WO2019111914A1 - Feuille de cuivre traitée en surface et stratifié cuivré et carte de circuit imprimé utilisant chacun celle-ci - Google Patents

Feuille de cuivre traitée en surface et stratifié cuivré et carte de circuit imprimé utilisant chacun celle-ci Download PDF

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Publication number
WO2019111914A1
WO2019111914A1 PCT/JP2018/044622 JP2018044622W WO2019111914A1 WO 2019111914 A1 WO2019111914 A1 WO 2019111914A1 JP 2018044622 W JP2018044622 W JP 2018044622W WO 2019111914 A1 WO2019111914 A1 WO 2019111914A1
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Prior art keywords
copper foil
roughened
particles
treated copper
particle
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PCT/JP2018/044622
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English (en)
Japanese (ja)
Inventor
貴広 齋藤
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古河電気工業株式会社
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Application filed by 古河電気工業株式会社 filed Critical 古河電気工業株式会社
Priority to JP2019523892A priority Critical patent/JP6623320B2/ja
Priority to CN201880078041.9A priority patent/CN111655908B/zh
Priority to KR1020207013808A priority patent/KR102390417B1/ko
Publication of WO2019111914A1 publication Critical patent/WO2019111914A1/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
    • 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
    • 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
    • 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
    • C25D5/615—Microstructure of the layers, e.g. mixed structure
    • C25D5/617—Crystalline layers
    • 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
    • C25D5/627—Electroplating characterised by the visual appearance of the layers, e.g. colour, brightness or mat appearance
    • 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
    • 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
    • C25D7/0614—Strips or 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
    • H05K1/00—Printed circuits
    • H05K1/02—Details
    • H05K1/09—Use of materials for the conductive, e.g. metallic pattern
    • 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
    • H05K3/38—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
    • H05K3/384—Improvement of the adhesion between the insulating substrate and the metal by special treatment of the metal by plating

Definitions

  • the present invention relates to a surface-treated copper foil, particularly to a surface-treated copper foil suitable for a printed wiring board used in a high frequency band. Furthermore, the present invention relates to a copper-clad laminate and a printed wiring board using the surface-treated copper foil.
  • the resin in order to enhance the adhesion with the resin substrate, in addition to the formation of the above-mentioned roughening treatment layer, the resin is processed by treating the copper foil surface with a silane coupling agent.
  • a technique is used to provide chemical adhesion to the substrate.
  • the resin base material in order to enhance the chemical adhesion between the silane coupling agent and the resin base material, it is necessary that the resin base material has a substituent of a somewhat large polarity.
  • the suppression of transmission loss and the adhesion between the copper foil and the resin substrate, in particular, the adhesion between the normal state and the heat resistant adhesion are trade-off with each other. It is related. Therefore, conventionally, with copper foils used in copper-clad laminates, various methods have been studied from the viewpoint of coexistence of suppression of transmission loss and normal adhesion with a resin substrate and heat resistant adhesion.
  • Patent Document 1 proposes a method of increasing the surface area ratio by fine asperities
  • Patent Document 2 proposes a method of making roughened particles into a special shape
  • Patent Document 3 discloses nickel or the like.
  • a method of forming fine roughened particles by alloy plating with cobalt or the like is proposed, and in Patent Document 4, fine roughened particles are formed, and an oxidation-resistant treatment layer containing molybdenum and cobalt is formed thereon.
  • a covering method has been proposed.
  • the present invention has been made in view of the above-described circumstances, and particularly when used for a conductor circuit of a printed wiring board, excellent transmission characteristics in a high frequency band (hereinafter, may be simply referred to as "high frequency characteristics").
  • An object of the present invention is to provide a surface-treated copper foil capable of achieving both excellent normal adhesion and heat-resistant adhesion with a resin substrate.
  • the surface-treated copper foil has a surface-treated copper foil having a surface-treated coating including a roughening-treated layer having roughened particles formed on at least one surface of the copper foil substrate.
  • the surface of the surface-treated film has an average value of the particle height (h) of the roughening particles of 0.05 to 0.30 ⁇ m,
  • the average value of the ratio (h / w) of the particle height (h) to the particle width (w) of the roughened particles is 0.7 to 5.0, and the line coverage (c) of the roughened particles
  • the gist configuration of the present invention is as follows.
  • a surface-treated copper foil having a surface treatment film comprising a roughening treatment layer having roughening particles formed on at least one surface of a copper foil substrate When the cross section of the surface-treated copper foil is observed with a scanning electron microscope (SEM), the surface of the surface-treated film is: The average value of the particle height (h) of the roughened particles is 0.05 to 0.30 ⁇ m, The average value of the ratio (h / w) of the particle height (h) to the particle width (w) of the roughened particles is 0.7 to 5.0,
  • a surface-treated copper foil, wherein the line coverage (c) of the roughened particles calculated by the following formula (1) is 15 to 60%.
  • c d ⁇ W ⁇ 100 (%) (1)
  • c is the line coverage (c)
  • d is calculated from the number of the roughened particles present per area of 2.5 ⁇ m in the width direction of the observation field of view
  • W is the average value of the particle width (w) of the roughened particles in the region.
  • G s 20 degrees specular glossiness G s (20 °), 60 degree specular glossiness Gs (60 °) and 85 degree specular glossiness G s (85 °) on the surface of the surface treatment film
  • the surface-treated copper foil as described in the above [1], wherein the value calculated in (2) is 0 to 10.
  • [5] The surface-treated copper foil according to any one of the above [1] to [4], which has a ten-point average roughness Rzjis value of 0.5 to 2.0 ⁇ m on the surface of the surface treatment film.
