JP2018205072A - Method for inspecting surface of electrolytic copper foil and method for manufacturing electrolytic copper foil - Google Patents
Method for inspecting surface of electrolytic copper foil and method for manufacturing electrolytic copper foil Download PDFInfo
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- RYGMFSIKBFXOCR-UHFFFAOYSA-N Copper Chemical compound [Cu] RYGMFSIKBFXOCR-UHFFFAOYSA-N 0.000 title claims abstract description 115
- 239000011889 copper foil Substances 0.000 title claims abstract description 104
- 238000000034 method Methods 0.000 title claims abstract description 93
- 238000004519 manufacturing process Methods 0.000 title claims abstract description 15
- 238000007689 inspection Methods 0.000 claims abstract description 43
- 230000002159 abnormal effect Effects 0.000 claims abstract description 41
- 239000011248 coating agent Substances 0.000 claims abstract description 41
- 238000000576 coating method Methods 0.000 claims abstract description 41
- 238000007788 roughening Methods 0.000 claims description 72
- 239000000463 material Substances 0.000 claims description 18
- 239000000126 substance Substances 0.000 claims description 13
- 229910052802 copper Inorganic materials 0.000 claims description 11
- 239000010949 copper Substances 0.000 claims description 11
- 239000007788 liquid Substances 0.000 claims description 8
- 239000011344 liquid material Substances 0.000 claims description 4
- 238000005507 spraying Methods 0.000 claims description 4
- 230000003287 optical effect Effects 0.000 claims description 3
- 238000001514 detection method Methods 0.000 abstract description 2
- 230000005856 abnormality Effects 0.000 description 21
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- 229910000365 copper sulfate Inorganic materials 0.000 description 3
- ARUVKPQLZAKDPS-UHFFFAOYSA-L copper(II) sulfate Chemical compound [Cu+2].[O-][S+2]([O-])([O-])[O-] ARUVKPQLZAKDPS-UHFFFAOYSA-L 0.000 description 3
- 238000001000 micrograph Methods 0.000 description 3
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- 238000010438 heat treatment Methods 0.000 description 2
- JEIPFZHSYJVQDO-UHFFFAOYSA-N iron(III) oxide Inorganic materials O=[Fe]O[Fe]=O JEIPFZHSYJVQDO-UHFFFAOYSA-N 0.000 description 2
- 235000010446 mineral oil Nutrition 0.000 description 2
- 238000007747 plating Methods 0.000 description 2
- 238000004439 roughness measurement Methods 0.000 description 2
- 239000000243 solution Substances 0.000 description 2
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 description 1
- XEEYBQQBJWHFJM-UHFFFAOYSA-N Iron Chemical compound [Fe] XEEYBQQBJWHFJM-UHFFFAOYSA-N 0.000 description 1
- ZOKXTWBITQBERF-UHFFFAOYSA-N Molybdenum Chemical compound [Mo] ZOKXTWBITQBERF-UHFFFAOYSA-N 0.000 description 1
- 235000019482 Palm oil Nutrition 0.000 description 1
- RTAQQCXQSZGOHL-UHFFFAOYSA-N Titanium Chemical compound [Ti] RTAQQCXQSZGOHL-UHFFFAOYSA-N 0.000 description 1
- 230000002547 anomalous effect Effects 0.000 description 1
- 229910052799 carbon Inorganic materials 0.000 description 1
- 239000011247 coating layer Substances 0.000 description 1
- 239000010941 cobalt Substances 0.000 description 1
- 229910017052 cobalt Inorganic materials 0.000 description 1
- GUTLYIVDDKVIGB-UHFFFAOYSA-N cobalt atom Chemical compound [Co] GUTLYIVDDKVIGB-UHFFFAOYSA-N 0.000 description 1
- 150000001875 compounds Chemical class 0.000 description 1
- 238000001816 cooling Methods 0.000 description 1
- USIUVYZYUHIAEV-UHFFFAOYSA-N diphenyl ether Chemical class C=1C=CC=CC=1OC1=CC=CC=C1 USIUVYZYUHIAEV-UHFFFAOYSA-N 0.000 description 1
- 238000004070 electrodeposition Methods 0.000 description 1
- 238000005530 etching Methods 0.000 description 1
- 238000011156 evaluation Methods 0.000 description 1
- 235000019000 fluorine Nutrition 0.000 description 1
- 125000001153 fluoro group Chemical class F* 0.000 description 1
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- 229910052750 molybdenum Inorganic materials 0.000 description 1
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- 239000010936 titanium Substances 0.000 description 1
- 229910052719 titanium Inorganic materials 0.000 description 1
- WFKWXMTUELFFGS-UHFFFAOYSA-N tungsten Chemical compound [W] WFKWXMTUELFFGS-UHFFFAOYSA-N 0.000 description 1
- 229910052721 tungsten Inorganic materials 0.000 description 1
- 239000010937 tungsten Substances 0.000 description 1
- LEONUFNNVUYDNQ-UHFFFAOYSA-N vanadium atom Chemical compound [V] LEONUFNNVUYDNQ-UHFFFAOYSA-N 0.000 description 1
- 235000015112 vegetable and seed oil Nutrition 0.000 description 1
- 239000008158 vegetable oil Substances 0.000 description 1
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 1
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- Investigating Materials By The Use Of Optical Means Adapted For Particular Applications (AREA)
- Electroplating Methods And Accessories (AREA)
Abstract
Description
本発明は、電解銅箔の表面検査方法及び電解銅箔の製造方法に関する。 The present invention relates to an electrolytic copper foil surface inspection method and an electrolytic copper foil manufacturing method.
