WO2005095951A1 - 銅箔粗化面の接着強度の評価方法 - Google Patents
銅箔粗化面の接着強度の評価方法 Download PDFInfo
- Publication number
- WO2005095951A1 WO2005095951A1 PCT/JP2005/006295 JP2005006295W WO2005095951A1 WO 2005095951 A1 WO2005095951 A1 WO 2005095951A1 JP 2005006295 W JP2005006295 W JP 2005006295W WO 2005095951 A1 WO2005095951 A1 WO 2005095951A1
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- WIPO (PCT)
- Prior art keywords
- copper foil
- adhesive strength
- area
- roughened surface
- measured
- Prior art date
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Classifications
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- 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
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- G—PHYSICS
- G01—MEASURING; TESTING
- G01B—MEASURING LENGTH, THICKNESS OR SIMILAR LINEAR DIMENSIONS; MEASURING ANGLES; MEASURING AREAS; MEASURING IRREGULARITIES OF SURFACES OR CONTOURS
- G01B11/00—Measuring arrangements characterised by the use of optical techniques
- G01B11/30—Measuring arrangements characterised by the use of optical techniques for measuring roughness or irregularity of surfaces
- G01B11/303—Measuring arrangements characterised by the use of optical techniques for measuring roughness or irregularity of surfaces using photoelectric detection means
-
- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N19/00—Investigating materials by mechanical methods
- G01N19/04—Measuring adhesive force between materials, e.g. of sealing tape, of coating
-
- 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
- H05K2201/00—Indexing scheme relating to printed circuits covered by H05K1/00
- H05K2201/03—Conductive materials
- H05K2201/0332—Structure of the conductor
- H05K2201/0335—Layered conductors or foils
- H05K2201/0355—Metal 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
- H05K2203/00—Indexing scheme relating to apparatus or processes for manufacturing printed circuits covered by H05K3/00
- H05K2203/16—Inspection; Monitoring; Aligning
- H05K2203/162—Testing a finished product, e.g. heat cycle testing of solder joints
Definitions
- the present invention relates to a method for evaluating the adhesive strength of a copper foil roughened surface.
- Copper foil is widely used as a material for forming printed wiring boards and the like. Since the printed wiring board is obtained by bonding a copper foil to another material such as a pre-preda, it is preferable that the adhesive strength between the copper foil and the pre-preda is high.
- a rough surface and a Z or gloss surface of an untreated copper foil may be provided with, for example, a roughness R measured by a stylus type roughness meter.
- a surface-treated copper foil is produced from the untreated copper foil, and a pre-preparation of the bump on the roughened surface is performed.
- a method that uses the anchor effect on the like has been used. Since the anchor effect is generated based on the bite of the bumps on the prepreg or the like, the adhesive strength between the copper foil roughened surface and the prepreg or the like generally indicates the size of the bumps and the roughened copper foil. It is thought that the surface roughness increases with the increase of the roughness R.
- a method of evaluating the adhesive strength between the rough surface of the copper foil and the pre-preda or the like using Z or the like has been performed.
- the adhesive strength may not be the same and the adhesive strength may vary. For this reason, the roughness R measured with a stylus-type roughness meter as described above
- Patent Document 1 Japanese Patent Application Laid-Open No. Hei 10-265991 discloses that a plating material having a plating film such as Cu formed on the surface of a metal plate is treated with an electron beam three-dimensional roughness analyzer.
- the arithmetic average roughness (Ra) is 0.03 to 0. based on the plating material surface obtained by magnifying 3000 times, and (measurement force)
- the alternative surface area defined as (vertical x horizontal) is 1.01 ⁇ : L1.
- An object of the present invention is to provide a metal material having adhesiveness to resin by setting the arithmetic mean roughness (Ra) and the surface area substitute value in appropriate ranges.
- Patent Document 1 Japanese Patent Application Laid-Open No. 10-265991 (page 2, column 1)
- an object of the present invention is to accurately measure the adhesive strength of a copper foil roughened surface from parameters such as the roughness of the copper foil roughened surface without actually measuring the adhesive strength of the copper foil roughened surface.
