WO2022244826A1 - Feuille de cuivre rugosifiée, feuille de cuivre comprenant un support, carte stratifiée plaquée de cuivre et carte de circuit imprimé - Google Patents

Feuille de cuivre rugosifiée, feuille de cuivre comprenant un support, carte stratifiée plaquée de cuivre et carte de circuit imprimé Download PDF

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Publication number
WO2022244826A1
WO2022244826A1 PCT/JP2022/020747 JP2022020747W WO2022244826A1 WO 2022244826 A1 WO2022244826 A1 WO 2022244826A1 JP 2022020747 W JP2022020747 W JP 2022020747W WO 2022244826 A1 WO2022244826 A1 WO 2022244826A1
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Prior art keywords
copper foil
roughened
peaks
valleys
carrier
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PCT/JP2022/020747
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English (en)
Japanese (ja)
Inventor
沙織 小出
眞 細川
美穂 栗原
知里 田坂
綾子 四井
美智 溝口
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三井金属鉱業株式会社
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Priority to JP2023522710A priority Critical patent/JPWO2022244826A1/ja
Priority to KR1020237038900A priority patent/KR20240009403A/ko
Priority to CN202280035616.5A priority patent/CN117321253A/zh
Publication of WO2022244826A1 publication Critical patent/WO2022244826A1/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
    • C25D1/00—Electroforming
    • C25D1/04—Wires; Strips; Foils
    • C—CHEMISTRY; METALLURGY
    • C25—ELECTROLYTIC OR ELECTROPHORETIC PROCESSES; APPARATUS THEREFOR
    • C25D—PROCESSES FOR THE ELECTROLYTIC OR ELECTROPHORETIC PRODUCTION OF COATINGS; ELECTROFORMING; APPARATUS THEREFOR
    • C25D3/00—Electroplating: Baths therefor
    • C25D3/02—Electroplating: Baths therefor from solutions
    • C25D3/38—Electroplating: Baths therefor from solutions of copper
    • 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
    • C25D5/16—Electroplating with layers of varying thickness
    • 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
    • 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
    • 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
    • H05K3/46—Manufacturing multilayer circuits

Definitions

  • the present invention relates to a roughened copper foil, a copper foil with a carrier, a copper-clad laminate, and a printed wiring board.
  • the MSAP method is a technique suitable for forming extremely fine circuits, and is carried out using a copper foil with a carrier in order to take advantage of its characteristics. For example, as shown in FIGS. 1 and 2, an ultra-thin copper foil (roughened copper foil 10) is placed on an insulating resin substrate 11 having a lower layer circuit 11b on a base substrate 11a, and a prepreg 12 and a primer layer 13 are formed thereon. (step (a)), peel off the carrier (not shown), and then form via holes 14 by laser drilling as necessary (step (b)).
  • step (c) After applying chemical copper plating 15 (step (c)), a predetermined pattern is masked by exposure and development using dry film 16 (step (d)), and electrolytic copper plating 17 is applied (step (e )).
  • step (e ) After the dry film 16 is removed to form the wiring portion 17a (step (f)), the unnecessary ultra-thin copper foil or the like between the mutually adjacent wiring portions 17a and 17a is removed by etching over the entire thickness thereof ( Step (g)), wiring 18 formed in a predetermined pattern is obtained.
  • Patent Document 1 International Publication No. 2016/117587
  • the average distance between surface peaks on the side of the release layer is 20 ⁇ m or less
  • the maximum height difference of the undulations on the side opposite to the release layer is A carrier-attached copper foil comprising an ultra-thin copper foil having a thickness of 1.0 ⁇ m or less
  • Patent Document 2 Japanese Patent Application Laid-Open No.
  • a carrier-attached copper foil having a ratio Sp/Spk to Spk of 3.271 or more and 10.739 or less is disclosed.
  • shear strength is one of the physical adhesion indices between a circuit and a substrate, and in order to effectively avoid the above-mentioned circuit peeling, a roughened copper foil suitable for improving the shear strength has been proposed. ing.
  • Patent Document 3 International Publication No.
  • a treated copper foil is disclosed. According to such a roughened copper foil, it is believed that both excellent etching properties and high shear strength can be achieved in the processing of copper-clad laminates or the manufacture of printed wiring boards.
  • a printed wiring board is provided with a copper foil processed into a wiring pattern and an insulating resin base material. Transmission loss consists of conductor loss caused by the copper foil and dielectric loss caused by the insulating resin base material.
  • Patent Document 4 Japanese Patent No. 6462961 describes a surface-treated copper foil in which a roughening treatment layer, an anti-corrosion treatment layer and a silane coupling layer are laminated in this order on at least one side of the copper foil.
  • the interface developed area ratio Sdr measured from the surface of the coupling layer is 8% or more and 140% or less, the root mean square surface gradient Sdq is 25° or more and 70° or less, and the surface texture aspect ratio Str is 0.25 or more and 0. 0.79 or less. It is said that such a surface-treated copper foil makes it possible to manufacture a printed wiring board with little transmission loss of high-frequency electrical signals and excellent adhesion during reflow soldering.