プリント配線板用電解銅箔は、一般的に、一方の表面が平滑な光沢面であり、他方の表面がプリプレグ等との密着性を確保するために、粗化処理が施された粗化処理面となっている。
この粗化処理は、通常、粗化処理前の電解銅箔のマット面(凹凸が大きい面)に銅等の粒子(以下、「粗化粒子」ともいう)を電析させる処理である。粗化処理前の電解銅箔の表面において、高い凸部が存在していたり、傷等によって表面形状が通常と異なっていた場合、電析時の電流密度が局所的に高くなることから、粗化粒子が局所的に多く析出してしまうことがある。このような現象は、粗化異常又は異常突起と呼ばれ、通常、その大きさは、直径が5〜100μm、高さが2〜30μmの範囲で発生することが多い。粗化異常又は異常突起が発生した箇所(以下、「粗化異常部」ともいう)が存在する銅張積層板を回路加工した場合、粗化異常部がエッチングで溶解されず、回路欠陥となったり、絶縁信頼性が損なわれるといった問題が生じる。
Electrolytic copper foil for printed wiring boards is generally a roughening treatment in which one surface is a smooth glossy surface and the other surface is subjected to a roughening treatment in order to ensure adhesion to a prepreg or the like. It is a surface.
This roughening treatment is usually a treatment in which particles such as copper (hereinafter also referred to as “roughened particles”) are electrodeposited on the mat surface (surface with large irregularities) of the electrolytic copper foil before the roughening treatment. If the surface of the electrolytic copper foil before the roughening treatment has high protrusions, or if the surface shape is different from normal due to scratches or the like, the current density during electrodeposition increases locally. In some cases, a large number of particles are deposited locally. Such a phenomenon is called a roughening abnormality or abnormal protrusion, and the size thereof usually occurs in a range of 5 to 100 μm in diameter and 2 to 30 μm in height. When a copper-clad laminate with a roughening abnormality or abnormal protrusions (hereinafter also referred to as “roughening abnormality part”) is processed, the roughening abnormality part is not melted by etching, resulting in a circuit defect. Or the insulation reliability is impaired.
電解銅箔の粗化処理面の品質検査方法としては、表面粗さ測定、電子顕微鏡、実体顕微鏡、CCDカメラ等による観察などが行われている(例えば、特許文献1参照)。 As a quality inspection method for the roughened surface of the electrolytic copper foil, surface roughness measurement, observation with an electron microscope, a stereomicroscope, a CCD camera, or the like is performed (for example, see Patent Document 1).
しかしながら、表面粗さ測定、電子顕微鏡等による検査方法は、極めて小さい面積しか測定できないため、粗化異常部を検出することが困難である。
また、実体顕微鏡、CCDカメラ等による観察は、粗化処理面の色調がほぼ均一であること、粗化異常部のサイズが小さいこと等に起因して、粗化異常部の検出及び判別が困難であるという課題がある。
However, the surface roughness measurement, the inspection method using an electron microscope, etc. can measure only a very small area, so that it is difficult to detect a roughened abnormal portion.
In addition, observation with a stereomicroscope, a CCD camera, etc. makes it difficult to detect and discriminate the roughened abnormal part due to the fact that the color tone of the roughened surface is almost uniform and the size of the roughened abnormal part is small. There is a problem of being.
本発明は、電解銅箔の粗化処理面に存在する粗化異常部を、容易かつ高精度で検出することができる電解銅箔の表面検査方法、及び該検査方法を適用した電解銅箔の製造方法を提供することを目的とする。 The present invention relates to an electrolytic copper foil surface inspection method capable of easily and highly accurately detecting a roughened abnormal portion present on the roughened surface of the electrolytic copper foil, and an electrolytic copper foil to which the inspection method is applied. An object is to provide a manufacturing method.