- An object of the present invention is to provide a method for evaluating the adhesive strength of a roughened copper foil surface, which can be well estimated. Means for solving the problem
- the present inventors have conducted intensive studies, and as a result, the three-dimensional surface area A (S) obtained by three-dimensionally measuring the surface area of the roughened surface of the copper foil sample S with a laser microscope.
- the area coefficient C (S) calculated by A (S) / B (S) from the measurement area B (S) which is the area of the measurement area of the three-dimensional surface area A (S)
- the method for evaluating the adhesive strength according to the present invention includes the three-dimensional surface area A (S) obtained by three-dimensionally measuring the surface area of the roughened surface of the copper foil sample S with a laser microscope, and The area coefficient C (S) defined by A (S) ZB (S) is determined from the measurement area B (S), which is the area of the measurement area of the three-dimensional surface area A (S), and the area coefficient C ( S) is applied to a calibration curve R indicating the relationship between the area coefficient C and the adhesive strength P obtained in advance on the roughened surface of the same type of copper foil as the copper foil sample S, and the calculated adhesive strength P (R) is obtained.
- An object of the present invention is to provide a method for evaluating the adhesive strength of a roughened surface of a copper foil, which is evaluated as strength.
- the laser used in the laser microscope is a violet laser having a visible light limit wavelength of 405 nm to 410 nm, wherein the copper foil has a roughened surface. It provides a method for evaluating strength.
- the copper foil sample S has a roughness R (S) of 1.0 on the roughened surface measured using a stylus type roughness meter. / ⁇ ⁇ 5. O / zm with copper foil
- Another object of the present invention is to provide a method for evaluating the adhesive strength of a roughened copper foil surface.
- the copper foil sample S is a copper foil having a thickness of 70 ⁇ m or less, wherein the copper foil sample S has an adhesive strength of a roughened copper foil surface. It provides an evaluation method for
- the method for evaluating the adhesive strength of the copper foil roughened surface according to the present invention includes calculating the roughened surface of the copper foil sample S obtained from the area coefficient C (S) measured using a laser microscope. Since the measured bond strength P (R) and the measured bond strength P (S), which is the measured bond strength of the roughened surface of the copper foil sample S, are very similar, the measured bond strength P (S) was not measured. However, the adhesive strength of the copper foil sample S can be accurately estimated.
- the copper foil used for the copper foil sample S in the present invention is a surface-treated copper foil in which a roughened surface is formed by performing a roughening treatment on a rough surface and a Z or gloss surface of an untreated copper foil.
- the surface-treated copper foil may be an untreated copper foil before the roughening treatment, or may be a deviation from an electrolytic copper foil or a rolled copper foil.
- the copper foil is a surface-treated copper foil obtained by subjecting the roughened surface and the Z or glossy surface of the untreated electrolytic copper foil to a roughening treatment such as a bump treatment, it is determined from the area coefficient C (S).
- the approximation between the calculated adhesive strength P (R) of the roughened surface of the copper foil sample S and the measured adhesive strength P (S), which is the measured adhesive strength of the roughened surface of the copper foil sample S, is high. This is preferable because the accuracy is easily obtained.
- the roughness R 1S measured by a stylus type roughness meter is usually 1. ⁇ ⁇
- the surface-treated copper foil has an area coefficient C (S)
- the roughness R measured with a stylus type roughness meter is a stylus using a stylus whose tip is a diamond ball with a diameter of 2 m.
- the value measured with a formula roughness meter is ⁇ ⁇ .
- the copper foil used for the copper foil sample S in the present invention is a surface-treated copper foil having a thickness of usually 70 m or less, preferably 35 ⁇ m or less, and more preferably 12 ⁇ m to 18 ⁇ m. . If the thickness of the copper foil is within the above range, the conformability of the roughened surface of the copper foil to the adhesive layer is within an appropriate range. Therefore, the roughness of the copper foil sample S obtained from the area coefficient C (S) is determined.