  • [6] A copper-clad laminate formed by using the surface-treated copper foil according to any one of the above [1] to [5].
  • [7] A printed wiring board formed by using the copper clad laminate according to the above [6].
  • the cross section of the surface-treated copper foil is When observed by a scanning electron microscope (SEM), the surface of the surface-treated film has an average value of the particle height (h) of the roughened particles of 0.05 to 0.30 ⁇ m, and The average value of the ratio (h / w) of the particle height (h) to the particle width (w) is 0.7 to 5.0, and the linear coverage (c) of the roughened particles is 15 to 60%
  • SEM scanning electron microscope
  • the surface-treated copper foil of the present invention even when high frequency signals exceeding 50 GHz are transmitted, for example, transmission loss can be highly suppressed, and the resin base (resin layer) can be used even at high temperatures. High adhesion can be maintained, and a printed wiring board excellent in durability under severe conditions can be obtained.
  • FIG. 1 is each example of the SEM image which observed the surface condition of the surface treatment film
  • FIG. 2 is an example of the procedure at the time of image-analyzing the SEM image of the processed cross section of surface treatment copper foil.
  • FIG. 3 is a diagram for explaining an example of a method of measuring roughened particles.
  • FIG. 4 is a diagram for explaining a method of measuring roughened particles having a special shape.
  • FIG. 5 is a view for explaining an example of a method of measuring roughened particles having a special shape, in particular, roughened particles having protrusions.
  • the surface-treated copper foil according to the present invention has a surface-treated film including a roughening-treated layer having roughened particles formed on at least one surface of a copper foil substrate, and a cross section of the surface-treated copper foil is scanned When observed with a scanning electron microscope (SEM), the surface of the surface-treated film has an average value of the particle height (h) of the roughened particles of 0.05 to 0.30 ⁇ m, and the particles of the roughened particles.
  • the average value of the ratio (h / w) of the ratio (h / w) of the particle height (h) to the width (w) is 0.7 to 5.0, and the line coverage of the roughened particles calculated by the following formula (1) It is characterized in that (c) is 15 to 60%.
  • c d ⁇ W ⁇ 100 (%) (1)
  • c is the line coverage (c)
  • d is calculated from the number of the roughened particles present per area of 2.5 ⁇ m in the width direction of the observation field of view
  • W is the average value of the particle width (w) of the roughened particles in the region.
  • the surface-treated copper foil of the present invention has a copper foil substrate and a surface-treated film including a roughened layer formed by forming roughened particles on at least one surface of the copper foil substrate.
  • the surface of such a surface-treated film is at least one of the outermost surfaces (front and back surfaces) of the surface-treated copper foil, and the formation state of roughened particles formed on at least one surface of the copper foil substrate.
  • the surface of such a surface-treated film (hereinafter referred to as "roughened surface”) may be, for example, the surface of a roughened layer formed on a copper foil substrate, or on this roughened layer.
  • Intermediate layer such as Ni-containing underlayer, Zn-containing heat-resistant layer, and Cr-containing rust-proof layer on the surface of the silane coupling agent layer directly formed on the surface or on the roughened layer It may be the surface of a silane coupling agent layer formed via Moreover, when the surface-treated copper foil of the present invention is used, for example, in a conductor circuit of a printed wiring board, the above-mentioned roughened surface becomes a surface (adhesion surface) for laminating a resin base material. .
  • FIGS. 1 (a) and (b) the appearance of the roughened surface of the surface-treated copper foil of the present invention is shown in FIGS. 1 (a) and (b).
  • Fig.1 (a) is an example of the SEM image which observed the roughening surface of the surface-treated copper foil of this invention from the upper right by the scanning electron microscope (SEM), and
  • FIG.1 (b) is surface-treated copper. It is an example of the SEM image which gave cross section processing using the ion milling device from the surface side of foil, and observed the processed cross section with a scanning electron microscope (SEM).
  • SEM scanning electron microscope
  • FIGS. 1A and 1B very fine roughened particles are relatively sparsely formed on the roughened surface of the surface-treated copper foil of the present invention.
  • the shape evaluation of roughened particles on such a special roughened surface is the limit of resolution (at present, the particle diameter is 0 in observation methods such as laser microscope and white interference microscope). Since it is less than about 1 ⁇ m, accurate evaluation is difficult, and a sufficient judgment can not be made because a clear judgment of the height difference of the roughened particles can not be made only by optical methods such as specular gloss measurement. Therefore, in the conventional method, strict evaluation of the roughened surface has limitations in terms of cost and technology. Therefore, in the present invention, as one method of evaluating the roughened surface, as shown in FIG. 1 (b), the formation state of the roughened particles in the roughened surface is analyzed from the cross section of the surface treated copper foil. It was decided to define and evaluate the characteristics of the roughened surface. Specifically, the following method is used.
  • cross-sectional processing is performed from the surface side of the surface-treated copper foil using an ion milling apparatus, and the processed cross-section is observed with a secondary electron image with a magnification of 50,000 times at an acceleration voltage of 3 kV of SEM.
  • the surface-treated copper foil is horizontally fixed on a smooth support base so as not to cause warpage or sag of the surface-treated copper foil, and the surface-treated copper in a cross-sectional SEM photograph The foil should be adjusted to be horizontal.
  • FIG. 2 shows an example of the image analysis procedure.
  • a cross-sectional SEM photograph with a magnification of 50,000 times as shown in FIG. 2 (a) is obtained.
  • the cross-sectional SEM photograph is image-processed to extract the contour of the cross-sectional shape as shown in FIG. 2 (b).
  • only the outline of the cross-sectional shape in the same processed cross-section as shown in FIG. 2C is extracted.