本発明者らは、上記課題を解決すべく鋭意検討を重ねた結果、電解銅箔の粗化処理面に塗膜を形成し、該塗膜を観察することで、容易かつ高精度で粗化異常部を検出できることを見出し、本発明を完成するに至った。すなわち、本発明は、以下の[1]〜[8]に関する。
[1]粗化処理面を有する電解銅箔の表面検査方法であって、前記電解銅箔の粗化処理面上に、粗化異常部観察用物質の塗膜を形成する工程と、前記塗膜を観察して粗化異常部を検出する工程と、を有する電解銅箔の表面検査方法。
[2]前記粗化異常部観察用物質が、25℃で液状の物質である、上記[1]に記載の電解銅箔の表面検査方法。
[3]前記25℃で液状の物質が、親油性の液体である、上記[2]に記載の電解銅箔の表面検査方法。
[4]前記塗膜を形成する工程が、前記電解銅箔の粗化処理面に前記粗化異常部観察用物質を噴霧して塗膜を形成する工程である、上記[1]〜[3]のいずれかに記載の電解銅箔の表面検査方法。
[5]前記電解銅箔が、プリント配線板用電解銅箔である、上記[1]〜[4]のいずれかに記載の電解銅箔の表面検査方法。
[6]前記塗膜の観察を、光学顕微鏡を用いて行う、上記[1]〜[5]のいずれかに記載の電解銅箔の表面検査方法。
[7]電解銅箔の少なくとも一方の面を粗化処理する工程と、得られた粗化処理後の電解銅箔に対して、上記[1]〜[6]のいずれかに記載の電解銅箔の表面検査方法を実施して良否を判定する工程を含む、電解銅箔の製造方法。
[8]前記粗化処理が、前記電解銅箔の表面に銅を析出させる処理である、上記[7]に記載の電解銅箔の製造方法。
As a result of intensive studies to solve the above problems, the present inventors formed a coating film on the roughened surface of the electrolytic copper foil, and observed the coating film, thereby easily and accurately roughening the surface. The present inventors have found that an abnormal part can be detected and have completed the present invention. That is, the present invention relates to the following [1] to [8].
[1] A method for inspecting a surface of an electrolytic copper foil having a roughened surface, the step of forming a coating film of a material for observing a roughened abnormal portion on the roughened surface of the electrolytic copper foil; And a step of observing the film to detect a roughened abnormal portion, and a method for inspecting the surface of the electrolytic copper foil.
[2] The surface inspection method for an electrolytic copper foil according to the above [1], wherein the material for observing a roughened abnormal portion is a liquid material at 25 ° C.
[3] The surface inspection method for an electrolytic copper foil according to the above [2], wherein the substance that is liquid at 25 ° C. is a lipophilic liquid.
[4] The above-mentioned [1] to [3], wherein the step of forming the coating film is a step of forming a coating film by spraying the roughening abnormality portion observing substance on the roughened surface of the electrolytic copper foil. ] The surface inspection method of the electrolytic copper foil in any one of.
[5] The surface inspection method for an electrolytic copper foil according to any one of the above [1] to [4], wherein the electrolytic copper foil is an electrolytic copper foil for a printed wiring board.
[6] The surface inspection method for an electrolytic copper foil according to any one of [1] to [5], wherein the coating film is observed using an optical microscope.
[7] The electrolytic copper according to any one of [1] to [6] above with respect to the step of roughening at least one surface of the electrolytic copper foil and the obtained electrolytic copper foil after the roughening treatment. The manufacturing method of electrolytic copper foil including the process of implementing the surface inspection method of foil and determining the quality.
[8] The method for producing an electrolytic copper foil according to [7], wherein the roughening treatment is a treatment for precipitating copper on a surface of the electrolytic copper foil.
本発明によれば、電解銅箔の粗化処理面に存在する粗化異常部を、容易かつ高精度で検出することができる電解銅箔の表面検査方法、及び該検査方法を適用した電解銅箔の製造方法を提供することができる。 ADVANTAGE OF THE INVENTION According to this invention, the surface inspection method of the electrolytic copper foil which can detect the roughening abnormality part which exists in the roughening process surface of electrolytic copper foil easily and with high precision, and the electrolytic copper which applied this inspection method A method for producing a foil can be provided.
以下、本発明の一実施形態について詳述するが、本発明は以下の実施形態に限定されるものではない。
なお、以下の実施形態において、粗化処理前の電解銅箔を「未処理電解銅箔」と称することがあり、単に「電解銅箔」という場合は、「粗化処理後の電解銅箔」を指すものとする。
Hereinafter, one embodiment of the present invention will be described in detail, but the present invention is not limited to the following embodiment.
In the following embodiments, the electrolytic copper foil before the roughening treatment may be referred to as “untreated electrolytic copper foil”, and when simply referred to as “electrolytic copper foil”, “the electrolytic copper foil after the roughening treatment”. Shall be pointed to.