- the calculated adhesive strength P (R) of the dangling surface and the measured adhesive strength P (S), which is the actual measured value of the adhesive strength of the roughened surface of the copper foil sample S, are preferably approximate because of high accuracy.
- the laser microscope used in the present invention is a laser microscope capable of 3D analysis. There is no particular limitation as long as a three-dimensional surface area A (S) and a measurement area B (S) described later can be measured. If the laser used in the laser microscope is a violet laser having a visible light limit wavelength of 405 nm to 410 nm, the calculated adhesive strength P (R) of the roughened surface of the copper foil sample S obtained from the area coefficient C (S) And the actual measured adhesive strength P (S), which is the actual measured value of the adhesive strength of the roughened surface of the copper foil sample S, are preferable because the accuracy tends to be particularly high.
- the three-dimensional surface area A obtained by three-dimensionally measuring the surface area of the roughened surface of the copper foil sample S with a laser microscope is described.
- the three-dimensional surface area A (S) is a surface area obtained by three-dimensionally measuring a roughened surface in a measurement area of the copper foil sample S with a laser microscope, and The surface area of the copper foil sample S including the roughness is obtained by moving the focal point by moving the lens of the laser microscope in the Z-axis direction.
- the three-dimensional surface area A (S) indicates the three-dimensional surface area A obtained for the copper foil sample S.
- the shape of the measurement area is not particularly limited, and examples thereof include a square and a rectangle.
- the measurement area B (S) is the area of the measurement area of the three-dimensional surface area A (S), and the measurement area B (S) is obtained for the copper foil sample S. Indicates that the measurement area is B.
- the area coefficient (3) is determined by dividing the three-dimensional surface area A (S) by the measurement area B (S) (A (S) 7 (3)). Since the three-dimensional surface area A (S) does not become smaller than the measurement area B (S), the area coefficient C (S) takes a value of 1 or more. In the present invention, the area coefficient C (S) indicates the area coefficient C obtained for the copper foil sample S.
- the method for evaluating the adhesive strength of a roughened surface of a copper foil according to the present invention is as follows: by applying an area coefficient C (S) to a calibration curve R to obtain a calculated adhesive strength P (R),
- the measured adhesive strength P (S) which is an actual measured value of the adhesive strength of the roughened surface of the foil sample S, is measured instead of the measured adhesive strength P (S) without measuring the copper.
- the calibration curve R is an aggregate of data indicating the relationship between the area coefficient C and the adhesive strength P, which is obtained in advance for the same type of copper foil as the copper foil sample S.
- the calibration curve R is obtained, for example, as a graph having a curve force having a shape that is upwardly convex and monotonically increases in coordinates where the horizontal axis is the area coefficient C and the vertical axis is the adhesive strength P.
- the calculated adhesive strength P (R) is obtained from the area coefficient C (S), and the copper foil sample S
- the measured adhesive strength P (S) which is an actual measured value of the adhesive strength of the roughened surface of the copper foil sample, was used instead of the measured adhesive strength P (S). Is evaluated as the adhesive strength of the roughened surface.
- the measured adhesive strength P (S) is a value obtained when the adhesive strength of the roughened surface of the copper foil sample S is actually measured.
- the calculated adhesive strength P (R) is calculated, and the calculated adhesive strength P (R) is evaluated as the measured adhesive strength P (S). There is no need to measure S).
- the calibration curve R is defined such that the horizontal axis represents the area coefficient C and the vertical axis represents the adhesive strength P.
- the graph has a curve force that is convex upward and has a monotonically increasing shape
- ⁇ , ⁇ , and ⁇ ⁇ on the calibration curve R indicate the values of the area coefficient C (S) on the vertical axis.
- a numerical value is obtained, and this is set as a calculated adhesive strength P (R), and the calculated adhesive strength P (R) is evaluated as the adhesive strength of the roughened surface of the copper foil sample S.
- the copper foil and copper foil sample S for which the calibration curve R was created is the same kind of copper foil is that the copper foil and the copper foil sample S for which the calibration curve R was created are the same as those of the copper foil sample S.