  • image processing can be performed by known processing software such as general image editing software "Photoshop”, “image J”, “Real World Paint” and the like. Specifically, this will be described in the following embodiment.
  • FIG. 3A An example of the simplest roughening particle measurement method is shown in FIG.
  • FIG. 3B An example of the simplest roughening particle measurement method is shown in FIG.
  • a convex portion (roughened particle) to be measured on a contour line
  • a line L passing through the apex V of the convex portion is drawn in the particle growth direction.
  • FIG. 3B a rectangle (including a square) Sq having upper and lower sides intersecting perpendicularly with the line L is drawn.
  • the upper side intersects with the vertex V, and one of the corners of the lower side intersects with the one of the roots of the convex portion that is farther from the vertex (this angle is referred to as “R1”). Furthermore, the other corner of the lower side of the rectangle Sq (this corner is referred to as “R2”) is orthogonal to one side extending parallel to the line L from the upper side direction, and the other root of the convex portion is located on the one side (This point is called "R2 '"). Then, as shown in FIG.
  • the dimension of one side parallel to the line L is taken as the particle height (h) of the roughening particle, and one side perpendicular to the line L Let the dimension be the particle width (w) of the roughened particles.
  • all the convex parts which drew and measured rectangle Sq are regarded as one roughening particle, respectively.
  • the ratio (h / w) of the particle height (h) to the particle width (w) is less than 0.40. Also, since they do not affect the adhesion and high-frequency characteristics to which the present invention is focused, they are not to be observed and are not included in the "roughened particles" of the present invention.
  • FIG.4 (b) is a measurement example of the convex part which has two or more vertices.
  • each vertex may be regarded as one particle and measured based on the above definition.
  • FIG.4 (c) is a measurement example of the convex part in which root vicinity is 2 steps or more.
  • the determination of the root it is determined in view of which portion of the convex portion the adhesion and high-frequency characteristics of interest of the present invention are affecting. That is, of the roots of the convex portion, the angle R1 which intersects with the one far from the vertex is the position of the lowermost step of the roots. Also, in this case, the growth direction of the particles is determined as the whole particle.
  • FIG. 4D as shown in FIG. 4A, another convex portion is present on a convex portion having an ambiguous root whose dimension ratio (h / w) is less than 0.40. It is an example of measurement when there is. In this case, an ambiguous root is not to be measured, and a convex portion having distinguishable roots may be focused and measured based on the above definition. In the first place, the gentle convex portion having an ambiguous root does not affect the adhesion and high frequency characteristics to which the present invention focuses.
  • the convex part which it is going to measure has the main part A and the projection part B branched from there, it measures as follows.
  • the height (h) and the width (w) of the particles are measured on the basis of the above-mentioned criteria for the convex portion which is the main part A, and the particles are recognized as rough particles .
  • FIG. 5 (c) from the position R1 B of the root of the protrusion is a branched protrusion B from the main portion A, draw a line perpendicular to the line L A of the main portion A , Let this intersection be R1 BLA .
  • height h AB is at least 1/4 of particle height h A of main part A.
  • the protrusion B is not to be measured and is not included in the "roughened particles" of the present invention.
  • the protrusion B measures the particle height (h) and the particle width (w) according to the above criteria. , Treated as a roughened particle different from the main part A.
  • the particle height (h) and the particle width (w) may be appropriately determined according to the above criteria, taking into consideration the effects of adhesion and high frequency characteristics to which the present invention focuses. Measure).
  • each cross-sectional photograph based on the above criteria, the particle height (h) and the particle width (w) of the roughened particles, and the roughened particles present around 2.5 ⁇ m in the width direction of the observation field (observation Measure the number of target particles). Based on these values, each average value of the particle height (h), the particle width (w) and the ratio (h / w) of the particle height (h) to the particle width (w) and the roughened particles described later The linear density (d) and the linear coverage (c) are calculated respectively. Then, each value calculated for every cross-sectional photograph is put together, it averages with the total of an observation cross section, and it is set as the measured value of each surface-treated copper foil. A more specific measurement method and calculation method will be described in Examples described later.
  • the average value of the particle height (h) of the roughened particles is 0.05 to 0.30 ⁇ m, preferably 0.05 to 0.20 ⁇ m, and more preferably 0.10 to 0 .20 ⁇ m.
  • the outstanding high frequency characteristic and the outstanding normal-state adhesiveness and heat-resistant adhesiveness can be made to be compatible.
  • the average value of the particle height (h) of the roughened particles is less than 0.05 ⁇ m, the heat-resistant adhesion tends to decrease, and when it exceeds 0.30 ⁇ m, the high frequency characteristics tend to decrease.
  • the average value of the width (w) of the roughened particles is preferably 0.02 to 0.15 ⁇ m, more preferably 0.02 to 0.10 ⁇ m, and still more preferably 0.02 to 0.08 ⁇ m. It is. In particular, when the average value of the width (w) of the roughening particles is 0.10 ⁇ m or less, the heat resistant adhesion can be further improved.
  • the average value of the ratio (h / w) of the particle height (h) to the particle width (w) of the roughened particles is 0.7 to 5.0, preferably 1.0 to 5.0. More preferably, it is 1.0 to 4.0, and more preferably 1.0 to 3.0. By setting it as the said range, the outstanding high frequency characteristic and the outstanding normal-state adhesiveness and heat-resistant adhesiveness can be made to be compatible. When the average value of the ratio (h / w) is less than 0.7, the heat resistant adhesion tends to be lowered. In addition, normal adhesion can be further improved by setting the average value of the ratio (h / w) to 1.0 or more.