[電解銅箔の表面検査方法]
本実施形態の電解銅箔の表面検査方法は、粗化処理面を有する電解銅箔の表面検査方法であって、前記電解銅箔の粗化処理面上に、粗化異常部観察用物質の塗膜を形成する工程(以下、「塗膜形成工程」ともいう)と、前記塗膜を観察して粗化異常部を検出する工程(以下、「観察工程」ともいう)と、を有する電解銅箔の表面検査方法である。
本実施形態の検査方法において、粗化異常部観察用物質は、粗化処理面に形成された粗化粒子間の微細な隙間に侵入し、表面張力によって粗化処理面上に塗膜が形成される。該塗膜が形成された部分は色調が殆ど一定となるが、粗化異常部では、正常な部分と比較して粗化粒子の高さが高いことに起因して塗膜が形成されなかったり、塗膜が薄くなり、色調、形状等が正常な部分とは異なって見える。このため、塗膜を形成した粗化処理面を、実体顕微鏡等で観察することで、塗膜を形成していない場合よりも、粗化異常部の検出、判別等を容易かつ高精度に行うことができる。
[Electrolytic copper foil surface inspection method]
The surface inspection method for an electrolytic copper foil according to the present embodiment is a surface inspection method for an electrolytic copper foil having a roughened surface. Electrolysis having a step of forming a coating film (hereinafter also referred to as “coating layer forming step”) and a step of observing the coating film and detecting a roughening abnormality portion (hereinafter also referred to as “observation step”) This is a surface inspection method for copper foil.
In the inspection method of the present embodiment, the roughening abnormal portion observation material enters fine gaps between the roughened particles formed on the roughened surface, and a coating film is formed on the roughened surface by surface tension. Is done. The color tone of the portion where the coating film is formed is almost constant, but in the roughening abnormal portion, the coating film is not formed due to the fact that the height of the roughening particles is higher than the normal portion. The film becomes thinner and looks different from the normal part in color, shape, etc. For this reason, by observing the roughened surface on which the coating film is formed with a stereomicroscope or the like, it is possible to detect and discriminate roughening abnormalities more easily and accurately than when the coating film is not formed. be able to.
<電解銅箔>
本実施形態の検査方法を適用する電解銅箔は、粗化処理面を有する電解銅箔である。
本実施形態の検査方法によると、回路欠陥等の原因となる粗化異常部を容易かつ高精度で検出できるため、本実施形態の検査方法は、特に、プリント配線板用銅張積層板等に用いられる、プリント配線板用電解銅箔に対して好適である。
電解銅箔が有する粗化処理面の表面粗さRzは、特に限定されず、例えば、0.5〜20μmであってもよく、また、回路のファインピッチ化の観点からは、0.5〜6μmであってもよい。電解銅箔の表面粗さRzは、JIS B0601:1982に準拠して測定することができる。
電解銅箔の厚さは、例えば、1〜100μmであってもよく、電解銅箔の機械強度及びプリント配線板の薄型化の観点からは、5〜50μmであってもよい。
次に、本実施形態の検査方法を、各工程順に説明する。
<Electrolytic copper foil>
The electrolytic copper foil to which the inspection method of this embodiment is applied is an electrolytic copper foil having a roughened surface.
According to the inspection method of the present embodiment, since the roughened abnormal portion that causes a circuit defect or the like can be detected easily and with high accuracy, the inspection method of the present embodiment is particularly suitable for a copper-clad laminate for printed wiring boards. It is suitable for the electrolytic copper foil for printed wiring boards used.
The surface roughness Rz of the roughened surface of the electrolytic copper foil is not particularly limited, and may be, for example, 0.5 to 20 μm. From the viewpoint of fine pitching of the circuit, 0.5 to It may be 6 μm. The surface roughness Rz of the electrolytic copper foil can be measured according to JIS B0601: 1982.
The thickness of the electrolytic copper foil may be, for example, 1 to 100 μm, and may be 5 to 50 μm from the viewpoint of mechanical strength of the electrolytic copper foil and thinning of the printed wiring board.
Next, the inspection method of this embodiment will be described in the order of each process.
<塗膜形成工程>
塗膜形成工程は、電解銅箔の粗化処理面上に、粗化異常部観察用物質の塗膜を形成する工程である。なお、塗膜形成工程の前に、必要に応じて、電解銅箔を観察し易い大きさに適宜加工しておいてもよい。
<Coating film formation process>
A coating-film formation process is a process of forming the coating film of the roughening abnormality part observation substance on the roughening process surface of an electrolytic copper foil. In addition, before a coating-film formation process, you may process an electrolytic copper foil suitably in the magnitude | size which is easy to observe as needed.