- the difference in the type of electrolytic copper foil or rolled copper foil in untreated copper foil is the same, and the difference in normal tensile strength, normal elongation, 180 ° C hot tensile strength and 180 ° C hot elongation of untreated copper foil is Each must be within ⁇ 30%, the difference in thickness of untreated copper foil must be within ⁇ 30%, and the type of surface treatment when using surface-treated copper foil must be the same.
- the copper foil sample S is an untreated copper foil, an HTE foil (hot elongation of 20% or more) corresponding to class 3 specified in IPC-MF-150F, and an electrolytic copper foil having a thickness of 18 m.
- the calibration curve R if the surface treatment performed on the untreated copper foil forms copper bumps, the calibration curve R Similarly, the untreated copper foil is the above-mentioned HTE foil and is an electrolytic copper foil having a thickness of 18 / zm, and the normal tensile strength, the normal elongation, the 180 ° C hot tensile strength, and the 180 ° C The difference in the hot elongation must be within ⁇ 30%, and the surface treatment performed on the untreated copper foil must form copper bumps.
- the roughness of the untreated copper foil or the roughness of the roughened surface of the surface-treated copper foil need not be the same.
- the roughness means R measured by a stylus type roughness meter.
- the adhesive strength of the copper foil sample S estimated using the calculated adhesive strength P (R) as described above is determined for the same adhesive layer as the adhesive layer used in preparing the calibration curve R. This is the adhesive strength estimated only when copper foil sample S was used.
- the adhesive layer of the copper foil sample S is of the same type as the adhesive layer used in preparing the calibration curve R is defined as the adhesive layer used in preparing the calibration curve R (hereinafter, also referred to as “adhesive layer R”).
- bonding layer S the adhesive layer to which the copper foil sample S is to be bonded in terms of the types of the base material and the resin constituting the adhesive layer, respectively.
- the difference between the bonding layer R and the bonding layer S in the mixing ratio of the base material in the bonding layer is within ⁇ 30%, and the bonding layer R and the bonding layer S in the mixing ratio of the resin in the bonding layer are within ⁇ 30%.
- the temperature, temperature rise rate, time, and time are within ⁇ 30%, and the pressing conditions for forming the adhesive layer by applying pressure and pressure from the copper foil and the pre-preder. It means that the difference between the adhesive layer R and the adhesive layer S under each condition such as pressure is within ⁇ 30%.
- the fact that the types of base materials have the same identity in the present invention corresponds to any of the base materials of the adhesive layer classified as glass fiber, paper, or no base.
- the phrase "the types of resins have the same identity” means that epoxy resins, phenol resins, polyimides, bismaleimide triazine resins (BT resins), arylipolypolyphenylene oxide resins. Any of the adhesive layer resins classified as (PPE resin) It is determined whether or not to do. For example, when the type of resin of the adhesive layer R is epoxy resin, if the type of resin of the adhesive layer S is epoxy resin, it is determined that the resin has the same identity, and the type of resin of the adhesive layer S is It is determined that the phenolic resin does not have the same identity. As described above, in the present invention, the identity of the type of resin is determined based on the type of resin.
- the resin is epoxy resin
- the resin of the adhesive layer R and the resin of the adhesive layer S are different.
- the same type of resin even if there is a difference in the basic skeleton such as bisphenol A type and novolak type in epoxy resin, the difference in curing agent, and the difference in the physical properties of epoxy resin. Is judged to have the property.
- the adhesive layer (adhesive layer R) force used for preparing the calibration curve R is a pre-preda containing a glass base material and an epoxy resin in a predetermined blending ratio, and the copper foil used for preparing the calibration curve R
- the present invention when the pressing conditions of the prepreg and the prepreg are performed under predetermined conditions, the present invention relates to a prepreg containing a glass base material and an epoxy resin whose mixing ratio is within ⁇ 30% of the predetermined mixing ratio. , Pressing conditions such as temperature, heating rate, time, pressure, etc.
