WO2016174998A1 - Feuille de cuivre rugueuse et carte de câblage imprimée - Google Patents

Feuille de cuivre rugueuse et carte de câblage imprimée Download PDF

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Publication number
WO2016174998A1
WO2016174998A1 PCT/JP2016/061127 JP2016061127W WO2016174998A1 WO 2016174998 A1 WO2016174998 A1 WO 2016174998A1 JP 2016061127 W JP2016061127 W JP 2016061127W WO 2016174998 A1 WO2016174998 A1 WO 2016174998A1
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Prior art keywords
roughened
copper foil
particles
roughening
treatment
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PCT/JP2016/061127
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English (en)
Japanese (ja)
Inventor
響介 柳
美智 溝口
咲子 朝長
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三井金属鉱業株式会社
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Application filed by 三井金属鉱業株式会社 filed Critical 三井金属鉱業株式会社
Priority to JP2017515456A priority Critical patent/JP6682516B2/ja
Priority to CN201680024676.1A priority patent/CN107532322B/zh
Priority to KR1020177023365A priority patent/KR101975135B1/ko
Publication of WO2016174998A1 publication Critical patent/WO2016174998A1/fr

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    • C—CHEMISTRY; METALLURGY
    • C25—ELECTROLYTIC OR ELECTROPHORETIC PROCESSES; APPARATUS THEREFOR
    • C25D—PROCESSES FOR THE ELECTROLYTIC OR ELECTROPHORETIC PRODUCTION OF COATINGS; ELECTROFORMING; APPARATUS THEREFOR
    • C25D5/00—Electroplating characterised by the process; Pretreatment or after-treatment of workpieces
    • C25D5/60—Electroplating characterised by the structure or texture of the layers
    • C25D5/605—Surface topography of the layers, e.g. rough, dendritic or nodular layers
    • 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
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B32—LAYERED PRODUCTS
    • B32B—LAYERED PRODUCTS, i.e. PRODUCTS BUILT-UP OF STRATA OF FLAT OR NON-FLAT, e.g. CELLULAR OR HONEYCOMB, FORM
    • B32B15/00—Layered products comprising a layer of metal
    • B32B15/04—Layered products comprising a layer of metal comprising metal as the main or only constituent of a layer, which is next to another layer of the same or of a different material
    • B32B15/08—Layered products comprising a layer of metal comprising metal as the main or only constituent of a layer, which is next to another layer of the same or of a different material of synthetic resin
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B32—LAYERED PRODUCTS
    • B32B—LAYERED PRODUCTS, i.e. PRODUCTS BUILT-UP OF STRATA OF FLAT OR NON-FLAT, e.g. CELLULAR OR HONEYCOMB, FORM
    • B32B15/00—Layered products comprising a layer of metal
    • B32B15/20—Layered products comprising a layer of metal comprising aluminium or copper
    • C—CHEMISTRY; METALLURGY
    • C25—ELECTROLYTIC OR ELECTROPHORETIC PROCESSES; APPARATUS THEREFOR
    • C25D—PROCESSES FOR THE ELECTROLYTIC OR ELECTROPHORETIC PRODUCTION OF COATINGS; ELECTROFORMING; APPARATUS THEREFOR
    • C25D7/00—Electroplating characterised by the article coated
    • C25D7/06—Wires; Strips; Foils
    • 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

Definitions

  • the present invention relates to a roughened copper foil and a printed wiring board, and more specifically to a printed wiring board for high frequency applications and a roughened copper foil suitable for the same.
  • Flexible printed wiring boards are widely used in electronic devices such as portable electronic devices.
  • the frequency of signals has been increased to perform high-speed processing of a large amount of information, and a flexible printed wiring board suitable for high-frequency applications is required.
  • Such a high-frequency flexible printed wiring board is desired to reduce transmission loss in order to enable transmission of high-frequency signals without degrading quality.
  • the flexible printed wiring board has a copper foil processed into a wiring pattern and an insulating resin base material, but the transmission loss is a conductor loss due to the copper foil and a dielectric loss due to the insulating resin base material. And mainly.
  • the conductor loss can be further increased by the skin effect of the copper foil that appears more prominently at higher frequencies.
  • Patent Document 1 Japanese Patent Laid-Open No. 2014-224313
  • a primary particle layer of copper is formed on the surface of a copper foil, and then a secondary layer of Cu—Co—Ni alloy is formed on the primary particle layer.
  • a copper foil for a high-frequency circuit which is a copper foil having a particle layer, in which the average value of the unevenness of the roughened surface by a laser microscope is 1500 or more.
  • Patent Document 2 Japanese Patent Laid-Open No.
  • a primary particle layer of copper is formed on the surface of a copper foil, and then a secondary layer of Cu—Co—Ni alloy is formed on the primary particle layer.
  • a copper foil for a high-frequency circuit in which a ratio of a three-dimensional surface area to a two-dimensional surface area by a laser microscope in a certain region of a roughened surface is 2.0 or more and less than 2.2, is a copper foil having a particle layer formed thereon. ing. It is said that both of the copper foils described in Patent Documents 1 and 2 can be satisfactorily suppressed by using a high frequency circuit board.
  • an insulating resin base material capable of reducing dielectric loss has been proposed.
  • An example of such an insulating resin substrate is a liquid crystal polymer (LCP) film.
  • LCP liquid crystal polymer
  • insulating resin base materials suitable for high-frequency applications such as liquid crystal polymer films tend to have poor adhesion to copper foil, and copper foils that address such improved adhesion to insulating resin base materials are also proposed.