  • copper foil with low transmission loss that is, copper foil with excellent high-frequency characteristics
  • transmission loss can be suppressed by smoothing the copper foil and miniaturizing the roughened particles, the physical adhesion (particularly shear strength) between the copper foil and the substrate resin will decrease. .
  • the present inventors have now found that in the roughened copper foil, the sum of the heights of the peaks and valleys calculated as the sum of the volume of the peaks and the volume of the valleys, and the average height of the peaks and the average height of the valleys Excellent transmission characteristics and high shear strength in the processing of copper-clad laminates or the manufacture of printed wiring boards by providing a surface profile in which the average height of peaks and valleys calculated as the sum is controlled within a predetermined range. I got the knowledge that it can be compatible with.
  • an object of the present invention is to provide a roughened copper foil that can achieve both excellent transmission characteristics and high shear strength in the processing of copper-clad laminates or the manufacture of printed wiring boards.
  • a roughened copper foil having a roughened surface on at least one side, wherein the roughened surface has a plurality of peaks that are convex with respect to a reference surface and a plurality of valleys that are concave with respect to the reference surface.
  • the mountain and the valley calculated as the sum of the volume of the mountain and the volume of the valley in an analysis area of 2000 nm ⁇ 2000 nm
  • the sum of the heights of the valleys is 1.4 ⁇ 10 8 nm 3 or more and 3.5 ⁇ 10 8 nm 3 or less
  • Aspect 7 The roughened copper foil according to aspect 6, wherein the surface voxel ratio is 0.25 or more and 0.35 or less.
  • Aspect 8 The roughened copper foil according to any one of aspects 1 to 7, further comprising an antirust layer and/or a silane coupling agent layer on the roughened surface.
  • a copper clad laminate comprising the roughened copper foil according to any one of aspects 1 to 8.
  • a printed wiring board comprising the roughened copper foil according to any one of aspects 1 to 8.
  • FIG. 2 is a flow chart of the steps for explaining the MSAP method, showing the first half of the steps (steps (a) to (d)).
  • FIG. 2 is a flow chart of the steps for explaining the MSAP method, showing the latter half of the steps (steps (e) to (g)).
  • FIG. 3 is a schematic cross-sectional view for explaining the reference surface of the roughened surface and the sum of the heights of peaks and valleys in the roughened copper foil.
  • FIG. 4 is a schematic cross-sectional view for explaining the reference plane of the roughened surface and the average height of peaks and valleys in the roughened copper foil.
  • FIG. 4 is a diagram in which mountains present on the roughened surface of the roughened copper foil are virtually partitioned by voxels.
  • FIG. 4 is a diagram showing regions where laser light cannot enter when a roughened surface is measured with a laser microscope.
  • 3 is a diagram showing x-, y-, and z-axes in 3D-SEM observation, and a slice plane S in relation to a roughened copper foil.
  • FIG. FIG. 4 is a diagram showing the relationship between each axis after rotating the x-axis, y-axis, and z-axis and the roughened copper foil in 3D-SEM image analysis.
  • image obtained using FIB-SEM on the roughened surface refers to cross-sectional processing by FIB (focused ion beam) on the roughened surface of the roughened copper foil. It means an aggregate of cross-sectional images acquired through cross-sectional observation by a SEM (scanning electron microscope), and constitutes three-dimensional shape data as a whole. Specifically, as shown in FIG. 7, the x-axis and z-axis are defined as the in-plane directions of the roughened copper foil 10, and the y-axis is defined as the thickness direction of the roughened copper foil 10.
  • a cross-sectional image including the roughened surface of the roughened copper foil 10 on the slice plane S parallel to the xy plane is acquired, and this slice plane is translated by a predetermined interval (for example, 10 nm) in the z-axis direction. It is a collection of cross-sectional images (for example, 1000 sheets in total) acquired in a predetermined analysis area (for example, 2000 nm ⁇ 2000 nm) while moving.
  • the “mountain” of the roughened surface is, as schematically shown in FIGS. It means the part that is convex with respect to .
  • the “valley” of the roughened surface is, as schematically shown in FIGS. It means a portion that is concave with respect to the surface R.
  • the "reference plane" of the roughened surface can be identified by three-dimensional image analysis of an image obtained using FIB-SEM for the roughened surface.
  • a median value (reference point) of the height (y direction) of the roughened surface in a predetermined matrix size (for example, 99) in the xz plane centered on the pixel of interest is obtained.
  • the matrix size is 99, it means obtaining the median value from the height of the roughened surface in each of 99 ⁇ 99 pixels centering on the pixel of interest.
  • This operation is performed for all the pixels in the xz plane that constitute the image of the concave-convex structure (each of them as a target pixel), and the median height of the roughened surface in each target pixel ( reference point). Then, a plane passing through all the reference points in each pixel of interest obtained in this manner can be created and used as a reference plane.
  • the three-dimensional image analysis described above can be automatically performed using commercially available software, and a median filter specifying a matrix size (for example, 99) is applied to the uneven structure of the roughened copper foil.
  • the reference plane can be determined systematically (that is, there is no item in commercially available software that allows arbitrary setting of conditions other than the matrix size for setting the reference plane).