(粗化異常部観察用物質)
粗化異常部観察用物質は、前述の通り、粗化処理面上に塗膜を形成し、粗化異常部の観察を容易にするために使用されるものであり、その目的を達成できるものであれば特に限定されない。
粗化異常部観察用物質は、通常、電解銅箔と反応性を有さず、かつ電解銅箔を溶解しないものであり、取り扱い性の観点から、25℃で液状である物質が好ましい。また、25℃で液状である物質は、表面張力が小さく、電解銅箔の粗化処理面上に塗膜を形成し易い観点から、親油性の液体であることが好ましい。
粗化異常部観察用物質の具体例としては、やし油等の植物油;パラフィン系、ナフテン系等の鉱物油;エステル化合物、ポリαオレフィン、ポリオールエステル化合物、アルキル置換ジフェニルエーテル、ポリフェニルエーテル、フッ素オイル、シリコーンオイル等の合成油;水;その他の有機溶剤;無機物質などが挙げられる。これらは1種を単独で用いてもよく、2種以上を混合して用いてもよい。これらの中でも、親油性の液体であり、電解銅箔上に塗膜を形成し易い観点から、油類(オイル)が好ましく、鉱物油及び合成油からなる群から選ばれる1種以上がより好ましく、鉱物油がさらに好ましい。さらに、上記の物質に対して、防錆添加剤等の特定の機能を付与した添加剤を適宜含ませたものであってもよい。
粗化異常部観察用物質として使用できる油類としては、例えば、市販品の潤滑油として入手することもできる。
(Material for observing roughening abnormalities)
As described above, the material for observing a roughened abnormal portion is used to form a coating film on the roughened surface to facilitate observation of the roughened abnormal portion, and can achieve its purpose. If it is, it will not specifically limit.
The material for observing a roughened abnormal part is usually a substance that is not reactive with the electrolytic copper foil and does not dissolve the electrolytic copper foil, and is preferably a liquid at 25 ° C. from the viewpoint of handleability. The substance that is liquid at 25 ° C. is preferably a lipophilic liquid from the viewpoint of low surface tension and easy formation of a coating film on the roughened surface of the electrolytic copper foil.
Specific examples of substances for observing anomalous roughening include vegetable oils such as palm oil; mineral oils such as paraffinic and naphthenic compounds; ester compounds, polyalphaolefins, polyol ester compounds, alkyl-substituted diphenyl ethers, polyphenyl ethers, fluorines Synthetic oils such as oil and silicone oil; water; other organic solvents; inorganic substances and the like. These may be used alone or in combination of two or more. Among these, from the viewpoint of being an oleophilic liquid and easily forming a coating film on the electrolytic copper foil, oils (oils) are preferable, and at least one selected from the group consisting of mineral oils and synthetic oils is more preferable. Mineral oil is more preferable. Furthermore, an additive provided with a specific function such as a rust preventive additive may be appropriately added to the above substance.
Examples of oils that can be used as the material for observing a roughening abnormality portion can also be obtained as commercially available lubricants.
粗化異常部観察用物質の25℃における動粘度は、粗化処理面の微小な空隙等にも侵入し易くする観点、及び粗化処理面上に塗膜を保持され易くする観点から、2〜70mm2/sが好ましく、5〜50mm2/sがより好ましい。
粗化異常部観察用物質の沸点は、短時間に揮発することを抑制し、作業性を良好にする観点から、常圧下において、150℃以上が好ましく、200℃以上がより好ましく、250℃以上がさらに好ましい。粗化異常部観察用物質の沸点の上限は特に制限はないが、例えば、500℃以下であってもよく、400℃以下であってもよい。
粗化異常部観察用物質は色調は、特に限定されないが、汎用性の観点から、透明であることが好ましい。
The kinematic viscosity at 25 ° C. of the material for observing a roughening abnormality portion is 2 from the viewpoint of making it easy to enter fine voids or the like on the roughening treatment surface, and from the viewpoint of easily holding the coating film on the roughening treatment surface. -70 mm < 2 > / s is preferable and 5-50 mm < 2 > / s is more preferable.
From the viewpoint of suppressing volatilization in a short time and improving workability, the boiling point of the material for observing a roughened abnormal portion is preferably 150 ° C. or higher, more preferably 200 ° C. or higher, and more preferably 250 ° C. or higher under normal pressure. Is more preferable. Although there is no restriction | limiting in particular in the upper limit of the boiling point of the roughening abnormality part observation substance, For example, 500 degrees C or less may be sufficient and 400 degrees C or less may be sufficient.
Although the color tone of the material for observing a roughened abnormal portion is not particularly limited, it is preferably transparent from the viewpoint of versatility.
