ｍｇ／ｄｍ２、Ｃｒ：０．３ｍｇ／ｄｍ２の表面処理後、シランカップリング剤処理（後処理）を行い、キャリア付き極薄銅箔を得た。
<Comparative Example 1>
Carrier foil → Diffusion prevention layer preparation plating conditions <Ni plating>
→ Peeling layer preparation plating condition 1 <Cr plating>
→ Ultra-thin copper foil plating condition 1 <Copper sulfate plating>
Manufacturing of ultra-thin copper foil with carrier, which was sequentially plated by the above.
A copper foil (thickness: 31 μm) having a Rz of 0.8 μm on one side was used as a carrier foil, and a diffusion prevention layer was applied on the carrier foil under the Ni plating conditions, followed by Cr plating under the following conditions. Formed.
Cr amount: 250 g / dm 3
Sulfuric acid: 2.5 g / dm 3
Current density: 10 A / dm 2
Energizing time: 60 seconds Bath temperature: 50 ° C
The adhesion amount of the formed release layer was 0.01 mg / dm 2 .
An ultrathin copper foil having a current density of 4.5 A / dm 2 and a thickness of 3 μm was formed on the release layer under the ultrathin copper foil plating condition 1 <copper sulfate plating> to obtain an ultrathin copper foil with a carrier.
Next, after surface treatment of Ni: 0.5 mg / dm 2 , Zn: 0.05 mg / dm 2 , Cr: 0.3 mg / dm 2 , silane coupling agent treatment (post treatment) is performed, and ultrathin copper with a carrier A foil was obtained.
＜比較例２＞
キャリア箔
→拡散防止層作製めっき条件〈Ｎｉめっき〉
→剥離層作製めっき条件２〈Ｍｏ−Ｃｏめっき〉
→極薄銅箔めっき条件１〈硫酸銅めっき〉
によるめっきを順次行ったキャリア付き極薄銅箔の製造。
片面がＲｚ：０．８μｍの銅箔（厚さ：３１μｍ）をキャリア箔とし、該キャリア箔上に前記Ｎｉめっき条件下において拡散防止層を施した後、下記条件にてＭｏ−Ｃｏめっきにより剥離層を形成した。
Ｃｏ量 ：４．０ｇ／ｄｍ３
Ｍｏ量 ：２.０ｇ／ｄｍ３
クエン酸 ：８０ｇ／ｄｍ３
電流密度 ：２Ａ／ｄｍ２
通電時間 ：１５秒
浴温 ：５０℃
形成した剥離層の付着量は１．５ｍｇ/ｄｍ２であった。
該剥離層上に前記極薄銅箔めっき条件１〈硫酸銅めっき〉により電流密度４．５Ａ／ｄｍ２で３μｍ厚さの極薄銅箔を形成し、キャリア付き極薄銅箔とした。
次いで、Ｎｉ：０．５ｍｇ／ｄｍ２、Ｚｎ：０．０５ｍｇ／ｄｍ２、Ｃｒ：０．３ｍｇ／ｄｍ２の表面処理後、シランカップリング剤処理（後処理）を行い、キャリア付き極薄銅箔を得た。
<Comparative example 2>
Carrier foil → Diffusion prevention layer preparation plating conditions <Ni plating>
→ Peeling layer preparation plating condition 2 <Mo-Co plating>
→ Ultra-thin copper foil plating condition 1 <Copper sulfate plating>
Manufacturing of ultra-thin copper foil with carrier, which was sequentially plated by the above.
A copper foil (thickness: 31 μm) with Rz: 0.8 μm on one side was used as a carrier foil, and a diffusion prevention layer was applied on the carrier foil under the Ni plating conditions, and then peeled off by Mo-Co plating under the following conditions: A layer was formed.
Co amount: 4.0 g / dm 3
Mo amount: 2.0 g / dm 3
Citric acid: 80 g / dm 3
Current density: 2 A / dm 2
Energizing time: 15 seconds Bath temperature: 50 ° C
The adhesion amount of the formed release layer was 1.5 mg / dm 2 .
An ultrathin copper foil having a current density of 4.5 A / dm 2 and a thickness of 3 μm was formed on the release layer under the ultrathin copper foil plating condition 1 <copper sulfate plating> to obtain an ultrathin copper foil with a carrier.
Next, after surface treatment of Ni: 0.5 mg / dm 2 , Zn: 0.05 mg / dm 2 , Cr: 0.3 mg / dm 2 , silane coupling agent treatment (post treatment) is performed, and ultrathin copper with a carrier A foil was obtained.
＜評価＞
上記実施例及び比較例で作製したキャリア付き極薄銅箔のキャリアピール評価用サンプル及びフクレ確認用サンプルを下記のように作製し評価した。
<Evaluation>
A carrier peel evaluation sample and a bulge confirmation sample of the ultrathin copper foil with carrier prepared in the above Examples and Comparative Examples were prepared and evaluated as follows.