  • Patent Document 3 Japanese Patent Application Laid-Open No. 2005-219379
  • Patent Document 4 Japanese Patent Laid-Open No. 2010-236058 discloses a roughened copper foil having a roughened surface on which fine copper particles having a protrusion shape with a vertex angle of 85 ° or less are deposited. ing.
  • JP 2014-224313 A JP 2014-225650 A JP 2005-219379 A JP 2010-236058 A
  • low profile copper foil is required from the viewpoint of skin effect.
  • the low profile copper foil reduces the anchor effect with the insulating resin base material (that is, the effect of improving physical adhesion utilizing the unevenness of the copper foil surface). Therefore, it is difficult to obtain sufficient peel strength with respect to an insulating resin base material that cannot be expected to be chemically adhered, such as a liquid crystal polymer film, and can therefore be inferior in reliability as a flexible printed wiring board.
  • transmission loss and peel strength are in a trade-off relationship with the surface profile of the copper foil, it is inherently difficult to achieve both.
  • the inventors of the present invention now have a ten-point average roughness Rzjis of 0.6 to 1.7 ⁇ m, and a roughening whose half-value width in the frequency distribution of the height of the roughening particles is 0.9 ⁇ m or less.
  • an object of the present invention is to provide a copper foil that can exhibit high peel strength even with respect to an insulating resin base material that cannot be expected to be chemically adhered, such as a liquid crystal polymer film, while having good transmission loss in high frequency applications. It is to provide.
  • a roughened copper foil having a roughened surface provided with roughened particles on at least one side, wherein the roughened surface is 0.6 to 1.7 ⁇ m.
  • a roughened copper foil having a point average roughness Rzjis and having a half-value width of 0.9 ⁇ m or less in the frequency distribution of the height of the roughened particles is provided.
  • a printed wiring for high-frequency applications comprising the roughened copper foil of the above aspect and an insulating resin layer provided in close contact with the roughened surface of the copper foil.
  • a board is provided.
  • ten-point average roughness Rzjis is a surface roughness measured in accordance with JIS B0601-2001, and is an average of the peak heights from the highest peak to the fifth highest in the roughness curve. , The average sum up to the fifth deepest from the deepest valley bottom.
  • the “half-value width in the frequency distribution of the height of the roughened particles” is shown in FIG. 1 in the frequency distribution of the height of the roughened particles existing on the roughened surface of the roughened copper foil.
  • it is defined as the full width of the frequency distribution peak at a value 1 ⁇ 2 of the maximum value of the frequency distribution peak.
  • the frequency distribution of the height of the roughened particles is obtained by using a three-dimensional roughness analyzer to obtain a desired magnification according to the size of the roughened particles (for example, 600 to 600). (30000 times).
  • the height of the roughened particles can be regarded as the particle size of the roughened particles.
  • the surface profile of the electrolytic copper foil (raw foil) before the roughening treatment is measured in advance, and the value resulting from the surface profile before the roughening treatment is calculated. Sometimes it is desirable to do so by removing as background.
  • the “specific surface area” is a value of X / Y obtained by dividing the three-dimensional surface area X of the roughened surface of the roughened copper foil by the measurement area Y.
  • the three-dimensional surface area X can be calculated by measuring a surface profile of a predetermined measurement area Y (for example, 14000 ⁇ m 2 ) of the roughened surface with a commercially available laser microscope.
  • the “roughened particle cross-sectional area ratio” is an index representing the degree of unevenness of the roughened particle surface (that is, the degree of fine roughening), and is a commercially available image processing analyzer and a commercially available focused ion beam processing observation.
  • FIB FIB SIM image
  • the FIB-SIM image is subjected to image analysis to measure the closed cross-sectional area and cross-sectional area, and the ratio of (closed cross-sectional area of roughened particles) / (cross-sectional area of roughened particles) is measured. It is a value determined by calculating the fractional particle cross-sectional area ratio.
  • the specific measurement procedure is as follows.
  • a straight line is drawn from the approximately bisected position of the head of the roughened particle to the long side direction of the roughened particle (that is, the height direction of the roughened particle).
  • the reference point a is specified at a position away from the top of the roughened particles on the straight line by a predetermined distance (for example, 2 ⁇ m).
  • Two tangent lines are drawn from the reference point a to the roughened particles, and the contact points b and c between the tangent lines and the roughened particles are specified.
  • a cross-sectional area of a cross-sectional area surrounded by a straight line connecting the contact points b and c (hereinafter referred to as a bc straight line) and a cross-sectional contour line of the head of the roughened particle is obtained by image analysis.
  • a bc straight line A cross-sectional area of a cross-sectional area surrounded by a straight line connecting the contact points b and c
  • a cross-sectional contour line of the head of the roughened particle is obtained by image analysis.
  • the closed curved cross-sectional area of the roughened particles is obtained as a value larger than the cross-sectional area of the roughened particles according to the degree of unevenness on the surface of the roughened particles (ie, the degree of fine roughening). Accordingly, by dividing the closed curved cross-sectional area of the roughened particles by the cross-sectional area of the roughened particles, a numerical value representing the degree of unevenness (that is, the degree of fine roughening) on the surface of the roughened particles can be obtained. That is, the roughened particle cross-sectional area ratio is calculated from the obtained closed curved cross-sectional area and the cross-sectional area of the roughened particles. The rough particle cross-sectional area ratio is calculated for each rough particle observed for each field of view, and the average value of the rough particle cross-sectional area ratios obtained for all the rough particles for five fields of view is calculated. Is preferred.
  • the copper foil of the present invention is a roughened copper foil.