(塗膜の形成)
電解銅箔の粗化処理面上に粗化異常部観察用物質の塗膜を形成する方法としては、例えば、粗化異常部観察用物質を、電解銅箔の粗化処理面上に塗工する方法、粗化異常部観察用物質を電解銅箔の粗化処理面上に噴霧する方法、電解銅箔を粗化異常部観察用物質に浸漬した後、取り出す方法などが挙げられる。これらの中でも、作業性の観点から、粗化異常部観察用物質を電解銅箔の粗化処理面上に噴霧する方法が好ましい。なお、粗化異常部観察用物質が常温で固体である場合には、粗化異常部観察用物質を加熱する方法、液状の物質と混合して溶液とする方法等によって液状にして、前記方法に適用することが好ましい。
(Formation of coating film)
As a method of forming a coating film of a roughening abnormal portion observation material on the roughened surface of the electrolytic copper foil, for example, a roughening abnormal portion observation material is coated on the roughened surface of the electrolytic copper foil. And a method of spraying a roughening abnormality portion observing substance on the roughened surface of the electrolytic copper foil, a method of taking out the electrolytic copper foil after immersing it in the roughening abnormality portion observing material, and the like. Among these, from the viewpoint of workability, a method of spraying the roughening abnormality portion observing substance on the roughened surface of the electrolytic copper foil is preferable. In the case where the material for observing a roughening abnormality portion is solid at room temperature, the above method is obtained by liquefying the material for observing the roughening abnormality portion by a method of heating, a method of mixing with a liquid material or the like It is preferable to apply to.
<観察工程>
観察工程は、塗膜形成工程で形成した塗膜を観察して粗化異常部を検出する工程である。
粗化異常部観察用物質の塗膜は、粗化異常部において、塗膜が形成されなかったり、塗膜が薄くなり、色調、形状等の外観が正常な部分とは異なって見えるため、観察によって、容易に粗化異常部を検出することができる。
塗膜の観察方法は特に限定されないが、作業性の観点から、光学顕微鏡を用いることが好ましく、実体顕微鏡を用いることがより好ましい。
粗化異常部は、前記顕微鏡等を介して目視することで検出することができるが、画像解析装置等を用いて自動カウントさせてもよい。
<Observation process>
An observation process is a process of observing the coating film formed at the coating film formation process, and detecting a roughening abnormal part.
The coating film of the material for observing the roughening abnormal part is observed because the coating film is not formed in the roughening abnormal part or the coating film becomes thin, and the appearance such as color tone and shape is different from the normal part. Thus, it is possible to easily detect the roughened abnormal portion.
The method for observing the coating film is not particularly limited, but from the viewpoint of workability, an optical microscope is preferably used, and a stereomicroscope is more preferably used.
The roughening abnormality portion can be detected by visual observation through the microscope or the like, but may be automatically counted using an image analysis device or the like.
塗膜観察時の圧力は、粗化異常部を検出し易い条件を適宜選択すればよいが、作業性の観点からは、常圧下で実施することが好ましい。
塗膜観察時の温度は、粗化異常部を検出し易い条件を適宜選択すればよいが、作業性の観点からは、0〜100℃が好ましく、15〜50℃がより好ましく、室温がさらに好ましく、常温(25℃)が特に好ましい。
なお、本明細書において、室温とは、加熱、冷却等の温度制御なしの雰囲気温度をいうものとし、一般に、15〜25℃程度であるが、天候、季節等によって変わり得るため、該範囲に限定されるものではない。
The pressure at the time of observing the coating film may be selected as appropriate so as to easily detect the roughened abnormal portion.
The temperature at the time of observing the coating film may be appropriately selected under conditions that allow easy detection of the roughened abnormal portion, but from the viewpoint of workability, 0-100 ° C is preferable, 15-50 ° C is more preferable, and room temperature is further Normal temperature (25 ° C.) is particularly preferable.
In this specification, room temperature refers to an ambient temperature without temperature control such as heating and cooling, and is generally about 15 to 25 ° C., but may vary depending on the weather, season, etc. It is not limited.
[電解銅箔の製造方法]
本実施形態の電解銅箔の製造方法は電解銅箔の少なくとも一方の面を粗化処理する工程(以下、「粗化処理工程」ともいう)と、得られた粗化処理後の電解銅箔に対して、前記本実施形態の電解銅箔の表面検査方法を実施して良否を判定する工程(以下、「検査工程」ともいう)を含む、電解銅箔の製造方法である。
[Method for producing electrolytic copper foil]
The method for producing an electrolytic copper foil of the present embodiment includes a step of roughening at least one surface of the electrolytic copper foil (hereinafter also referred to as “roughening step”), and the obtained electrolytic copper foil after the roughening treatment. On the other hand, it is a manufacturing method of electrolytic copper foil including the process (henceforth an "inspection process") which implements the surface inspection method of the electrolytic copper foil of the said embodiment, and determines a quality.