  • the total height of peaks and valleys is a parameter representing the sum of the volume of peaks and the volume of valleys in an analysis area of 2000 nm x 2000 nm (size when viewed from above). That is, as schematically shown in FIG. 3, the total volume Ap of peaks with respect to the reference plane R (total volume of all peaks in the analysis region) and the total volume Av of valleys with respect to the reference plane R (in the analysis region The total volume of all valleys) corresponds to the sum of the heights of peaks and valleys.
  • the “sum of heights of peaks and valleys” may be referred to as "sum of volumes of peaks and valleys". Since it is a value calculated by accumulating the numerical value referred to by the name "height”, the expression “total height of peaks and valleys" is daringly used in this specification so that those skilled in the art can easily carry out the measurement. I am using
  • the “average height of peaks and valleys” is a parameter that represents the sum of the average height of peaks and the average height of valleys in an analysis area of 2000 nm ⁇ 2000 nm (size when viewed in plan). . That is, as schematically shown in FIG. 4, the average peak height Hp with respect to the reference plane R (the average height of all peaks in the analysis region) and the average valley height Hv with respect to the reference plane R ( The average height H of all valleys in the analysis area) corresponds to the average height H of peaks and valleys.
  • total volume of mountains per unit area of 1 nm2 means dividing the total volume of all mountains in an analysis area of 2000 nm x 2000 nm (size when viewed from above) by the area of the analysis area. It is a parameter calculated by
  • the sum of the heights of the peaks and valleys, the average height of the peaks and valleys, and the total volume of the peaks per unit area of 1 nm2 are the three-dimensional images of the roughened surface obtained using FIB-SEM. It can be identified by analysis. Such three-dimensional image analysis can be performed using commercially available software. For example, three-dimensional alignment software "ExFact Slice Aligner (version 2.0)” (Nippon Visual Science Co., Ltd. ) and three-dimensional image analysis software “ExFact VR (version 2.2)” and “foil Analysis (version 1.0)” (both manufactured by Nippon Visual Science Co., Ltd.), described in the examples of this specification. Image analysis can be performed according to the conditions specified. Also, a method for obtaining a cross-sectional image obtained by using the FIB-SEM will be described in Examples below.
  • the term “surface voxel ratio” refers to, when the peaks of the roughened surface are divided into a plurality of voxels, all voxels that constitute the peaks in an analysis area of 2000 nm ⁇ 2000 nm (size when viewed in plan) means the ratio of the total volume of voxels that make up the surface of the mountain (surface voxels) to the total volume of .
  • the surface voxel ratio can be specified by three-dimensional image analysis of an image obtained using FIB-SEM for the roughened surface. Specifically, as schematically shown in FIG. 5, an image obtained using an FIB-SEM of the roughened surface is shown in FIG.
  • electrode surface of the carrier refers to the surface that was in contact with the cathode when the carrier was manufactured.
  • the "deposition surface" of the carrier refers to the surface on which electrolytic copper is deposited during carrier production, that is, the surface that is not in contact with the cathode.
  • the copper foil according to the present invention is a roughened copper foil.
  • This roughened copper foil has a roughened surface on at least one side.
  • This roughened surface has a plurality of peaks that are convex with respect to the reference plane and a plurality of valleys that are concave with respect to the reference plane. Then, when the image obtained using FIB-SEM on the roughened surface is subjected to three-dimensional image analysis, the peaks and valleys calculated as the sum of the volume of the peaks and the volume of the valleys in the analysis area of 2000 nm ⁇ 2000 nm is 1.4 ⁇ 10 8 nm 3 or more and 3.5 ⁇ 10 8 nm 3 or less.
  • the average height of peaks and valleys calculated as the sum of the average height of peaks and the average height of valleys in an analysis area of 2000 nm ⁇ 2000 nm is 40 nm or more and 90 nm or less.
  • the copper clad laminate can be processed or processed. In the production of printed wiring boards, it is possible to achieve both excellent transmission characteristics (especially excellent high-frequency characteristics) and high shear strength (and thus high circuit adhesion in terms of shear strength).
  • the sum of the heights of the peaks and valleys represents the total volume of the peaks and valleys with respect to the reference plane R, which is the portion in contact with the substrate (the portion that bites into the substrate). roughly corresponds to the volume of Therefore, the greater the sum of the heights of the peaks and valleys, the greater the volume of the portion in contact with the substrate, leading to an increase in shear strength. Also, as described above with reference to FIG. In other words, the smaller the average height of peaks and valleys, the smaller the unevenness of the surface.
  • the unevenness of the surface is small, even if the skin depth is reduced due to the increase in frequency, the current path is less likely to be affected by the unevenness of the surface, leading to a reduction in transmission loss. Therefore, by controlling both the total height of the peaks and valleys on the roughened surface and the average height of the peaks and valleys within a predetermined range, when used in a copper-clad laminate or a printed wiring board, It is possible to realize excellent transmission characteristics and high shear strength in a well-balanced manner.
  • FIG. 6 schematically shows an example of measurement of the roughened surface using a laser microscope.