  • This roughened copper foil has a roughened surface with roughened particles on at least one side.
  • the roughened surface has a 10-point average roughness Rzjis of 0.6 to 1.7 ⁇ m, and the half width in the frequency distribution of the height of the roughened particles is 0.9 ⁇ m or less.
  • a roughened surface having a 10-point average roughness Rzjis of 0.6 to 1.7 ⁇ m and a half-value width in the frequency distribution of the height of the roughened particles being 0.9 ⁇ m or less is made of copper foil.
  • the mechanism that makes it possible to achieve both good transmission loss and high peel strength is not necessarily clear, but is thought to be as follows.
  • the ten-point average roughness Rzjis of the roughened surface is set to a low value range of 0.6 to 1.7 ⁇ m, thereby significantly reducing the skin effect of copper foil in high frequency applications and reducing conductor loss.
  • transmission loss can be reduced.
  • the above-mentioned 10-point average roughness Rzjis of 0.6 to 1.7 ⁇ m is a low value, and by itself, adhesion with an insulating resin base material, such as a liquid crystal polymer film, that cannot be expected to be chemically adhered is poor. Can be enough.
  • the adhesion strength becomes unstable when the height of the roughened particles varies.
  • the variation in the height of the roughened particles is reduced by setting the half-value width in the frequency distribution of the height of the roughened particles to 0.9 ⁇ m or less.
  • the roughened particles can contribute to the improvement of adhesion, and thereby the adhesion strength can be stabilized. As a result, it becomes possible to exhibit high peel strength (for example, 1.2 kgf / cm or more with a copper foil having a thickness of 18 ⁇ m) even for an insulating resin base material such as a liquid crystal polymer film that cannot be expected to have chemical adhesion.
  • the ten-point average roughness Rzjis (measured according to JIS B0601-2001) of the roughened surface is 0.6 to 1.7 ⁇ m, preferably 0.7 to 1.6 ⁇ m, more preferably Is 0.9 to 1.5 ⁇ m. Rzjis within these ranges can desirably reduce transmission loss in high frequency applications and contribute to securing adhesion to the insulating resin substrate.
  • the half width in the frequency distribution of the height of the roughened particles is 0.9 ⁇ m or less, preferably 0.2 to 0.9 ⁇ m, more preferably 0.2 to 0.7 ⁇ m, and still more preferably 0.2 to 0.6 ⁇ m.
  • the half-value width is within these ranges, the variation in the height of the roughened particles can be reduced, and more roughened particles can contribute to improving the adhesion, thereby stabilizing the adhesion strength.
  • the roughened copper foil further comprises fine roughened particles that are finer than the roughened particles on the roughened particles.
  • fine roughened particles By forming fine roughened particles on the roughened particles and increasing the surface area, the peel strength can be further improved. Nevertheless, since the particle size of the finely roughened particles is extremely small, typically 150 nm or less, the influence on the transmission loss is extremely low in the frequency band of 100 GHz or less.
  • the roughened surface preferably has a specific surface area of 1.1 to 2.1, more preferably 1.2 to 2.0, still more preferably 1.3 to 1.9, particularly preferably. 1.5 to 1.9.
  • the specific surface area is a value of X / Y obtained by dividing the three-dimensional surface area X of the roughened surface by the measurement area Y.
  • the specific surface area is appropriately large as 1.1 or more, the peel strength with respect to the insulating resin substrate can be improved.
  • the specific surface area is not too large as 2.1 or less, it is possible to suppress peeling of the roughened particles (so-called powder falling) due to physical contact that may occur when the specific surface area is too large. It is possible to effectively avoid a decrease in peel strength and contamination in the subsequent process.
  • the roughened surface preferably has a roughened particle cross-sectional area ratio of 1.10 to 1.50, more preferably 1.15 to 1.30, and even more preferably 1.15 to 1.20. .
  • the roughened particle cross-sectional area ratio is an index representing the degree of unevenness of the roughened particle surface (that is, the degree of fine roughening). Therefore, the larger the protrusion on the roughened particle, the larger the value of the cross-sectional area ratio of the roughened particle. Therefore, when the roughened surface is bonded to the insulating resin base material, the contact area with the insulating resin base material is large. As a result, the physical adhesion is increased as compared with the roughened particles alone (that is, when there are no finely roughened particles).
  • the rough particle cross-sectional area ratio is 1.15 or more
  • the physical adhesion of the rough particles can be effectively increased.
  • the roughened particle cross-sectional area ratio is 1.50 or less, it is possible to suppress peeling of fine roughened particles (so-called powder falling) due to physical contact that may occur when the specific surface area is too large. As a result, it is possible to effectively avoid a decrease in peel strength and contamination in the subsequent process.
  • the thickness of the roughened copper foil of the present invention is not particularly limited, but is preferably 0.1 to 35 ⁇ m, more preferably 0.5 to 18 ⁇ m.
  • the roughening copper foil of this invention performed the roughening process or the fine roughening process of the copper foil surface not only what performed the roughening process on the surface of the normal copper foil but the copper foil with a carrier. It may be a thing.
  • the roughened copper foil of the present invention is preferably used for a printed wiring board for high frequency applications. That is, according to a preferred aspect of the present invention, there is provided a printed wiring board for high frequency applications, comprising the roughened copper foil of the present invention and an insulating resin layer provided in close contact with the roughened surface of the copper foil. Provided.
  • the roughened copper foil of the present invention has good transmission loss in high-frequency applications, but against insulating resin substrates that cannot be expected to be chemically adhered, such as liquid crystal polymer films. However, it is possible to exhibit high peel strength (for example, 1.2 kgf / cm or more with a 18 ⁇ m thick copper foil).