<粗化処理工程>
粗化処理工程は、電解銅箔の少なくとも一方の面を粗化処理する工程である。
本実施形態の製造方法において、粗化処理に供する未処理電解銅箔は、公知の方法によって製造することができる。その一例としては、硫酸銅水溶液等の電解液中に、SUS、チタン等の陰極回転ドラムと、該陰極回転ドラムに対して同心円状に鉛等の陽極を配置し、電解液を供給させつつ両極間に電流を流して電解液を電解させ、該陰極回転ドラムの表面に所定の厚さに銅を析出させ、この析出した銅を連続的に剥がして巻取る方法が挙げられる。この方法によると、通常は、陰極回転ドラム側の表面が光沢面となり、電解液と接していた面がマット面(凹凸面)となる。マット面の表面粗さRzは、製造容易性及びファインピッチ化の観点から、0.01〜2μmであることが好ましい。
<Roughening process>
The roughening treatment step is a step of roughening at least one surface of the electrolytic copper foil.
In the production method of the present embodiment, the untreated electrolytic copper foil subjected to the roughening treatment can be produced by a known method. As an example, a cathode rotating drum such as SUS or titanium and an anode such as lead concentrically with respect to the cathode rotating drum are arranged in an electrolytic solution such as an aqueous copper sulfate solution, and both electrodes are supplied while supplying the electrolytic solution. There is a method in which an electric current is passed between them to electrolyze the electrolytic solution, copper is deposited to a predetermined thickness on the surface of the cathode rotating drum, and the deposited copper is continuously peeled off and wound up. According to this method, normally, the surface on the cathode rotating drum side becomes a glossy surface, and the surface in contact with the electrolytic solution becomes a mat surface (uneven surface). The surface roughness Rz of the mat surface is preferably 0.01 to 2 μm from the viewpoint of ease of manufacture and fine pitch.
次に、未処理電解銅箔に対して、粗化処理を行う。
粗化処理は、例えば、硫酸銅等の電解液を電解させて、未処理電解銅箔のマット面(凹凸面)側に、銅を含む粗化粒子を均一に析出させる、めっき法によって行うことができる。より具体的には、未処理電解銅箔を陰極とし、対極に不溶性陽極を配置して、例えば、液温20〜40℃の硫酸銅等の銅めっき液を用い、平均陽極電流密度5A/dm2〜40A/dm2の条件で電解させ、未処理電解銅箔のマット面に粗化粒子を析出させることができる。さらに、上記の操作を必要に応じて複数回実施してもよい。
前記粗化処理工程によって形成する粗化粒子は、通常は、銅を含むものであり、銅以外の元素として、モリブデン(Mo)、ニッケル(Ni)、コバルト(Co)、鉄(Fe)、炭素(C)、バナジウム(V)及びタングステン(W)からなる群から選ばれる1種以上の元素を含有していてもよい。
前記粗化処理工程によって形成される粗化処理面の表面粗さRz及び厚さの好ましい範囲は、[電解銅箔の表面検査方法]において説明した電解銅箔の好ましい範囲と同じである。
また、粗化処理工程後には、要求品質に応じて、防錆処理等の表面処理を適宜実施してもよい。
Next, a roughening treatment is performed on the untreated electrolytic copper foil.
The roughening treatment is performed by, for example, a plating method in which an electrolytic solution such as copper sulfate is electrolyzed and the roughened particles containing copper are uniformly deposited on the mat surface (uneven surface) side of the untreated electrolytic copper foil. Can do. More specifically, an untreated electrolytic copper foil is used as a cathode, an insoluble anode is disposed on the counter electrode, and an average anode current density of 5 A / dm is used, for example, using a copper plating solution such as copper sulfate at a liquid temperature of 20 to 40 ° C. Electrolysis is performed under conditions of 2 to 40 A / dm 2 , and roughened particles can be deposited on the mat surface of the untreated electrolytic copper foil. Furthermore, the above operation may be performed a plurality of times as necessary.
The roughened particles formed by the roughening treatment step usually contain copper, and as an element other than copper, molybdenum (Mo), nickel (Ni), cobalt (Co), iron (Fe), carbon It may contain one or more elements selected from the group consisting of (C), vanadium (V) and tungsten (W).
The preferable range of the surface roughness Rz and the thickness of the roughened surface formed by the roughening process is the same as the preferable range of the electrolytic copper foil described in [Surface inspection method for electrolytic copper foil].
Further, after the roughening treatment step, surface treatment such as rust prevention treatment may be appropriately performed according to the required quality.
<検査工程>
検査工程は、粗化処理工程で得られた粗化処理後の電解銅箔に対して、前記本実施形態の電解銅箔の表面検査方法を実施して良否を判定する工程である。良否の判定は、事前に決定した基準に基づいて実施すればよく、例えば、製造ロットごとに、所定の面積の電解銅箔を切り出し、切り出した面積内において、本実施形態の電解銅箔の表面検査方法によって粗化異常部の個数を計測し、所定の基準を満たしたものを、「良」と判定し、満たさなかったものを「否」と判定することができる。
<Inspection process>
An inspection process is a process of determining the quality by implementing the surface inspection method of the electrolytic copper foil of this embodiment with respect to the electrolytic copper foil after the roughening process obtained at the roughening process. The determination of acceptability may be performed based on a predetermined criterion. For example, for each production lot, an electrolytic copper foil having a predetermined area is cut out, and the surface of the electrolytic copper foil of the present embodiment is cut out within the cut area. The number of roughened abnormal portions is measured by the inspection method, and those satisfying a predetermined standard can be determined as “good” and those not satisfied can be determined as “no”.