  • a laser beam is irradiated from above the roughened surface.
  • the roughened copper foil has a total height of peaks and valleys on the roughened surface of 1.4 ⁇ 10 8 nm 3 or more and 3.5 ⁇ 10 8 nm 3 or less. , preferably 2.0 ⁇ 10 8 nm 3 or more and 3.5 ⁇ 10 8 nm 3 or less from the viewpoint of further improving shear strength, or 1.4 ⁇ 10 8 nm 3 from the viewpoint of further improving transmission characteristics. 1.8 ⁇ 10 8 nm 3 or less.
  • the roughened copper foil has an average height of peaks and valleys on the roughened surface of 40 nm or more and 90 nm or less, preferably 40 nm or more and 80 nm or less, and more preferably transmission characteristics. From the viewpoint of further improving the shear strength, it is 40 nm or more and 50 nm or less, or from the viewpoint of further improving the shear strength, it is 70 nm or more and 80 nm or less.
  • the roughened copper foil preferably has a total volume of ridges per unit area of 1 nm 2 on the roughened surface of 7.0 nm 3 or more and 50.0 nm 3 or less, more preferably 30.0 nm 3 or more and 50.0 nm. 3 or less. By doing so, even higher shear strength can be achieved when used in a copper-clad laminate or a printed wiring board.
  • the roughened copper foil preferably has a surface voxel ratio of 0.25 or more and 0.60 or less on the roughened surface, and more preferably, to further improve the shear strength. It is 0.25 or more and 0.35 or less from a viewpoint, or 0.40 or more and 0.60 or less from a viewpoint of further improvement of transmission characteristics.
  • FIG. 5 schematically shows an example in which the peaks (P 1 , P 2 , P 3 ) present on the roughened surface of the roughened copper foil 10 are virtually partitioned by voxels B.
  • the peaks P 1 , P 2 and P 3 shown in FIG. 5 have the same total volume and therefore the same number of voxels B (20) that define each of these peaks.
  • the number of surface voxels Bs (voxels located at the outermost surface portion in contact with the resin) constituting the surface of the mountain is 20, 14 and 10, respectively.
  • the shear strength by the surface voxel ratio. Also, from the viewpoint of achieving excellent transmission characteristics, it is desirable to control the surface voxel ratio within the above range in consideration of the average height of peaks and valleys.
  • the thickness of the roughened copper foil is not particularly limited, it is preferably 0.1 ⁇ m or more and 35 ⁇ m or less, more preferably 0.5 ⁇ m or more and 5.0 ⁇ m or less, and still more preferably 1.0 ⁇ m or more and 3.0 ⁇ m or less.
  • the roughened copper foil is not limited to a general copper foil whose surface has been roughened, and may be a carrier-attached copper foil whose copper foil surface has been roughened.
  • the thickness of the roughened copper foil is the thickness not including the height of the roughened particles formed on the surface of the roughened surface (thickness of the copper foil itself constituting the roughened copper foil). is.
  • a copper foil having a thickness within the above range is sometimes called an ultra-thin copper foil.
  • the roughened copper foil has a roughened surface on at least one side. That is, the roughened copper foil may have roughened surfaces on both sides, or may have a roughened surface only on one side.
  • the roughened surface is typically provided with a plurality of roughening particles (nobs), and each of these roughening particles preferably consists of copper particles.
  • the copper particles may consist of metallic copper, or may consist of a copper alloy.
  • the roughening treatment for forming the roughened surface can be preferably carried out by forming roughening particles with copper or a copper alloy on the copper foil.
  • This roughening treatment is preferably carried out according to a plating technique involving three stages of plating processes.
  • a copper sulfate solution having a copper concentration of 5 g/L or more and 15 g/L or less and a sulfuric acid concentration of 200 g/L or more and 250 g/L or less is used, and the liquid temperature is 25° C. or more and 45° C. or less.
  • Electrodeposition is preferably carried out under the plating conditions of a current density of 2 A/dm 2 or more and 4 A/dm 2 or less.
  • the first-stage plating process is preferably performed twice in total using two tanks.
  • a copper sulfate solution with a copper concentration of 60 g/L or more and 80 g/L or less and a sulfuric acid concentration of 200 g/L or more and 260 g/L or less was used, and the liquid temperature was 45 ° C. or more and 55 ° C. or less, and the current density was 10 A. /dm 2 or more and 15 A/dm 2 or less.
  • the copper concentration is 5 g/L or more and 20 g/L or less
  • the sulfuric acid concentration is 60 g/L or more and 90 g/L or less
  • the chlorine concentration is 20 mg/L or more and 40 mg/L or less
  • the 9-phenylacridine (9PA) concentration is preferably performed using a copper sulfate solution of 100 mg/L or more and 200 mg/L or less under plating conditions of a liquid temperature of 25° C. or more and 35° C. or less and a current density of 30 A/dm 2 or more and 60 A/dm 2 or less.
  • Each of the second and third plating steps may be performed twice in total using two baths, but is preferably completed in one time. Through such a plating process, it becomes easier to form bumps on the treated surface that are convenient for satisfying the surface parameters described above.