  • the average value of the ratio (h / w) is not particularly significant even if it exceeds 5.0, and in some cases, powder failure may occur, and the strength of the roughened particles is reduced by heating (especially heat-resistant adhesion) Tend to decrease.
  • the linear density (d) of the roughened particles in the roughened surface is preferably 2.0 particles / ⁇ m or more, more preferably 3.0 particles / ⁇ m or more, and still more preferably 4.0 particles. / ⁇ m or more.
  • the linear density (d) of the roughened particles is a value calculated from the number of roughened particles (observed particles) present in the vicinity of 2.5 ⁇ m in the width direction of the observation field, and a unit line area (width area) Means the number density of particles per).
  • the line coverage (c) of the roughened particles calculated by the following formula (1) is 15 to 60%, preferably 20 to 50%, and more preferably 25 to 50. %, More preferably 25 to 45%.
  • the outstanding high frequency characteristic and the outstanding normal-state adhesiveness and heat-resistant adhesiveness can be made to be compatible.
  • the line coverage (c) of the roughened particles exceeds 60%, the surface area is excessively increased to deteriorate the high frequency characteristics.
  • the heat-resistant adhesion tends to decrease in both cases of less than 15% and more than 60%.
  • the heat resistant adhesion can be further improved.
  • c d ⁇ W ⁇ 100 (%) (1)
  • c is the line coverage (c)
  • d is the rough calculated from the number of the roughening particles present in an area of 2.5 ⁇ m in the width direction of the observation field of view. It is a linear density (d) [pieces / ⁇ m] of the solidified particles, and W is an average value of the particle width (w) of the roughened particles in the region.
  • the fine roughened particles exert an effect like a tear-off line on the resin substrate which is to be peeled off by some stress.
  • the resin layer in which the ductility is reduced particularly under a high thermal environment is easily cohesively broken along the tip of the roughening particles, and the heat-resistant adhesion is reduced.
  • the linear density (d) and the linear coverage (c) of the roughened particles on the roughened surface can be seen as similar indicators.
  • the line coverage (c) is more correlated with the effect of the above-mentioned cut line than the line density (d) of the roughened particles.
  • the line coverage (c) is smaller. It is considered that the effect of the above-mentioned tearing line is diminished because the number of parts is increased.
  • the effect of the above-mentioned perforation line is not simply the density as the number of roughening particles per unit line area, but it means that it has an appropriate gap (portion where roughening particles do not exist) between roughening particles In Japan, the influence of sparseness is considered to be large. Therefore, as in the surface-treated copper foil of the present invention, in the roughened surface (the bonding surface with the resin base material) on which the very fine level roughened particles are formed, the effect of the above-mentioned tearing line is suppressed In order to do so, it is considered desirable that the roughening particles be moderately sparse.
  • the specular glossiness measured in accordance with JIS Z 8741-1997 be in the following range for each light receiving angle.
  • the measurement of specular gloss is generally measured and evaluated at a single light receiving angle, but the roughened surface of the surface-treated copper foil of the present invention has a complicated shape due to the formation of roughened particles. Therefore, it is difficult to sufficiently evaluate the characteristics of the surface shape at a single light receiving angle. Therefore, in the roughened surface of the surface-treated copper foil of the present invention, the surface shape of the roughened surface can be evaluated in more detail by measuring the specular glossiness using the following three light receiving angles. .
  • the average value of the height (h) of the roughened particles described above and the ratio (h / w) of the particle height (h) to the particle width (w) of the roughened particles is preferred because the evaluation of the average value of and the line coverage of roughened particles (c) is prioritized, but a certain degree of tendency is also observed in the mirror glossiness.
  • the evaluation of the glossiness it is possible to evaluate in more detail also the features of the fine shape of the roughened particles in the roughened surface of the copper foil of the present invention.
  • the measurement of the specular gloss on the roughened surface is not a measurement on a smooth surface, so the measured values at the three light reception angles are not in a simple proportional relationship.
  • the 20 ° specular gloss G s (20 °) is preferably 0.5 to 120%, more preferably 0.5 to 100%, in particular, from the viewpoint of achieving both high frequency characteristics and heat resistant adhesion. More preferably, it is 5 to 100%, and still more preferably, 15 to 100%.
  • the 60 ° specular gloss G s (60 °) is preferably 5 to 200%, more preferably 10 to 200%, and still more preferably 20, particularly from the viewpoint of achieving both high frequency characteristics and heat resistant adhesion. It is ⁇ 200%, and more preferably 20 ⁇ 150%.
  • the 85 ° specular gloss G s (85 °) is preferably 75 to 120%, more preferably 75 to 115%, and still more preferably 80 to 120, from the viewpoint of achieving both high frequency characteristics and heat resistant adhesion. It is 115%, more preferably 85 to 115%.
  • the surface-treated copper foil of the present invention 20 degrees in the roughened surface specular glossiness G s (20 °), 60 ° specular gloss Gs (60 °) and 85 degree specular gloss G s of (85 °)
  • the value calculated by the following formula (2) according to each value is preferably 0 to 10, more preferably 0 to 9, and still more preferably 0 to 5. By setting it as the said range, the outstanding high frequency characteristic and heat-resistant adhesiveness can be reconciled more reliably. When the value calculated by the following formula (2) is less than 0, the heat-resistant adhesion tends to decrease, and when it is more than 10, the high frequency characteristics tend to decrease. (Gs (85 °)-Gs (60 °)) / Gs (20 °) (2) Detailed measurement conditions will be described in the following examples.
  • the surface-treated copper foil of the present invention preferably has a ten-point average roughness Rzjis value of 0.5 to 2.0 ⁇ m, and more preferably 0.5 to 1.5 ⁇ m on the roughened surface.