  • the insulating resin layer preferably includes a liquid crystal polymer (LCP), for example, a liquid crystal polymer (LCP) film.
  • LCP liquid crystal polymer
  • Preferred examples of high frequency applications include high frequency components mounted on portable electronic devices such as smartphones, such as liquid crystal display modules, camera modules, and antenna modules.
  • the preferred manufacturing method comprises the steps of ten-point average roughness Rzjis is prepared copper foil having the surface 1.5 [mu] m, the first crude performing electrolytic deposition at a predetermined current density J 1 to said surface step a, roughening performed a second roughened step of performing electrolytic deposition at a predetermined current density J 2 relative to the surface, the electrolytic deposition at a predetermined current density J 3 relative to the surface
  • a third roughening step for forming a treatment surface, and preferably a ratio of current densities J 1 , J 2 and J 3 in the first roughening step, the second roughening step and the third roughening step ( That is, J 1 : J 2 : J 3 ) is set within the range of 1.0: 1.4: 1.2 to 1.0: 1.6: 1.5.
  • the roughened copper foil according to the present invention is not limited to the method described below, and may be manufactured by any method.
  • the copper foil As copper foil used for manufacture of a roughening process copper foil, use of both electrolytic copper foil and rolled copper foil is possible, More preferably, it is electrolytic copper foil. Further, the copper foil may be a non-roughened copper foil or a pre-roughened copper foil. The thickness of the copper foil is not particularly limited, but is preferably 0.1 to 35 ⁇ m, more preferably 0.5 to 18 ⁇ m. When the copper foil is prepared in the form of a copper foil with a carrier, the copper foil is prepared by a wet film formation method such as an electroless copper plating method and an electrolytic copper plating method, a dry film formation method such as sputtering and chemical vapor deposition, or It may be formed by a combination thereof.
  • a wet film formation method such as an electroless copper plating method and an electrolytic copper plating method
  • a dry film formation method such as sputtering and chemical vapor deposition
  • the surface of the copper foil to be roughened preferably has a surface with a ten-point average roughness Rzjis measured in accordance with JIS B0601-2001 of 1.5 ⁇ m or less, more preferably 1. It is 3 ⁇ m or less, more preferably 1.0 ⁇ m or less. Although a lower limit is not specifically limited, For example, it is 0.1 micrometer or more. Within the above range, the surface profile required for the roughened copper foil of the present invention, in particular, the 10-point average roughness Rzjis of 0.6 to 1.7 ⁇ m can be easily imparted to the roughened surface.
  • (1) Roughening treatment It is preferable to perform a three-step roughening step, a first roughening step, a second roughening step, and a third roughening step, on the surface of the copper foil having Rzjis of 1.5 ⁇ m or less.
  • electrolytic deposition is performed at a predetermined current density J 1 at a temperature of 20 to 40 ° C. in a copper sulfate solution containing a copper concentration of 8 to 12 g / L and a sulfuric acid concentration of 200 to 280 g / L.
  • this electrolytic deposition is performed for 5 to 20 seconds.
  • electrolytic deposition is performed at a predetermined current density J 2 at a temperature of 20 to 40 ° C. in a copper sulfate solution containing a copper concentration of 8 to 12 g / L and a sulfuric acid concentration of 200 to 280 g / L. Preferably, this electrolytic deposition is performed for 5 to 20 seconds.
  • electrolytic deposition is performed at a predetermined current density J 3 at a temperature of 45 to 55 ° C. in a copper sulfate solution containing a copper concentration of 65 to 80 g / L and a sulfuric acid concentration of 200 to 280 g / L.
  • a roughened surface is preferably formed, and this electrolytic deposition is preferably performed for 5 to 25 seconds.
  • the first roughening step, the second coarse step and the third ratio roughening current density J 1 in step J 2 and J 3, i.e. J 1: J 2: J 3 1.0: 1.4 : 1.2 to 1.0: 1.6: 1.5 is preferable.
  • the current density ratio is within this range, the surface profile required for the roughened copper foil of the present invention, particularly the half-value width in the frequency distribution of the height of the roughened particles of 0.9 ⁇ m or less on the roughened surface. It becomes easy to give.
  • the current density J 1 in the first roughening step is 8 to 20 A / dm 2
  • the current density J 2 in the second roughening step is 12 to 32 A / dm 2
  • the current in the third roughening step The density J 3 is 10 to 30 A / dm 2 .
  • Fine roughening treatment It is preferable that the fine roughening treatment is further performed on the roughening treatment surface formed in the third roughening step.
  • the fine roughening treatment is performed at 20 to 40 ° C. in a copper sulfate solution having a copper concentration of 10 to 20 g / L, a sulfuric acid concentration of 30 to 130 g / L, a 9-phenylacridine concentration of 100 to 200 mg / L, and a chlorine concentration of 20 to 100 mg / L. It is preferable to carry out the electrolytic deposition of fine copper particles at a current density of 10 to 40 A / dm 2 at this temperature, and this electrolytic deposition is preferably carried out for 0.3 to 1.0 seconds.
  • the copper foil after the roughening treatment may be subjected to a rust prevention treatment.
  • the rust prevention treatment preferably includes a plating treatment using zinc.
  • the plating treatment using zinc may be either a zinc plating treatment or a zinc alloy plating treatment, and the zinc alloy plating treatment is particularly preferably a zinc-nickel alloy treatment.
  • the zinc-nickel alloy treatment may be a plating treatment containing at least Ni and Zn, and may further contain other elements such as Sn, Cr, and Co.