  • the roughened copper foil may be subjected to antirust treatment and may have an antirust treatment layer formed thereon.
  • the antirust treatment preferably includes plating with zinc.
  • the plating treatment using zinc may be either zinc plating treatment or zinc alloy plating treatment, and the zinc alloy plating treatment is particularly preferably 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, Co and Mo.
  • 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 mass ratio.
  • the rust prevention treatment preferably further includes chromate treatment, and this chromate treatment is more preferably performed on the surface of the plating containing zinc after the plating treatment using zinc.
  • a particularly preferred antirust treatment is a combination of zinc-nickel alloy plating treatment and subsequent chromate treatment.
  • the surface of the roughened 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 the silane coupling agent, coating it, and drying it.
  • silane coupling agents include epoxy-functional silane coupling agents such as 4-glycidylbutyltrimethoxysilane, 3-glycidoxypropyltrimethoxysilane, or 3-aminopropyltrimethoxysilane, N-(2- aminoethyl)-3-aminopropyltrimethoxysilane, N-3-(4-(3-aminopropoxy)butoxy)propyl-3-aminopropyltrimethoxysilane, N-phenyl-3-aminopropyltrimethoxysilane, etc.
  • epoxy-functional silane coupling agents such as 4-glycidylbutyltrimethoxysilane, 3-glycidoxypropyltrimethoxysilane, or 3-aminopropyltrimethoxysilane, N-(2- aminoethyl)-3-aminopropyltrimethoxysilane, N-3-(4-(3-aminopropoxy)but
  • amino-functional silane coupling agents or mercapto-functional silane coupling agents such as 3-mercaptopropyltrimethoxysilane or olefin-functional silane coupling agents such as vinyltrimethoxysilane, vinylphenyltrimethoxysilane, or 3-methacrylic Acrylic functional silane coupling agents such as roxypropyltrimethoxysilane, or imidazole functional silane coupling agents such as imidazole silane, or triazine functional silane coupling agents such as triazine silane, and the like.
  • the roughened copper foil preferably further comprises an antirust treatment layer and/or a silane coupling agent layer on the roughened surface, more preferably the antirust treatment layer and the silane coupling agent layer.
  • the antirust layer and the silane coupling agent layer may be formed not only on the roughened surface side of the roughened copper foil, but also on the side where the roughened surface is not formed.
  • the roughened copper foil of the present invention may be provided in the form of a carrier-attached copper foil.
  • a carrier By adopting the form of a copper foil with a carrier, it is possible to realize excellent laser workability and fine line circuit formability. That is, according to a preferred embodiment of the present invention, a carrier, a release layer provided on the carrier, and the roughened copper foil provided on the release layer with the roughened surface facing outward, A copper foil with carrier is provided.
  • a known layer structure can be employed, except for using the roughened copper foil of the present invention.
  • a carrier is a support for supporting the roughened copper foil to improve its handling properties
  • a typical carrier includes a metal layer.
  • Examples of such a carrier include aluminum foil, copper foil, stainless steel (SUS) foil, resin film or glass whose surface is metal-coated with copper or the like, and copper foil is preferred.
  • the copper foil may be a rolled copper foil or an electrolytic copper foil, preferably an electrolytic copper foil.
  • the thickness of the carrier is typically 250 ⁇ m or less, preferably 7 ⁇ m or more and 200 ⁇ m or less.
  • the surface of the carrier on the release layer side is preferably smooth. That is, in the manufacturing process of the carrier-attached copper foil, an ultra-thin copper foil (before roughening treatment) is formed on the release layer side surface of the carrier.
  • the roughened copper foil of the present invention is used in the form of a carrier-attached copper foil, the roughened copper foil can be obtained by roughening such an ultra-thin copper foil. Therefore, by smoothing the surface of the carrier on the release layer side, the outer surface of the ultra-thin copper foil can also be smoothed. It becomes easy to realize a roughened surface having the sum of the heights of peaks and valleys and the average height of peaks and valleys within the predetermined range.
  • the surface of the carrier on the release layer side can be smoothed, for example, by polishing the surface of the cathode used in electrolytic foil production of the carrier with a buff of a predetermined number to adjust the surface roughness. That is, the surface profile of the cathode adjusted in this way is transferred to the electrode surface of the carrier, and an ultra-thin copper foil is formed on the electrode surface of the carrier with a release layer interposed therebetween. It is possible to impart a smooth surface condition that facilitates the realization of the roughened surface described above.
  • the buff number is preferably #2000 or more and #3000 or less, more preferably #2000 or more and #2500 or less.
  • the electrode surface of the carrier obtained by using the cathode polished with a buff of #2000 or more and #2500 or less has a slight undulation compared to the smooth foil deposition surface, so it is possible to ensure adhesion and smoothness. , it is possible to achieve a good balance between high adhesion and excellent transmission characteristics.
  • electrolytic foil manufacturing was performed using an electrolytic solution containing additives.
  • the carrier deposition surface side may be the surface of the carrier on the peeling layer side.
  • the release layer is a layer that has the function of weakening the peeling strength of the carrier, ensuring the stability of the strength, and suppressing interdiffusion that may occur between the carrier and the copper foil during press molding at high temperatures. .