  • Rzjis value 0.5 to 2.0 ⁇ m, and more preferably 0.5 to 1.5 ⁇ m on the roughened surface.
  • the surface-treated copper foil of the present invention by using this for the conductor circuit of the printed wiring board, it is possible to highly suppress the transmission loss when transmitting high frequency signals in the GHz band, and also under high temperature.
  • the adhesion between the surface-treated copper foil and the resin substrate (resin layer) can be favorably maintained, and a printed wiring board excellent in durability under severe conditions can be obtained.
  • the copper foil substrate As the copper foil substrate, it is preferable to use an electrolytic copper foil or a rolled copper foil having a smooth and glossy surface free of coarse irregularities. Among them, it is preferable to use an electrodeposited copper foil in view of productivity and cost, and it is more preferable to use an electrodeposited copper foil which is generally referred to as “double-sided glossy foil” and is smooth on both sides. From the viewpoint of properly forming the fine roughened particles of the present invention on the surface of the copper foil substrate as described above, the 20 degree specular gloss Gs (20 °), 60 degree specular gloss on the surface of the copper foil substrate The degree Gs (60 °) and the 85 ° specular gloss Gs (85 °) are both preferably 50% or more.
  • the smooth and glossy surface is, for example, an S (shiny) surface in a normal electrolytic copper foil, and in a double-sided glossy foil, both an S surface and an M (mat) surface.
  • the smooth and glossy surface is an M surface.
  • the S-shaped and M-shaped stripes or depressions are very macroscopic and different in scale as compared to the particle size of the roughened particles that the present invention intends to form. Therefore, such a ridge or recess having a streak shape undulates the baseline of the roughened surface but does not affect the shape of the roughened particles formed thereon. Therefore, although not explicitly described in the above definition, it is needless to say that macro unevenness such as undulation of the roughened surface is not to be measured as roughened particles in the present invention.
  • the ten-point average on the roughened surface of the surface-treated copper foil is It may affect the value of the roughness Rzjis value. Therefore, from the viewpoint of controlling the predetermined ten-point average roughness Rzjis value in the above-described roughened surface to a predetermined range, the ten-point average roughness Rzjis value of the surface to be roughened described later is preferably 0.5. It is -2.0 ⁇ m, more preferably 0.5-1.5 ⁇ m.
  • the measuring method is the same as the measurement in a roughening surface. Detailed measurement conditions will be described in Examples described later.
  • roughening treatment for example, it is preferable to perform a roughening plating treatment (1) as shown below. In addition, you may combine fixed plating process (2) as needed.
  • the roughening plating process (1) is a process for forming roughening particles on at least one surface of a copper foil substrate. Specifically, plating is performed in a copper sulfate bath. In such a copper sulfate bath (rough plating plating solution basic bath), molybdenum (Mo), arsenic (As), antimony (Sb), bismuth for the purpose of preventing the falling off of roughened particles, that is, “powdering off” It is possible to add conventionally known additives such as (Bi), selenium (Se), tellurium (Te) and tungsten (W), and it is particularly preferable to add molybdenum (Mo).
  • the present inventor has found that the following factors affect the surface properties of surface-treated copper foils, and by precisely setting those conditions, the high frequency characteristics that are the effects of the present invention It has been found that the required characteristics of adhesion and adhesion (normal adhesion and heat resistant adhesion) can be satisfied at a high level.
  • the copper concentration is preferably 5 to 13 g / L.
  • the additive added to the copper sulfate bath will be described by taking, for example, molybdenum (Mo) as an example.
  • Mo molybdenum
  • the concentration of molybdenum (Mo) is less than 500 mg / L, the formation of roughening particles may be concentrated on macro-striped convex portions of a copper foil substrate, etc., and the uniformity of roughening formation is deteriorated.
  • the roughened particles are refined while maintaining the average value of the ratio (h / w) of the particle height (h) to the particle width (w) of the roughened particles to which the present invention is focused, at a predetermined value. And it tends to be difficult to achieve both adhesion and high frequency characteristics.
  • the concentration of molybdenum (Mo) exceeds 1000 mg / L, the density of generation of nuclei serving as the origin of roughening particle generation becomes excessively large, and the line coverage (c) of roughened particles becomes excessively large.
  • the heat-resistant adhesion tends to deteriorate. Therefore, the concentration of molybdenum (Mo) is preferably 500 to 1000 mg / L.
  • the plating process is preferably a roll-to-roll plating process, for example, in terms of mass production and production cost.
  • the conditions of the plating treatment may be appropriately adjusted according to the processing method, but it is preferable to set the conditions that stirring of the plating solution is difficult to occur, particularly from the viewpoint of suppressing the diffusion of copper ions. Therefore, in the roll-to-roll method, it is preferable to match the processing direction (direction of processing speed) with the direction of flow of the plating solution between the poles (direction of flow velocity between the poles). Moreover, in systems other than a roll-to-roll system, it is desirable to process in the state of a stationary bath, and it is preferable not to perform stirring during a plating process.
  • gas may be generated during the plating process, and agitation may occur as the generated gas floats.
  • agitation may occur as the generated gas floats.
  • the process of the present invention is completed in a very short time of about 3 seconds at most. There is no need to do it.
  • the gas continues to be generated in the processing tank and the gas generated continuously rises one after another, so the plating solution flows in the floating direction.
  • the copper foil substrate is continuously supplied to the plating solution, so that the flow of the plating solution occurs in the transport direction of the copper foil substrate. If the two flows coincide, the above-mentioned gas evolution need not be substantially considered. However, if the two flows are in the opposite direction to each other, unnecessary stirring force may be generated on the treated surface to promote the diffusion of copper ions.