  • the Ni / Zn adhesion ratio in the zinc-nickel alloy plating is preferably 1.2 to 10, more preferably 2 to 7, and still more preferably 2.7 to 4 in terms of mass ratio.
  • the rust prevention treatment preferably further includes a chromate treatment, and this chromate treatment is more preferably performed on the surface of the plating containing zinc after the plating treatment using zinc.
  • rust prevention property can further be improved.
  • a particularly preferable antirust treatment is a combination of a zinc-nickel alloy plating treatment and a subsequent chromate treatment.
  • the copper foil may be treated with a silane coupling agent to form a silane coupling agent layer.
  • a silane coupling agent layer can be formed by appropriately diluting and applying a silane coupling agent and drying.
  • silane coupling agents include epoxy-functional silane coupling agents such as 4-glycidylbutyltrimethoxysilane and 3-glycidoxypropyltrimethoxysilane, or 3-aminopropyltriethoxysilane, N-2 (amino Amino functions such as ethyl) 3-aminopropyltrimethoxysilane, N-3- (4- (3-aminopropoxy) butoxy) propyl-3-aminopropyltrimethoxysilane, N-phenyl-3-aminopropyltrimethoxysilane Silane coupling agents, or mercapto-functional silane coupling agents such as 3-mercaptopropyltrimethoxysilane, or olefin-functional silane coupling agents such as vinyltrimethoxysilane and vinylphenyltrimethoxysilane, or 3-methacryloxypropyl Trime Acrylic-functional silane coupling agent such as Kishishiran, or imid
  • the roughened copper foil of the present invention may be provided in the form of a copper foil with carrier.
  • the carrier-attached copper foil includes a carrier, a release layer provided on the carrier, and the roughened copper foil of the present invention provided on the release layer with the roughened treatment surface outside. It becomes.
  • a known layer structure can be adopted as the carrier-attached copper foil except that the roughened copper foil of the present invention is used.
  • the carrier is a foil-like or layer-like member for supporting the roughened copper foil and improving its handleability.
  • the carrier include an aluminum foil, a copper foil, a resin film whose surface is metal-coated, and the like, preferably a copper foil.
  • the copper foil may be a rolled copper foil or an electrolytic copper foil.
  • the thickness of the carrier is typically 200 ⁇ m or less, preferably 12 ⁇ m to 70 ⁇ m.
  • the release layer is a layer having a function of weakening the peeling strength of the carrier, ensuring the stability of the strength, and further suppressing the interdiffusion that may occur between the carrier and the copper foil during press molding at a high temperature. .
  • the release layer is generally formed on one side of the carrier, but may be formed on both sides.
  • the release layer may be either an organic release layer or an inorganic release layer. Examples of organic components used in the organic release layer include nitrogen-containing organic compounds, sulfur-containing organic compounds, carboxylic acids and the like. Examples of nitrogen-containing organic compounds include triazole compounds, imidazole compounds, and the like. Among these, triazole compounds are preferred in terms of easy release stability.
  • triazole compounds examples include 1,2,3-benzotriazole, carboxybenzotriazole, N ′, N′-bis (benzotriazolylmethyl) urea, 1H-1,2,4-triazole and 3-amino- And 1H-1,2,4-triazole.
  • sulfur-containing organic compound examples include mercaptobenzothiazole, thiocyanuric acid, 2-benzimidazolethiol and the like.
  • carboxylic acid examples include monocarboxylic acid and dicarboxylic acid.
  • examples of inorganic components used in the inorganic release layer include Ni, Mo, Co, Cr, Fe, Ti, W, P, Zn, and a chromate-treated film.
  • the release layer may be formed by bringing a release layer component-containing solution into contact with at least one surface of the carrier and fixing the release layer component to the surface of the carrier.
  • the carrier may be brought into contact with the release layer component-containing solution by immersion in the release layer component-containing solution, spraying of the release layer component-containing solution, flowing down of the release layer component-containing solution, or the like.
  • the release layer component may be fixed to the carrier surface by adsorption or drying of the release layer component-containing solution, electrodeposition of the release layer component in the release layer component-containing solution, or the like.
  • the thickness of the release layer is typically 1 nm to 1 ⁇ m, preferably 5 nm to 500 nm.
  • the roughened copper foil of the present invention described above is used as the roughened copper foil.
  • the roughened copper foil of the present invention has been subjected to a roughening treatment, or a roughening treatment and a fine roughening treatment, but as a procedure, first, a copper layer is formed on the surface of the release layer as a copper foil, Thereafter, at least roughening treatment and / or fine roughening treatment may be performed. Details of the roughening treatment and the fine roughening treatment are as described above.
  • copper foil is comprised with the form of an ultra-thin copper foil in order to utilize the advantage as copper foil with a carrier.
  • a preferable thickness of the ultrathin copper foil is 0.1 ⁇ m to 7 ⁇ m, more preferably 0.5 ⁇ m to 5 ⁇ m, and still more preferably 0.5 ⁇ m to 3 ⁇ m.
  • auxiliary metal layer is preferably made of nickel and / or cobalt.
  • the thickness of the auxiliary metal layer is preferably 0.001 to 3 ⁇ m.
  • the roughening treatment was performed in the following three stages on the precipitation surface side of the electrode surface and the precipitation surface included in the electrolytic copper foil.
  • the first stage of the roughening treatment is a copper electrolytic solution for roughening treatment (copper concentration: 10.8 g / L, sulfuric acid concentration: 240 g / L, 9-phenylacridine concentration: 0 mg / L, chlorine concentration: 0 mg / L ), Electrolysis was performed under the conditions shown in Table 1A, followed by washing with water.