  • 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.
  • organic components used in the organic release layer include nitrogen-containing organic compounds, sulfur-containing organic compounds, carboxylic acids, and the like.
  • Examples of the nitrogen-containing organic compound include triazole compounds, imidazole compounds, etc. Among them, triazole compounds are preferable in terms of easily stabilizing peelability.
  • triazole compounds examples include 1,2,3-benzotriazole, carboxybenzotriazole, N',N'-bis(benzotriazolylmethyl)urea, 1H-1,2,4-triazole and 3-amino- 1H-1,2,4-triazole and the like.
  • sulfur-containing organic compounds examples include mercaptobenzothiazole, thiocyanuric acid, 2-benzimidazolethiol, and the like.
  • carboxylic acids include monocarboxylic acids, dicarboxylic acids, and the like.
  • examples of inorganic components used for the inorganic release layer include Ni, Mo, Co, Cr, Fe, Ti, W, P, Zn, chromate treatment films, and the like.
  • the release layer may be formed by contacting at least one surface of the carrier with a release layer component-containing solution to fix the release layer component on the surface of the carrier.
  • this contact may be performed by immersion in the release layer component-containing solution, spraying the release layer component-containing solution, or flowing the release layer component-containing solution.
  • Fixing of the release layer component to the carrier surface may be carried out 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 or more and 1 ⁇ m or less, preferably 5 nm or more and 500 nm or less.
  • another functional layer may be provided between the release layer and the carrier and/or the roughened copper foil.
  • auxiliary metal layers include auxiliary metal layers.
  • the auxiliary metal layer preferably consists of nickel and/or cobalt. By forming such an auxiliary metal layer on the surface side of the carrier and/or on the surface side of the roughened copper foil, during hot press molding at high temperature or for a long time, it may occur between the carrier and the roughened copper foil. Mutual diffusion can be suppressed and the stability of carrier peeling strength can be ensured.
  • the thickness of the auxiliary metal layer is preferably 0.001 ⁇ m or more and 3 ⁇ m or less.
  • the roughened copper foil of the present invention is preferably used for producing a copper-clad laminate for printed wiring boards. That is, according to a preferred aspect of the present invention, there is provided a copper-clad laminate comprising the roughened copper foil.
  • This copper-clad laminate comprises the roughened copper foil of the present invention and a resin layer provided in close contact with the roughened surface of the roughened copper foil.
  • the roughened copper foil may be provided on one side of the resin layer, or may be provided on both sides.
  • the resin layer comprises resin, preferably insulating resin.
  • the resin layer is preferably prepreg and/or resin sheet.
  • Prepreg is a general term for composite materials in which synthetic resin is impregnated into a base material such as a synthetic resin plate, a glass plate, a glass woven fabric, a glass non-woven fabric, or paper.
  • insulating resins include epoxy resins, cyanate resins, bismaleimide triazine resins (BT resins), polyphenylene ether resins, and phenol resins.
  • the insulating resin forming the resin sheet include insulating resins such as epoxy resins, polyimide resins, and polyester resins.
  • the resin layer may contain filler particles made of various inorganic particles such as silica and alumina from the viewpoint of improving insulation.
  • the thickness of the resin layer is not particularly limited, it is preferably 1 ⁇ m or more and 1000 ⁇ m or less, more preferably 2 ⁇ m or more and 400 ⁇ m or less, and still more preferably 3 ⁇ m or more and 200 ⁇ m or less.
  • the resin layer may be composed of multiple layers.
  • a resin layer such as a prepreg and/or a resin sheet may be provided on the roughened copper foil in advance via a primer resin layer that is applied to the surface of the copper foil.
  • the roughened copper foil of the present invention is preferably used for producing a printed wiring board. That is, according to a preferred aspect of the present invention, there is provided a printed wiring board comprising the roughened copper foil.
  • the printed wiring board according to this aspect includes a layer structure in which a resin layer and a copper layer are laminated.
  • the copper layer is a layer derived from the roughened copper foil of the present invention.
  • the resin layer is as described above for the copper-clad laminate.
  • the printed wiring board can employ a known layer structure except for using the roughened copper foil of the present invention.
  • printed wiring boards include a single-sided or double-sided printed wiring board formed by bonding the roughened copper foil of the present invention to one or both sides of a prepreg to form a cured laminate, and then forming a circuit on the printed wiring board.
  • a multilayer printed wiring board etc. are mentioned.
  • other specific examples include flexible printed wiring boards, COF, TAB tapes, etc., in which the roughened copper foil of the present invention is formed on a resin film to form a circuit.
  • a resin-coated copper foil (RCC) is formed by applying the above resin layer to the roughened copper foil of the present invention, and the resin layer is used as an insulating adhesive layer and laminated on the above printed circuit board.
  • the roughened copper foil is used as all or part of the wiring layer, and the circuit is formed by the modified semi-additive (MSAP) method, the subtractive method, etc.
  • the build-up wiring board and the roughened copper foil are removed.
  • an electronic material for glass, an electromagnetic wave shielding film obtained by applying a conductive adhesive to the roughened copper foil of the present invention, and the like are also included.