  • the reaction vessel is subjected to the plating process so that the floating direction of the gas coincides with the transport direction of the copper foil substrate (the processing direction of the plating process). It is preferable to select.
  • the absolute value of the difference between the processing speed and the flow velocity between the plating solutions flowing along the processing direction (hereinafter referred to as "processing flow velocity between electrodes").
  • processing flow velocity between electrodes When it exceeds 1.0 m / min, unnecessary stirring power is generated on the treated surface to promote the diffusion of copper ions.
  • the promotion of copper ion diffusion affects the line coverage of roughened particles and the ratio (h / w) of the particle height (h) to the particle width (w) of roughened particles, as described above, resulting in heat-resistant adhesion. Sex tends to deteriorate. Therefore, the absolute value of the difference between the treatment speed and the treatment direction inter-electrode flow velocity is preferably less than 1.0 m / min.
  • the product S exceeds 80 ⁇ (A / dm 2 ) ⁇ sec ⁇ , the roughened particles grow excessively, which makes it difficult to obtain the high frequency characteristics required by the present invention. Therefore, the product S is preferably 10 to 80 ⁇ (A / dm 2 ) ⁇ second ⁇ .
  • the ratio of the product S of the current density to the processing time to the concentration of molybdenum (Mo) is less than 0.02 [ ⁇ (A / dm 2 ) ⁇ second ⁇ / (mg / L)].
  • the S / Mo concentration exceeds 0.10 [ ⁇ (A / dm 2 ) ⁇ second ⁇ / (mg / L)]
  • the roughened particles or the like of the macro streak-like convex portion of the copper foil substrate are In addition to the formation being concentrated in some cases, and in addition to the deterioration of the uniformity of the roughing formation, it becomes difficult to finely form the roughening particles while maintaining the shape having the characteristics required by the present invention. There is a tendency that it is difficult to make high frequency characteristics compatible. Therefore, it is preferable to set the S / Mo concentration to 0.02 to 0.10 [ ⁇ (A / dm 2 ) ⁇ second] / (mg / L)].
  • the fixed plating process (2) is a process for performing smooth covering plating on the copper foil substrate surface-treated by the roughening plating process (1). Specifically, plating is performed in a copper sulfate bath. Usually, this treatment is performed to prevent the detachment of the roughened particles, that is, to immobilize the roughened particles. In the present invention, the fixed plating process (2) is not essential and can be performed as needed. For example, in the production of a copper-clad laminate, in combination with a flexible substrate using a hard resin such as polyimide resin, etc. It is preferable to carry out in order to make the roughened surface correspond to a hard resin.
  • the plating process is preferably a roll-to-roll plating process, for example, in terms of mass production and production cost. If the absolute value of the difference between the processing speed and the interelectrode flow velocity is less than 9 m / min when the fixed plating process is performed by the roll-to-roll method, it becomes difficult to perform normal fixed plating, and powder fall off Is more likely to occur. Also, if it exceeds 24 m / min, the root of the roughening particles is likely to be buried, and the average value of the ratio (h / w) of the particle height (h) to the width (w) of the roughening particles may be increased.
  • the absolute value of the difference between the treatment speed and the interelectrode flow velocity is preferably 9 to 24 m / min.
  • the flow direction of the processing speed may not coincide with the flow direction of the flow velocity between the poles, and in the case of mutually opposite directions, one flow velocity is the other flow velocity Calculated as negative flow velocity.
  • the ratio [(K / S) ⁇ 100] (%) of the product K of the current density of the fixed plating process (2) to the product S of the current density of the roughening plating process (1) and the processing time is If it exceeds 50%, it becomes difficult to maintain the shape of the roughened particles obtained by the roughening plating process (1), and it becomes difficult to satisfactorily maintain various properties such as heat resistant adhesion. Therefore, the ratio [(K / S) ⁇ 100] is preferably 50% or less.
  • the method of controlling the shape of roughened particles on the roughened surface, etc. has been described together with the conditions of the plating treatment, but the method of controlling the specular gloss on the roughened surface is also as described above. That is, in the surface-treated copper foil of the present invention, the specular glossiness on the roughened surface is the average value of the height (h) of the roughened particles, and the particle height (h) to the particle width (w) of the roughened particles.
  • the average value of the ratio (h / w) and the line shape factor (c) of the roughened particles are values that comprehensively reflect the characteristics of the particle shape of the roughened particles, and in particular, the values of the roughened particles The value roughly correlates to the product of the average value of the ratio (h / w) of the particle height (h) to the particle width (w) and the line coverage (c) of the roughened particles.
  • composition of the plating solution for roughening plating treatment and the electrolytic conditions will be shown.
  • the following conditions are a preferable example and the kind and quantity of an additive, and electrolysis conditions can be suitably changed and adjusted as needed in the range which does not prevent the effect of this invention.
  • the surface-treated copper foil of the present invention has a roughening treatment layer having a predetermined fine uneven surface shape, which is formed by electrodeposition of roughening particles on at least one surface of the copper foil substrate, Directly or via an intermediate layer such as a nickel (Ni) -containing underlayer, a zinc (Zn) -containing heat-resistant layer, and a chromium (Cr) -containing anticorrosion layer on the roughened layer.
  • a silane coupling agent layer may further be formed.
  • middle layer and a silane coupling agent layer are very thin, they do not affect the particle shape of the roughening particle
  • the particle shape of the roughened particles in the roughened surface of the surface-treated copper foil is substantially determined by the particle shape of the roughened particles in the surface of the roughened layer corresponding to the roughened surface.