  • the second stage of the roughening treatment is a copper electrolytic solution for roughening treatment (copper concentration: 10.8 g / L, sulfuric acid concentration: 240 g / L, 9-phenylacridine concentration: 0 mg / L, chlorine concentration: 0 mg / L ), Electrolysis was performed under the conditions shown in Table 1A, followed by washing with water.
  • the third stage of the roughening treatment is in a copper electrolytic solution for roughening treatment (copper concentration: 70 g / L, sulfuric acid concentration: 240 g / L, 9-phenylacridine concentration: 0 mg / L, chlorine concentration: 0 mg / L) The electrolysis was performed under the conditions shown in Table 1A, followed by washing with water.
  • Fine roughening treatment A fine roughening treatment was performed by electrolysis under the conditions shown in Table 1. The fine roughening treatment is performed in Table 1B in a copper electrolytic solution for roughening treatment (copper concentration: 13 g / L, sulfuric acid concentration: 70 g / L, 9-phenylacridine concentration: 140 mg / L, chlorine concentration: 35 mg / L). It was carried out by electrolyzing under the indicated conditions and washing with water.
  • Rust prevention treatment consisting of inorganic rust prevention treatment and chromate treatment was performed on both surfaces of the electrolytic copper foil after the fine roughening treatment.
  • an inorganic rust prevention treatment using a pyrophosphate bath, potassium pyrophosphate concentration 80 g / L, zinc concentration 0.2 g / L, nickel concentration 2 g / L, liquid temperature 40 ° C., current density 0.5 A / dm 2 Zinc-nickel alloy rust prevention treatment was performed.
  • a chromate treatment a chromate layer was further formed on the zinc-nickel alloy rust preventive treatment. This chromate treatment was performed at a chromic acid concentration of 1 g / L, pH 11, a solution temperature of 25 ° C., and a current density of 1 A / dm 2 .
  • Silane coupling agent treatment The copper foil that has been subjected to the above rust prevention treatment is washed with water and then immediately treated with a silane coupling agent to adsorb the silane coupling agent on the rust prevention treatment layer of the roughened surface. It was.
  • this silane coupling agent treatment pure water is used as a solvent, a solution having a 3-aminopropyltrimethoxysilane concentration of 3 g / L is used, and this solution is sprayed onto the roughened surface by showering to perform an adsorption treatment. went. After adsorption of the silane coupling agent, water was finally evaporated by an electric heater to obtain a roughened copper foil having a thickness of 18 ⁇ m.
  • Example 4 A roughened copper foil was produced in the same manner as in Example 1 except that i) the fine roughening treatment was omitted, and ii) the roughening treatment was performed under the conditions shown in Table 1A.
  • Example 5 (Comparison) i) The surface of the electrolytic copper foil (that is, the side opposite to the deposition surface, Rzjis: 1.5 ⁇ m) was subjected to a treatment such as a roughening treatment, and ii) The roughening treatment and the fine roughening treatment were performed in Table 1A. And the roughened copper foil was produced like Example 1 except having performed according to the conditions shown by 1B.
  • Example 6 (Comparison) i) Roughing was performed in the same manner as in Example 1 except that the following one-step roughening treatment was performed instead of the first, second and third roughening steps, and ii) the fine roughening treatment was omitted.
  • the copper foil was prepared.
  • a copper electrolytic solution for roughening treatment having the following composition is used for the deposition surface side, a solution temperature of 30 ° C., a current density of 50 A / dm 2 , Roughening was performed by electrolysis under conditions of time 4 seconds.
  • Example 7 (Comparison) i) The surface of the electrolytic copper foil (that is, the side opposite to the deposition surface, Rzjis: 1.5 ⁇ m) was subjected to a treatment such as a roughening treatment, ii) the fine roughening treatment was omitted, and iii) A roughened copper foil was produced in the same manner as in Example 1 except that the roughening treatment was performed under the conditions shown in Table 1A.
  • Example 8 (Comparison) i) The electrode surface side of the electrolytic copper foil (that is, the side opposite to the deposition surface side, Rzjis: 1.5 ⁇ m) was subjected to a treatment such as a roughening treatment, ii) the second roughening step and the fine roughening treatment were omitted. And iii) Preparation of a roughened copper foil in the same manner as in Example 1 except that the roughening treatment (that is, the first roughening step and the third roughening step) was performed under the conditions shown in Table 1A. Went.
  • ⁇ 10-point average roughness Rzjis> The ten-point average roughness Rzjis of the roughened copper foil was measured with a contact surface roughness meter (Kosaka Laboratory, SE3500) in accordance with JIS B0601-2001. This measurement was performed using a diamond ball having a diameter of 2 ⁇ m as a stylus and a reference length of 0.8 mm.
  • the measurement of Rzjis of the deposition surface or electrode surface of the electrolytic copper foil before the roughening treatment in each of the examples described above was also performed in the same procedure as described above.
  • ⁇ Half width in the frequency distribution of the height of the roughened particles> The surface profile of the roughened copper foil was measured with a three-dimensional roughness analyzer (manufactured by Elionix Co., Ltd., ERA-8900) under conditions of a magnification of 600 to 30000 times and an acceleration voltage of 10 kV. The measurement magnification was adjusted within the above range according to the size of the coarse particles. The particle size was calculated based on the measured surface profile. At that time, the height of the roughened particles measured at intervals of 0.01 ⁇ m in the z-axis (foil thickness direction) interval was regarded as the particle size.