以下、実施例を示し、本発明について具体的に説明するが、本発明はこれらに限定されるものではない。 EXAMPLES Hereinafter, although an Example is shown and this invention is demonstrated concretely, this invention is not limited to these.
実施例1
(検査対象の準備)
検査対象の電解銅箔として、市販品である、厚さ18μmのプリント配線板用電解銅箔(表面粗さRz:7±1.5μm)と、厚さ35μmのプリント配線板用電解銅箔(表面粗さRz:8.5±1.5μm)の2種類を、各々5ロットずつ準備をした。さらに、各ロットの任意の位置から、A4サイズ(210mm×297mm)を2枚ずつ切り出して、これらを試験サンプルとした。
Example 1
(Preparation for inspection)
As electrolytic copper foils to be inspected, commercially available electrolytic copper foils for printed wiring boards having a thickness of 18 μm (surface roughness Rz: 7 ± 1.5 μm) and electrolytic copper foils for printed wiring boards having a thickness of 35 μm ( Two types of surface roughness Rz: 8.5 ± 1.5 μm) were prepared for 5 lots each. Further, two A4 sizes (210 mm × 297 mm) were cut out from arbitrary positions in each lot, and these were used as test samples.
(塗膜形成工程)
上記で準備した試験サンプルの粗化処理面上に、粗化異常部観察用物質として、オイル(呉工業株式会社製、商品名:CRC−556、鉱物油を主成分として含むオイル)を噴霧して、試験サンプルの粗化処理面全体が均一に濡れるように塗膜)を形成した。
(Coating film formation process)
On the roughened surface of the test sample prepared above, oil (product of Kure Kogyo Co., Ltd., trade name: CRC-556, oil containing mineral oil as a main component) is sprayed as a material for observing a roughening abnormality. Then, a coating film) was formed so that the entire roughened surface of the test sample was uniformly wetted.
(検査工程)
上記で塗膜を形成した試験サンプルの塗膜形成面を、実体顕微鏡(倍率:15倍)を用いて観察して、粗化異常部(正常な部分と色調又は形状が異なっている箇所)の数を目視で計測した。評価結果を表1に示す。なお、表1における粗化異常部の個数は、A4サイズの試験サンプル2枚当たりに含まれる粗化異常部の個数である。
(Inspection process)
The coating surface of the test sample on which the coating film was formed was observed using a stereomicroscope (magnification: 15 times), and a roughened abnormal portion (a portion having a different color tone or shape from a normal portion) was observed. The number was measured visually. The evaluation results are shown in Table 1. In addition, the number of roughening abnormal parts in Table 1 is the number of roughening abnormal parts included per two A4 size test samples.
比較例1
実施例1において、塗膜形成工程を実施しなかったことを以外は、実施例1と同様にして、検査を実施した。
Comparative Example 1
In Example 1, the inspection was performed in the same manner as in Example 1 except that the coating film forming step was not performed.
表1より、本発明の検査方法である実施例1では、塗膜形成工程を行わずに粗化処理面を観察した比較例1では検出できなかった粗化異常部を検出されており、電解銅箔の粗化処理面に発生する粗化異常部を容易かつ高精度で検出できることが分かる。
また、図1及び2には、実施例1及び比較例1で得られた、粗化処理面を有する電解銅箔の実体顕微鏡画像((a)視野1、(b)視野2)を各々示した。図1から明らかなように、本実施形態の検査方法で得られた実体顕微鏡画像においては、粗化異常部が正常な部分とは大きく異なって見えるため、粗化異常部の検出を容易にできることが分かる。
From Table 1, in Example 1 which is the inspection method of the present invention, a roughening abnormal portion that was not detected in Comparative Example 1 in which the roughened surface was observed without performing the coating film forming step was detected. It turns out that the roughening abnormality part which generate | occur | produces in the roughening process surface of copper foil can be detected easily and with high precision.
1 and 2 show stereoscopic microscope images ((a) field of view 1 and (b) field of view 2) of electrolytic copper foils having a roughened surface obtained in Example 1 and Comparative Example 1, respectively. It was. As apparent from FIG. 1, in the stereomicroscopic image obtained by the inspection method of the present embodiment, the roughened abnormal part appears to be significantly different from the normal part, so that the roughened abnormal part can be easily detected. I understand.
1 粗化処理面
2 粗化異常部
1 Roughening surface 2 Roughening abnormal part
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