  • the printed wiring board provided with the roughened copper foil of the present invention is used in applications such as automobile antennas, mobile phone base station antennas, high-performance servers, collision prevention radars, etc., which are used in high frequency bands with signal frequencies of 10 GHz or higher. It is suitably used as a high-frequency substrate to be used.
  • the roughened copper foil of the present invention is suitable for the MSAP method. For example, when the circuit is formed by the MSAP method, the configurations shown in FIGS. 1 and 2 can be adopted.
  • Examples 1, 2 and 4 A copper foil with a carrier provided with a roughened copper foil was produced as follows.
  • the carrier on which the organic release layer was formed was immersed in a solution containing nickel concentration of 20 g/L prepared using nickel sulfate, and the liquid temperature was 45° C., pH 3, current density 5 A/L. Under conditions of dm 2 , a deposition amount of nickel equivalent to a thickness of 0.001 ⁇ m was deposited onto the organic release layer. Thus, a nickel layer was formed as an auxiliary metal layer on the organic release layer.
  • the surface of the ultra-thin copper foil thus formed was subjected to a roughening treatment to form a roughened copper foil, thereby obtaining a carrier-attached copper foil.
  • a roughening treatment in Examples 1 and 2, the following three stages of roughening treatment were performed.
  • the roughening treatment in the first step was carried out in two steps. Specifically, using an acidic copper sulfate solution having the copper concentration and sulfuric acid concentration shown in Table 1, the roughening treatment was performed twice at the current density and liquid temperature shown in Table 1.
  • the acid copper sulfate solution having the copper concentration and sulfuric acid concentration shown in Table 1 was used, and the roughening treatment was performed at the current density and liquid temperature shown in Table 1.
  • the third stage roughening treatment uses an acidic copper sulfate solution with the copper concentration, sulfuric acid concentration, chlorine concentration and 9-phenylacridine (9PA) concentration shown in Table 1, and the current density and liquid temperature shown in Table 1 was subjected to roughening treatment.
  • Example 4 two stages of roughening treatment were performed.
  • This two-stage roughening treatment consists of a baking plating process for depositing fine copper grains on an ultra-thin copper foil and a covering plating process for preventing the fine copper grains from falling off.
  • carboxybenzotriazole (CBTA) was added to an acidic copper sulfate solution with a copper concentration of 10 g / L and a sulfuric acid concentration of 200 g / L so that the concentration shown in Table 1 was obtained, and the current density shown in Table 1 was obtained.
  • the roughening treatment was performed at liquid temperature.
  • electrodeposition was performed under smooth plating conditions of a liquid temperature of 52° C. and a current density shown in Table 1 using an acidic copper sulfate solution with a copper concentration of 70 g/L and a sulfuric acid concentration of 240 g/L.
  • the roughened surface of the obtained copper foil with carrier was subjected to antirust treatment comprising zinc-nickel alloy plating treatment and chromate treatment.
  • antirust treatment comprising zinc-nickel alloy plating treatment and chromate treatment.
  • the roughening treatment layer and the carrier A zinc-nickel alloy plating treatment was performed on the surface of the Next, the zinc-nickel alloy plated surface was subjected to chromate treatment using an aqueous solution containing 1 g/L of chromic acid under the conditions of pH 12 and current density 1 A/dm 2 .
  • Silane coupling agent treatment An aqueous solution containing a commercially available silane coupling agent is adsorbed on the surface of the roughened copper foil side of the carrier-attached copper foil, and the water is evaporated with an electric heater to perform the silane coupling agent treatment. did At this time, the carrier side was not treated with the silane coupling agent.
  • Example 3 A roughened copper foil was produced in the same manner as in Example 1 except for the following a) and b). a) Instead of the carrier-attached copper foil, the deposition surface of the following electrolytic copper foil was subjected to a roughening treatment. b) The roughening treatment conditions were changed as shown in Table 1.
  • Example 5 (Comparison) Roughening was performed in the same manner as in Example 3, except that in the roughening treatment step, the first and second roughening treatments were not performed, and the third-stage roughening treatment conditions were changed as shown in Table 1. A heat treated copper foil was produced.
  • the roughened copper foils or carrier-attached copper foils produced in Evaluation Examples 1 to 5 were subjected to various evaluations shown below.
  • ⁇ SEM conditions> - acceleration voltage: 1.0 kV -Working distance: 5mm -Tilt: 54° (with SEM image tilt correction) -Detector: InLens detector -Column Mode: High Resolution - Number of pixels: 2048 (x direction) ⁇ FIB conditions> - acceleration voltage: 30 kV - Slice thickness: 10 nm (interval between slice planes S) - Voxel size setting: Determine the voxel size you want to set, such as (x, y, z) (5 nm, 5 nm, 10 nm).
  • the slice thickness is set to 10 nm when z is desired to be 10 nm. Note that the observation magnification can be appropriately changed by the device (model, software, etc.) so as to obtain the determined voxel size.
  • Peaks and valleys were labeled separately, and the average height of peaks and valleys in the analysis area, the sum of the heights of peaks and valleys, the surface voxel ratio, and the total volume of peaks per unit area of 1 nm2 were calculated as follows: .