  • the surface profile of the electrolytic copper foil (raw foil) before the roughening treatment is measured in advance, and the value resulting from the surface profile before the roughening treatment is calculated. Sometimes done by removing as background. A frequency distribution of the height of the roughened particles based on the height or particle size calculated in this way is created, and the full width of the frequency distribution peak at half the maximum value of the frequency distribution peak as shown in FIG. It calculated as a value range (micrometer).
  • ⁇ Roughening surface specific surface area The surface profile of a region (100 ⁇ m ⁇ 140 ⁇ m) having an area of 14000 ⁇ m 2 on the roughened surface of the roughened copper foil was measured using a laser microscope (manufactured by Keyence Corporation, VK-X100) at a magnification of 2000 times. A three-dimensional surface area X ( ⁇ m 2 ) of the surface profile of the obtained roughened surface was calculated, and a value X / Y obtained by dividing the value of X by a measurement area Y (14000 ⁇ m 2 ) was defined as a specific surface area.
  • ⁇ Peel strength> As an insulating resin substrate, a liquid crystal polymer (LCP) film (Vecstar CTZ manufactured by Kuraray Co., Ltd.) having a thickness of 50 ⁇ m was prepared. Laminated copper foil is laminated on this insulating resin base material so that the roughened surface is in contact with the insulating resin base material, and hot press molding is performed at a pressure of 4 MPa and a temperature of 310 ° C. for 10 minutes to form a copper-clad laminate. A plate sample was prepared. The copper-clad laminate sample was peeled in the direction of 90 ° with respect to the surface of the insulating resin substrate in accordance with JIS C 5016-1994, Method A, and the normal peel strength (kgf / cm) was measured.
  • LCP liquid crystal polymer
  • ⁇ Roughened particle cross-sectional area ratio The ratio of the roughened particle cross-sectional area on the roughened surface of the roughened copper foil was measured. This measurement is performed using a desktop automatic multifunctional image processing analyzer (manufactured by Nireco Corporation, LUZEX AP) and a focused ion beam processing observation apparatus (FIB), and a predetermined visual field range (8 ⁇ m ⁇ 8 ⁇ m) of the roughened surface. ) By observing the cross-section of each roughened particle and obtaining a FIB SIM image (hereinafter referred to as FIB-SIM image) at a magnification of 18000 times.
  • FIB-SIM image a FIB SIM image
  • the area was measured, and the ratio of the roughened particle cross-sectional area was calculated as the ratio of (closed curved cross-sectional area of the roughened particles) / (cross-sectional area of the roughened particles).
  • the binarization setting in this image analysis was set to 127. The specific procedure was as follows.
  • the reason why the distance from the top of the roughened particles is set to 2 ⁇ m in determining the reference point a is that the length of the scale of the FIB-SIM image is 2 ⁇ m, which is such a length. This is because, even if the position of the reference point a fluctuates somewhat, the positions of the contacts b and c are identified almost uniquely, so that the value of the cross-sectional area of the roughened particles can be obtained with high accuracy.
  • FIG. 3 illustrates an enlarged image of the head of roughened particles.
  • the closed curved cross-sectional area of the roughened particles is determined by measuring the tips of the fine convex shapes on the surface of the roughened particles (if fine roughened particles exist, The area of the region surrounded by the line connecting each tip) and the bc line was defined, and this was determined by image analysis. The positioning of each tip was automatically performed by software included in the image processing analyzer.
  • the roughened particle cross-sectional area ratio was calculated from the obtained closed curved cross-sectional area and the cross-sectional area of the roughened particles.
  • the roughened particle cross-sectional area ratio was applied to each roughened particle observed for each visual field, and the average value of the roughened particle cross-sectional area ratios obtained for all the roughened particles for five visual fields was calculated.
  • a liquid crystal polymer (LCP) film (Vecstar CTZ manufactured by Kuraray Co., Ltd.) having a thickness of 50 ⁇ m was prepared.
  • a roughened copper foil was laminated on both surfaces of the insulating resin base material so that the roughened surface was in contact with the insulating resin base material, and was bonded together by a batch press.
  • only the roughened copper foil on one side of the insulating resin base material 40 is etched to form a microstrip line so that the characteristic impedance is 50 ⁇ to form the signal layer 42 (thickness 18 ⁇ m). ).
  • the roughened copper foil on the opposite side of the signal layer 42 of the insulating resin substrate 40 was not etched, and was used as a ground layer 44 (thickness 18 ⁇ m).
  • a sample for transmission loss measurement was obtained by laminating as a ray 46.
  • the obtained sample microstrip line is subjected to a transmission loss S of 40 GHz at a circuit length of 5 cm using a network analyzer (N5247A, Keysight Technology, Inc.) and a prober system (SUMMIT 9000, Cascade Microtech). 21 was obtained.

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Abstract

L'invention concerne une feuille de cuivre qui peut présenter une résistance élevée au pelage sur des substrats en résine isolante avec lesquels on n'attend pas de liaison chimique, par exemple des films polymères à cristaux liquides, tout en présentant une bonne perte de transmission dans des applications haute fréquence. Ladite feuille de cuivre rugueuse présente une surface ayant des particules rugueuses sur au moins un côté de feuille, la surface rugueuse a une rugosité moyenne sur dix points Rzjis de 0,6 à 1,7 μm et la largeur à la valeur médiane est de 0,9 µm dans une courbe de distribution de la hauteur des particules rugueuses.