  • a silane coupling agent solution is applied directly or through an intermediate layer on the uneven surface of the roughened layer of the surface-treated copper foil, and then air-dried ( Methods of forming by natural drying) or heat drying can be mentioned.
  • the applied coupling agent solution when the water in the solution evaporates, the effect of the present invention is sufficiently exhibited by the formation of a silane coupling agent layer. Heating and drying at 50 to 180 ° C. is preferable in that the reaction between the silane coupling agent and the copper foil is promoted.
  • the silane coupling agent layer is any one of epoxy based silane, amino based silane, vinyl based silane, methacrylic based silane, acrylic based silane, styryl based silane, ureido based silane, mercapto based silane, sulfide based silane and isocyanate based silane. It is preferable to contain more than species.
  • it is selected from an underlayer containing Ni, a heat-resistant layer containing Zn, and an anticorrosion layer containing Cr between the roughened layer and the silane coupling agent layer. It is preferred to have at least one intermediate layer.
  • the underlayer containing Ni is preferably formed of at least one selected from nickel (Ni), nickel (Ni) -phosphorus (P), and nickel (Ni) -zinc (Zn).
  • the heat-resistant layer containing Zn is preferably formed when it is necessary to further improve the heat resistance.
  • the heat-resistant layer containing Zn is, for example, zinc or an alloy containing zinc, that is, zinc (Zn) -tin (Sn), zinc (Zn) -nickel (Ni), zinc (Zn) -cobalt (Co) And an alloy containing at least one kind of zinc selected from zinc (Zn) -copper (Cu), zinc (Zn) -chromium (Cr) and zinc (Zn) -vanadium (V) preferable.
  • the anticorrosion layer containing Cr is preferably formed when it is necessary to further improve the corrosion resistance.
  • the rustproofing layer include a chromium layer formed by chromium plating and a chromate layer formed by chromate treatment.
  • (S4) Step of Forming Antirust Treatment Layer An anticorrosion treatment layer containing Cr if necessary is formed on the roughening treatment layer or on the underlayer and / or the heat-resistant treatment layer optionally formed on the roughening treatment layer.
  • (S5) Step of Forming a Silane Coupling Agent Layer An intermediate layer in which a silane coupling agent layer is directly formed on the roughened layer, or at least one of an underlayer, a heat-resistant layer and an anticorrosive layer is formed. Form a silane coupling agent layer.
  • the surface-treated copper foil of this invention is used suitably for manufacture of a copper clad laminated board.
  • a copper-clad laminate is suitably used for the production of a printed wiring board excellent in high adhesion and high frequency transmission characteristics, and exhibits excellent effects.
  • the surface-treated copper foil of the present invention is suitable, for example, when it is used as a printed wiring board for high frequency bands of 40 GHz or more, particularly 60 GHz or more.
  • a copper clad laminated board can be formed by a well-known method using the surface-treated copper foil of this invention.
  • a surface-treated copper foil and a resin substrate are laminated and attached such that the roughened surface (adhesion surface) of the surface-treated copper foil faces the resin substrate.
  • the insulating substrate include a flexible resin substrate and a rigid resin substrate, but the surface-treated copper foil of the present invention is particularly suitable in combination with the rigid resin substrate.
  • a copper-clad laminate in the case of producing a copper-clad laminate, it may be produced by bonding a surface-treated copper foil having a silane coupling agent layer and an insulating substrate by a heat press. In addition, it is manufactured by applying a silane coupling agent on an insulating substrate and bonding the insulating substrate on which the silane coupling agent is applied and a surface-treated copper foil having an antirust treatment layer on the outermost surface by a heating press.
  • the copper clad laminate also has the same effect as the present invention.
  • a printed wiring board can be formed by a well-known method using the said copper clad laminated board.
  • Specular gloss Gs 60.degree. 365.8 to 412.1%
  • a roll-shaped electrolytic copper foil double-sided glossy foil having an 85-degree specular gloss Gs (85 °) of 121.5 to 125.7% and a thickness of 18 ⁇ m was produced.
  • ten-point average roughness Rzjis and specular glossiness in M surface of an electrolytic copper foil are the values measured on the conditions similar to the surface-treated copper foil mentioned later. Details will be described in the section of the evaluation method described later.
  • ⁇ Cathode and Anode> Cathode: A titanium rotating drum whose roughness has been adjusted by buffing from # 1000 to # 2000 Anode: Dimensionally stable anode DSA (registered trademark) ⁇ Electrolyte composition> Cu: 80 g / L H 2 SO 4 : 70 g / L Chlorine concentration: 25 mg / L (Additive) -Sodium 3-mercapto-1-propanesulfonate: 2 mg / L ⁇ Hydroxyethyl cellulose: 10 mg / L ⁇ Low molecular weight glue (molecular weight 3000): 50 mg / L ⁇ Electrolysis condition> Bath temperature: 55 ° C Current density: 45A / dm 2
  • Example 1 In Example 1, the following steps [1] to [3] were performed to obtain a surface-treated copper foil. Details will be described below.
  • Roughening plating treatment (1) uses the following roughening plating solution basic bath composition, copper concentration and molybdenum (Mo) concentration as shown in Table 1 below, and processing speed, processing direction interpolar flow rate, current The density and treatment time were as shown in Table 1 below.
  • the molybdenum (Mo) concentration was adjusted by adding and dissolving disodium molybdate (VI) dihydrate to the roughening plating solution basic bath.
  • a fixed plating process (2) continuously it carried out as processing speed, the flow velocity between electrodes, current density, and processing time as described in the following Table 1 using the following fixed plating solution composition.
  • the fixed plating process was not performed, it advanced to the process of following [2].