  • voxels forming the surface of each labeled mountain were defined as surface voxels Bs.
  • volume_voxels_sum calculated in the "voidsSummary_kobu” Excel data generated by the three-dimensional image analysis software "foil Analysis (version 1.0)" is the total volume of all the voxels that make up the mountain. (voxel value)
  • surface_voxels_sum is the total volume (voxel value) of the surface voxels Bs.
  • the surface voxel ratio in the analysis region was calculated by dividing the total volume of the surface voxels Bs by the total volume of all the voxels forming the mountain.
  • a laminate for evaluation was produced. That is, on the surface of the inner layer substrate, a carrier-attached copper foil or a roughened copper foil is laminated via a prepreg (Mitsubishi Gas Chemical Co., Ltd., GHPL-830NSF, thickness 30 ⁇ m) so that the roughened surface is in contact. and thermocompression bonded at a pressure of 4.0 MPa and a temperature of 220° C. for 90 minutes. After that, in the case of the carrier-attached copper foil, the carrier was peeled off to obtain a laminate for evaluation.
  • a prepreg Mitsubishi Gas Chemical Co., Ltd., GHPL-830NSF, thickness 30 ⁇ m
  • a dry film was attached to the laminate for evaluation described above, and exposure and development were performed. After depositing a copper layer by pattern plating on the laminate masked with the developed dry film, the dry film was peeled off. The exposed copper portion was etched with a sulfuric acid-hydrogen peroxide-based etchant to prepare a sample for shear strength measurement having a height of 15 ⁇ m, a width of 14 ⁇ m, and a length of 150 ⁇ m. Using a bonding strength tester (4000Plus Bondtester manufactured by Nordson DAGE), the shear strength when the sample for shear strength measurement was pushed down from the side was measured.
  • a bonding strength tester 4000Plus Bondtester manufactured by Nordson DAGE
  • the test type was a destructive test, and the measurement was performed under the conditions of a test height of 5 ⁇ m, a descending speed of 0.05 mm/s, a test speed of 200 ⁇ m/s, a tool movement of 0.03 mm, and a rupture recognition point of 10%.
  • the obtained shear strength was rated and evaluated according to the following criteria, and evaluations A and B were judged to be acceptable. The results were as shown in Table 2.

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  • Chemical & Material Sciences (AREA)
  • Engineering & Computer Science (AREA)
  • Chemical Kinetics & Catalysis (AREA)
  • Electrochemistry (AREA)
  • Materials Engineering (AREA)
  • Metallurgy (AREA)
  • Organic Chemistry (AREA)
  • Manufacturing & Machinery (AREA)
  • Microelectronics & Electronic Packaging (AREA)
  • Laminated Bodies (AREA)
  • Parts Printed On Printed Circuit Boards (AREA)

Abstract

L'invention concerne une feuille de cuivre rugosifiée pouvant présenter à la fois d'excellentes propriétés de transmission et une résistance au cisaillement élevée, dans le traitement d'un stratifié cuivré ou la production d'une carte de circuit imprimé. Ladite feuille de cuivre rugosifiée comprend une surface rugosifiée sur au moins un côté de celle-ci. Cette surface rugosifiée comprend une pluralité de pics, qui font saillie par rapport à un plan de référence, et une pluralité de vallées, qui sont en retrait par rapport au plan de référence. Lorsqu'une image de la surface rugueuse obtenue à l'aide du FIB-SEM a été soumise à une analyse d'image tridimensionnelle, la somme totale des hauteurs de pic et de vallée calculées en tant que somme du volume de pic et du volume de vallée dans une zone d'analyse de 2 000 nm x 2 000 nm est de 1,4 × 108 nm3 à 3,5 ×108 nm3, et la hauteur moyenne des pics et des vallées calculée en tant que somme de la hauteur de pic moyenne et de la hauteur de vallée moyenne est de 40 nm à 90 nm.
PCT/JP2022/020747 2021-05-20 2022-05-18 Feuille de cuivre rugosifiée, feuille de cuivre comprenant un support, carte stratifiée plaquée de cuivre et carte de circuit imprimé WO2022244826A1 (fr)

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JP2023522710A JPWO2022244826A1 (fr) 2021-05-20 2022-05-18
KR1020237038900A KR20240009403A (ko) 2021-05-20 2022-05-18 조화 처리 구리박, 캐리어 구비 구리박, 동장 적층판 및 프린트 배선판
CN202280035616.5A CN117321253A (zh) 2021-05-20 2022-05-18 粗糙化处理铜箔、带载体的铜箔、覆铜层叠板及印刷电路板

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WO2019093494A1 (fr) * 2017-11-10 2019-05-16 ナミックス株式会社 Feuil composite de cuivre
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JP5204908B1 (ja) * 2012-03-26 2013-06-05 Ｊｘ日鉱日石金属株式会社 キャリア付銅箔、キャリア付銅箔の製造方法、プリント配線板用キャリア付銅箔及びプリント配線板
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KR20240009403A (ko) 2024-01-22

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