PCT/JP2016/061127 2015-04-28 2016-04-05 Feuille de cuivre rugueuse et carte de câblage imprimée WO2016174998A1 (fr)

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JP2021001398A (ja) * 2019-06-19 2021-01-07 金居開發股▲分▼有限公司 ミクロ粗面化した電着銅箔及び銅張積層板
JP2021021137A (ja) * 2019-06-19 2021-02-18 金居開發股▲分▼有限公司 長尺島状の微細構造を有するアドバンスト電解銅箔及びそれを適用した銅張積層板
JPWO2019188712A1 (ja) * 2018-03-27 2021-04-22 三井金属鉱業株式会社 粗化処理銅箔、キャリア付銅箔、銅張積層板及びプリント配線板
US11332839B2 (en) 2019-06-19 2022-05-17 Co-Tech Development Corp. Advanced electrodeposited copper foil and copper clad laminate using the same
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KR20200073051A (ko) 2018-12-13 2020-06-23 엘지이노텍 주식회사 인쇄회로기판
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WO2018198905A1 (fr) * 2017-04-25 2018-11-01 古河電気工業株式会社 Feuille de cuivre traitée en surface
CN110382745B (zh) * 2017-05-19 2021-06-25 三井金属矿业株式会社 粗糙化处理铜箔、带载体铜箔、覆铜层叠板及印刷电路板
WO2018211951A1 (fr) * 2017-05-19 2018-11-22 三井金属鉱業株式会社 Feuille de cuivre rugosifiée, feuille de cuivre fixée à un support, stratifié plaqué cuivre et carte de circuits imprimés
JP6430092B1 (ja) * 2017-05-19 2018-11-28 三井金属鉱業株式会社 粗化処理銅箔、キャリア付銅箔、銅張積層板及びプリント配線板
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KR102297790B1 (ko) 2017-05-19 2021-09-06 미쓰이금속광업주식회사 조화 처리 구리박, 캐리어를 구비한 구리박, 동장 적층판 및 프린트 배선판
JP2020509224A (ja) * 2017-07-31 2020-03-26 サーキット フォイル ルクセンブルグ エス．エイ．アール．エル．Ｃｉｒｃｕｉｔ Ｆｏｉｌ Ｌｕｘｅｍｂｏｕｒｇ Ｓ．Ａ．Ｒ．Ｌ． 表面処理銅箔および銅張積層基板
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JP7166335B2 (ja) 2018-03-27 2022-11-07 三井金属鉱業株式会社 粗化処理銅箔、キャリア付銅箔、銅張積層板及びプリント配線板
JPWO2019188712A1 (ja) * 2018-03-27 2021-04-22 三井金属鉱業株式会社 粗化処理銅箔、キャリア付銅箔、銅張積層板及びプリント配線板
JP7146274B2 (ja) 2018-09-26 2022-10-04 金居開發股▲分▼有限公司 微小粗面化電解銅箔及び銅箔基板
US11047061B2 (en) 2018-09-26 2021-06-29 Co-Tech Development Corp. Micro-roughened electrodeposited copper foil and copper foil substrate
JP2020050954A (ja) * 2018-09-26 2020-04-02 金居開發股▲分▼有限公司 微小粗面化電解銅箔及び銅箔基板
JP7325022B2 (ja) 2019-02-04 2023-08-14 パナソニックＩｐマネジメント株式会社 銅張積層板、樹脂付銅箔、および、それらを用いた回路基板
JPWO2020162056A1 (fr) * 2019-02-04 2020-08-13
WO2020162056A1 (fr) * 2019-02-04 2020-08-13 パナソニックＩｐマネジメント株式会社 Plaque stratifiée revêtue de cuivre, feuille de cuivre fixée à une résine, et carte de circuit imprimé l'utilisant
WO2020230870A1 (fr) * 2019-05-15 2020-11-19 パナソニックＩｐマネジメント株式会社 Plaque stratifiée plaquée de cuivre, feuille de cuivre plaquée de résine et substrat de circuit utilisant ladite plaque et ladite feuille
JP2021001398A (ja) * 2019-06-19 2021-01-07 金居開發股▲分▼有限公司 ミクロ粗面化した電着銅箔及び銅張積層板
US11408087B2 (en) 2019-06-19 2022-08-09 Co-Tech Development Corp. Advanced electrodeposited copper foil having island-shaped microstructures and copper clad laminate using the same
TWI776168B (zh) * 2019-06-19 2022-09-01 金居開發股份有限公司 進階反轉電解銅箔及應用其的銅箔基板
US11332839B2 (en) 2019-06-19 2022-05-17 Co-Tech Development Corp. Advanced electrodeposited copper foil and copper clad laminate using the same
JP2021021137A (ja) * 2019-06-19 2021-02-18 金居開發股▲分▼有限公司 長尺島状の微細構造を有するアドバンスト電解銅箔及びそれを適用した銅張積層板
CN112118672A (zh) * 2019-06-19 2020-12-22 金居开发股份有限公司 具有长岛状微结构的进阶反转电解铜箔及应用其的铜箔基板
KR20230159392A (ko) 2021-03-26 2023-11-21 미쓰이금속광업주식회사 조화 처리 구리박, 캐리어를 구비한 구리박, 동장 적층판 및 프린트 배선판
KR20230160813A (ko) 2021-03-26 2023-11-24 미쓰이금속광업주식회사 조화 처리 구리박, 캐리어를 구비한 구리박, 동장 적층판 및 프린트 배선판

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TWI588302B (zh) 2017-06-21
TW201706457A (zh) 2017-02-16
KR20170107040A (ko) 2017-09-22
CN107532322B (zh) 2019-07-16
JP6682516B2 (ja) 2020-04-15
CN107532322A (zh) 2018-01-02

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