  • Example 2 to 9 and Comparative Examples 1 to 7 the M surface having the ten-point average roughness Rzjis and the specular glossiness shown in the above Table 1 was used as a copper foil substrate in the roughening treatment layer formation step [1].
  • the conditions of roughening plating treatment (1) and fixed plating treatment (2) were as described in Table 1 above using the electrodeposited copper foil of the above production example. , Surface-treated copper foil was obtained.
  • the processed surface of the surface-treated copper foil exposed on the surface of the prepared measurement sample was exposed to the acceleration voltage of 3 kV from the vertical direction of the processed surface using a scanning electron microscope ("SU 8020" manufactured by Hitachi High-Technologies Corporation) A secondary electron image at 50,000 ⁇ magnification is observed, and a cross-sectional photograph (SEM image, 1.89 ⁇ m long ⁇ 2.54 ⁇ m wide) near the roughened surface is prepared.
  • SU 8020 manufactured by Hitachi High-Technologies Corporation
  • the ratio (h) of the particle height (h) to the particle height (h), particle width (w) and particle width (w) of roughened particles in the region of 2.5 ⁇ m in the width direction of the observation field of view Each average value of h / w) and the linear density (d) and the linear coverage (c) of roughened particles are determined.
  • the analysis up to here is carried out at 10 arbitrary cross sections for the same surface treated copper foil. And based on each measured value of a total of 10 cross-sectional photographs, the average value of the particle height (h) of the roughened particles, the average value of the particle width (w), the particle height (h) to the particle width (w) The average value of the ratio (h / w), the average value of the linear density (d) and the linear coverage (c) was calculated, and the average value was taken as the measured value of the surface-treated copper foil to be observed. .
  • the measured values of the surface-treated copper foil of each of the examples and the comparative examples are shown in Table 2.
  • a ten-point average roughness Rzjis (defined by JIS B 0601: 2001) using a contact-type surface roughness measuring machine ("Surfcoder SE1700" manufactured by Kosaka Laboratory Ltd.) ( ⁇ m) was measured in a direction perpendicular to the longitudinal direction (conveying direction) of the surface-treated copper foil.
  • the ten-point average roughness Rzjis ( ⁇ m) in the M plane of the electrodeposited copper foil prepared in the above production example was also measured under the same conditions.
  • the transmission loss in the high frequency band was measured as an evaluation of the high frequency characteristics. Details will be described below.
  • the obtained copper-clad laminate was subjected to circuit processing to produce a circuit board on which a microstrip line having a transmission path width of 300 ⁇ m and a length of 70 mm was formed.
  • a high frequency signal was transmitted to the transmission path of this circuit board using a network analyzer ("N5247A" manufactured by Keysight Technologies), and the transmission loss was measured.
  • the characteristic impedance was 50 ⁇ .
  • the measured value of transmission loss means that the smaller the absolute value, the smaller the transmission loss and the better the high frequency characteristics.
  • the high frequency characteristics were evaluated based on the following evaluation criteria using the obtained measured value as an index.
  • Peeling strength when the circuit wiring portion (copper foil portion) of 10 mm width of this circuit wiring board is peeled from the resin base at a speed of 50 mm / min in the direction of 90 degrees using a Tensilon tester manufactured by Toyo Seiki Co., Ltd. was measured. The adhesion was evaluated based on the following evaluation criteria using the obtained measured value as an index. ⁇ Evaluation criteria for normal adhesion> ⁇ : Peeling strength is 0.55 kN / m or more ⁇ : Peeling strength is 0.50 kN / m or more and less than 0.55 kN / m ⁇ : Peeling strength is less than 0.50 kN / m
  • the roughened surface has an average value of the particle height (h) of the roughened particles of 0. 05 to 0.30 ⁇ m, the average value of the ratio (h / w) of the particle height (h) to the particle width (w) of the roughening particles is 0.7 to 5.0, and the line coverage of the roughening particles Since (c) is controlled to be 15 to 60%, it was confirmed that the high-frequency characteristics are excellent and high adhesion (normal adhesion and heat-resistant adhesion) is exhibited.
  • the average value of the particle height (h) of the roughened particles is 0.05 to 0.30 ⁇ m
  • the particle width of the roughened particles is at least one of an average value of 0.7 to 5.0 and a linear coverage (c) of the roughened particles of 15 to 60% It was confirmed that one or both of the high frequency characteristics and the adhesion (particularly heat resistant adhesion) are inferior to the surface-treated copper foils of Examples 1 to 9 because

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Abstract

L'invention concerne une feuille de cuivre traitée en surface portant, sur au moins une surface d'un substrat de type feuille de cuivre, un film de revêtement de traitement de surface qui comprend une couche de rugosification qui est pourvue de particules de rugosification. Si une section transversale de cette feuille de cuivre traitée en surface est examinée à l'aide d'un microscope électronique à balayage (MEB), la surface de ce film de revêtement de traitement de surface a une moyenne des hauteurs de particule (h) des particules de rugosification de 0,05 à 0,30 µm, une moyenne des rapports (h/w) des hauteurs de particule (h) sur les largeurs de particule (w) des particules de rugosification de 0,7 à 5,0 et une couverture de ligne (c), telle que calculée par la formule (1), des particules de rugosification de 15 à 60 %. (1) : c = d × W × 100 (%)
PCT/JP2018/044622 2017-12-05 2018-12-04 Feuille de cuivre traitée en surface et stratifié cuivré et carte de circuit imprimé utilisant chacun celle-ci WO2019111914A1 (fr)

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CN201880078041.9A CN111655908B (zh) 2017-12-05 2018-12-04 表面处理铜箔以及使用该表面处理铜箔的覆铜层叠板和印刷布线板
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