- the calculated adhesive strength P (R) of the roughened surface of the copper foil sample S obtained from the area coefficient C (S) and the adhesive strength of the roughened surface of the copper foil sample S The approximation to the measured bond strength P (S), which is the measured value of P, is highly accurate, and even if the measured bond strength P (S) is not measured, the calculated bond strength P (R) is It can be evaluated as the adhesive strength of the dangling surface.
- the adhesive strength of the roughened surface of the copper foil sample S can be accurately estimated from the calculated adhesive strength P (R). .
- the method for evaluating the adhesive strength of a roughened surface of a copper foil according to the present invention is described, for example, in the case of producing a printed wiring board or the like. It can be used for evaluation of the adhesive strength of the surface.
- an untreated copper foil roll of electrolytic copper foil (Super HTE manufactured by Mitsui Kinzoku Mining Co., Ltd., thickness 18 m) was used.
- the surface treatment equipment includes an acid pickling tank, a one-step roughening tank, a washing tank, a two-step roughening tank, a washing tank, and a hot-air dryer.
- Surface treatment An apparatus capable of continuously producing copper foil was used.
- an anode was arranged at a position opposed to the rough side of the copper foil at a certain distance from the copper foil.
- two anodes are arranged apart from each other in the flow direction of the copper foil, and of the two anodes, the anode on the unwinding side of the copper foil is defined as a first-stage roughened anode,
- the anode on the take-up side was used as a post-stage roughing treatment anode.
- an anode was arranged at a position opposite to the copper foil at a certain distance from the rough surface side of the copper foil.
- the two anodes are arranged apart from each other in the flow direction of the copper foil, and among the two anodes, the anode on the unwinding side of the copper foil is used as a two-stage pre-roughening anode, and the copper foil is wound.
- the anode on the removal side was the second-stage roughened anode.
- the pickling tank, the first-stage roughening tank, and the two-step roughening tank of the above surface treatment equipment had the following composition, respectively.
- the processing solution was filled with the 1st-stage roughening solution (1st-stage roughening solution A) and 2nd-stage roughening solution (2nd-stage roughening solution A), and the two washing tanks were both filled with pure water. .
- Dilute sulfuric acid was prepared by adding sulfuric acid to pure water.
- the first-stage roughening solution A having the following composition.
- two-stage roughening solution A having the following composition.
- the untreated copper foil is continuously unwound at a constant speed, and the untreated copper foil is subjected to pickling treatment, one-step roughening treatment, water washing under the following conditions. Step roughening treatment, water washing and drying treatment were performed to obtain a surface-treated copper foil.
- the untreated copper foil was immersed in the pickling solution for 5 seconds.
- a one-stage roughening treatment was performed.
- Table 1 shows the electrolysis conditions.
- the roughening treatment using the first-stage roughening anode of the above surface treatment equipment is referred to as the first-stage roughening treatment, and the roughening treatment performed using the first-stage roughening anode is the first-stage roughening treatment. It was processed.
- the copper foil after the one-step roughing treatment was immersed in pure water for 5 seconds.
- a two-stage roughening treatment was performed.
- Table 2 shows the electrolysis conditions.
- the roughening treatment using the two-stage pre-roughening anode of the above surface treatment equipment is referred to as the two-stage pre-roughening treatment, and the roughening treatment performed using the two-stage post-roughening anode is the second-stage roughening treatment. It was processed.
- the copper foil after the two-stage roughing treatment was immersed in pure water for 5 seconds.
- the copper foil after the two-stage roughening treatment was dried using a hot-air dryer.
- the area and the measured adhesive strength were measured.
- an area coefficient was calculated from the three-dimensional surface area and the area of the measurement area in the measurement of the three-dimensional surface area, and the calculated area strength was calculated by applying the area coefficient to the following calibration curve R. Table 3 shows the results.
- the calibration curve R shown was constructed.
- the calibration curve R was represented by the following equation (1).
- Fig. 3 shows the calibration curve R.
- the obtained surface-treated copper foil (copper foil sample S) was also cut into square samples of 100 mm in length and 100 mm in width.
- a narrow rectangular strip of 0.8 mm wide ⁇ 100 mm long is placed on the dry film resist side of the single-sided copper clad laminate.