（１）キャリアピール測定及びフクレ確認用サンプル
キャリア付き極薄銅箔（実施例１〜９、比較例１、２）を、縦２５０ｍｍ、横２５０ｍｍに切断したのち、温度３５０℃、１０分間加熱しフクレ確認用のサンプルを作製した。
また、上記熱処理したサンプルの極薄銅箔側に、両面テープで樹脂基板を貼り付け、キャリア箔付きのキャリアピール測定用片面銅張積層板とした。
(1) Sample for carrier peel measurement and blister confirmation Ultra thin copper foil with carrier (Examples 1 to 9, Comparative Examples 1 and 2) was cut into 250 mm length and 250 mm width, and then heated at 350 ° C. for 10 minutes. A sample for checking blisters was produced.
Moreover, the resin substrate was affixed with the double-sided tape on the ultra-thin copper foil side of the heat-treated sample, and a single-sided copper-clad laminate for carrier peel measurement with a carrier foil was obtained.
（２）ピンホール確認サンプル
キャリア付き極薄銅箔（実施例１〜９、比較例１、２）を、縦２５０ｍｍ、横２５０ｍｍに切断し、透明テープを極薄銅箔側に貼り付け、極薄銅箔をキャリア箔から剥離してピンホール確認用のサンプルとした。
(2) Pinhole Confirmation Sample Ultrathin copper foil with carrier (Examples 1-9, Comparative Examples 1 and 2) is cut into 250 mm length and 250 mm width, and a transparent tape is attached to the ultrathin copper foil side. The thin copper foil was peeled from the carrier foil to obtain a sample for pinhole confirmation.
＜極薄銅箔の特性評価＞
（１）キャリアピールの測定方法とフクレの確認
（ａ）フクレの確認
キャリア箔上の極薄銅箔が膨れているかどうかを目視で観察し、フクレの数を数えた。その結果を表１に示す。
（ｂ）キャリアピールの測定
上記（１）の方法により作製した試料を、ＪＩＳＣ６５１１に規定する方法に準拠して、測定試料幅１０ｍｍでキャリア箔から極薄銅箔を引き剥がし、キャリアピール（ピール強度）をｎ数３で測定した。評価結果を表１に示す。
<Characteristic evaluation of ultrathin copper foil>
(1) Confirmation of carrier peel measurement and blistering (a) Checking blistering Whether or not the ultrathin copper foil on the carrier foil is swollen was visually observed and the number of blisters was counted. The results are shown in Table 1.
(B) Measurement of carrier peel In accordance with the method specified in JISC6511, the sample prepared by the method of (1) above is peeled off from the carrier foil with a measurement sample width of 10 mm, and the carrier peel (peel strength) ) Was measured by n number 3. The evaluation results are shown in Table 1.
（ｃ）ピンホール確認
上記（２）ピンホール測定用サンプルに暗室にて下から光を照射し、ピンホールにより光が透過した数をピンホール数とした。結果を表１に示す。
(C) Pinhole confirmation The sample for pinhole measurement (2) was irradiated with light from below in a dark room, and the number of light transmitted through the pinhole was defined as the number of pinholes. The results are shown in Table 1.
＜評価結果＞
実施例１〜３の極薄銅箔作製工程時に、剥離層Ｃｒ上にＰを介在させることにより、比較例１に比べキャリアピールが低くなった。また、実施例４〜９の極薄銅箔作製工程時に、各複合めっき剥離層上にＰを介在させることにより比較例２に比べキャリアピールが低くなった。このように、剥離層上にＰを介在させることによりキャリアピールが低くなっている。
また、Ｐを介在させてもフクレ・ピンホールに対する影響が無いことも示された。
<Evaluation results>
By interposing P on the release layer Cr during the ultrathin copper foil manufacturing steps of Examples 1 to 3, the carrier peel was lower than that of Comparative Example 1. Moreover, the carrier peel became low compared with the comparative example 2 by interposing P on each composite plating peeling layer at the time of the ultra-thin copper foil preparation process of Examples 4-9. Thus, the carrier peel is lowered by interposing P on the release layer.
It was also shown that there was no effect on the bulge / pinhole even if P was interposed.
本発明は上述したように、各種剥離層上にＰを介在させてもフクレ・ピンホールに影響を与えずキャリアピールを低減することができため、キャリア付き極薄銅箔の製造条件が緩和され、管理範囲が広がるため製造品質を安定化させることができ、高温下の環境に置かれてもキャリア箔と極薄銅箔とを容易に剥がすことができるキャリア付き極薄銅箔を提供することができる。
また本発明は、前記キャリア付き極薄銅箔を使用したファインパターン用途のプリント配線板、多層プリント配線板、チップオンフィルム用配線板等の基材として、製造品質が安定したプリント配線基板を提供することができる、優れた効果を有するものである。
As described above, since the present invention can reduce the carrier peel without affecting the blister pinhole even if P is interposed on various release layers, the manufacturing conditions of the ultra-thin copper foil with the carrier are eased. To provide an ultra-thin copper foil with a carrier that can stabilize the manufacturing quality due to the wide range of management, and can easily peel off the carrier foil and the ultra-thin copper foil even when placed in a high temperature environment Can do.
In addition, the present invention provides a printed wiring board having a stable production quality as a substrate for a fine pattern use printed wiring board, multilayer printed wiring board, chip-on-film wiring board, etc., using the ultra-thin copper foil with carrier. It has an excellent effect.
Claims (5)
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| JP2006147770A JP2007314855A (en) | 2006-05-29 | 2006-05-29 | Ultra-thin copper foil provided with carrier, copper-clad laminate and printed circuit board |
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