- a mask film having a plurality of shaped slits is placed thereon, and a latent image is formed on the exposed dry film resist portion by exposing it to ultraviolet light, and then a KOH aqueous solution is sprayed onto the single-sided copper-clad laminate for development. The latent image was cured and the unexposed portions of the dry film resist were removed.
- the dry film resist is removed and the exposed copper foil portion is etched by spraying the salted copper on the single-sided copper-clad laminate, an aqueous NaOH solution is sprayed on the cured dry film resist portion.
- the portion was peeled off, and a plurality of rectangular circuits having a line width of 0.8 mm and a length of 100 mm were formed on the glass cloth substrate epoxy resin plate.
- the single-sided copper-clad laminate was cut so as to be separate for each circuit, and a plurality of samples for measuring the adhesive strength in which one rectangular circuit having a line width of 0.8 mm and a length of 100 mm were formed. did.
- a portion of the sample for measuring adhesive strength which is about several mm inside one end force in the length direction, is bent in a direction substantially perpendicular to the length direction of the rectangular circuit so that the rectangular circuit is inside. Only the substrate portion was cut, and a sample for measuring adhesive strength in a state where the rectangular circuits were connected and the substrate portion was cut was produced.
- the adhesive strength measurement sample is placed on a peel strength measuring machine such that the rectangular circuit faces upward, and the sample is fixed. After the base material portion is cut, the peel strength measurement is performed. I was caught in the chuck of the machine. Next, the chuck is pulled up at a constant speed, the rectangular circuit is peeled off from the substrate of the adhesive strength measurement sample, and the peeling strength is measured, and the maximum value at that time is measured for the surface-treated copper foil ( The measured adhesive strength of the roughened surface of the copper foil sample S) was used.
- a surface-treated copper foil was obtained in the same manner as in Production Example 1, except that the electrolysis conditions for the one-step roughening treatment and the two-step roughening treatment were changed as shown in Tables 1 and 2.
- Roughened surface of the obtained surface-treated copper foil The roughness R, the three-dimensional surface area, and the measured adhesive strength were measured in the same manner as in Production Example 1.
- a surface-treated copper foil was obtained in the same manner as in Production Example 1, except that the electrolysis conditions for the one-step roughening treatment and the two-step roughening treatment were changed as shown in Tables 1 and 2.
- the roughness R, the three-dimensional surface area, and the measured adhesive strength were measured in the same manner as in Production Example 1.
- a surface-treated copper foil was obtained in the same manner as in Production Example 1, except that the electrolysis conditions for the one-step roughening treatment and the two-step roughening treatment were changed as shown in Tables 1 and 2.
- the roughness R, the three-dimensional surface area, and the measured adhesive strength were measured in the same manner as in Production Example 1.
- a surface-treated copper foil was obtained in the same manner as in Production Example 1, except that the electrolysis conditions for the one-step roughening treatment and the two-step roughening treatment were changed as shown in Tables 1 and 2.
- the roughness R, the three-dimensional surface area, and the measured adhesive strength were measured in the same manner as in Production Example 1.
- a surface-treated copper foil was obtained in the same manner as in Production Example 1, except that the electrolysis conditions for the one-step roughening treatment and the two-step roughening treatment were changed as shown in Tables 1 and 2.
- the roughness R, the three-dimensional surface area, and the measured adhesive strength were measured in the same manner as in Production Example 1.
- a one-stage roughening treatment solution (one-stage roughening treatment solution B) having the following composition was prepared, and the one-stage roughening treatment solution was replaced with the one-stage roughening treatment solution A.
- a surface-treated copper foil was obtained in the same manner as in Production Example 1, except that B was used and the electrolysis conditions for the one-step roughening treatment and the two-step roughening treatment were changed as shown in Tables 1 and 2.
- About the rough surface of the obtained surface-treated copper foil the same as in Production Example 1 Then, measure the roughness R, the three-dimensional surface area and the measured adhesive strength, and calculate the area coefficient and
- one-stage roughening solution B having the following composition.
- the above-mentioned one-stage roughening treatment solution B was used as the one-stage roughening treatment solution, and the electrolysis conditions for the one-stage roughening treatment and the two-stage roughening treatment were changed as shown in Tables 1 and 2. Except for the above, a surface-treated copper foil was obtained in the same manner as in Production Example 1. For the roughened surface of the obtained surface-treated copper foil, the roughness R, the three-dimensional surface area, and the measured adhesive strength were measured in the same manner as in Production Example 1, and the area coefficient and calculation were performed.
- the one-step roughening treatment liquid As the one-step roughening treatment liquid, the above-mentioned one-step roughening treatment liquid B was used, and the electrolysis conditions of the one-step roughening treatment and the two-step roughening treatment were changed as shown in Tables 1 and 2. Except for the above, a surface-treated copper foil was obtained in the same manner as in Production Example 1. For the roughened surface of the obtained surface-treated copper foil, the roughness R, the three-dimensional surface area, and the measured adhesive strength were measured in the same manner as in Production Example 1, and the area coefficient and calculation were performed.
- the above-mentioned one-stage roughening treatment solution B was used as the one-stage roughening treatment solution, and the electrolysis conditions for the one-stage roughening treatment and the two-stage roughening treatment were changed as shown in Tables 1 and 2. Except for the above, a surface-treated copper foil was obtained in the same manner as in Production Example 1. For the roughened surface of the obtained surface-treated copper foil, the roughness R, the three-dimensional surface area, and the measured adhesive strength were measured in the same manner as in Production Example 1, and the area coefficient and calculation were performed.
- the one-stage roughening treatment liquid As the one-stage roughening treatment liquid, the above-mentioned one-stage roughening treatment liquid B was used, and a one-stage roughening treatment and a two-stage A surface-treated copper foil was obtained in the same manner as in Production Example 1, except that the electrolysis conditions for the roughening treatment were changed as shown in Tables 1 and 2.
- the roughness R, the three-dimensional surface area, and the measured adhesive strength were measured in the same manner as in Production Example 1, and the area coefficient and calculation were performed.
- Two-stage roughening solution Two-stage pre-stage roughening process
- Two-stage post-stage roughening process Reverse / night dish Current density Electrolysis time
- Current density Electrolysis time Current density Electrolysis time
- FIG. 1 shows the relationship between the measured adhesive strength and the area coefficient in Production Examples 1 to 11.
- FIG. 1 is a graph showing the relationship between the measured adhesive strength and the area coefficient in Production Examples 1 to 11, with the vertical axis representing the measured adhesive strength (kgfZcm) and the horizontal axis representing the area coefficient.
- FIG. 2 shows the relationship between the measured adhesive strength and R in Production Examples 1 to 11.
- Figure 2 shows the relationship between the measured adhesive strength and R in Production Examples 1 to 11.
- the graph shows the relationship with Z, with the vertical axis representing the measured bonding strength (kgfZcm) and the horizontal axis representing R ( ⁇ m).
- Example 1 ⁇ Confirmation of Effect of Invention in Evaluation Method of Adhesive Strength of Copper Foil Roughened Surface According to the Present Invention> From FIG. 2, in Example 1, all plots of Production Examples 1 to 11 are almost on the same curve. It can be seen that there is a strong correlation between the measured adhesive strength and the area coefficient. That is, a plot group of a group of Production Examples 1 to 6 (hereinafter also referred to as “Group A”) and a plot group of a group of Production Examples 7 to 11 (hereinafter also referred to as “Group B”). This means that, although there is a difference in the one-step roughing process between group A and group B, they are almost on the same curve.
- Group A a plot group of a group of Production Examples 1 to 6
- Group B a plot group of a group of Production Examples 7 to 11
- the method for evaluating the adhesive strength of a roughened copper foil surface according to the present invention can be used to evaluate the adhesive strength of a roughened surface of a surface-treated copper foil used as a raw material for producing a printed wiring board.
- FIG. 1 shows the relationship between the measured adhesive strength and the area coefficient in Production Examples 1 to 11, with the vertical axis representing the measured adhesive strength (kgfZcm) and the horizontal axis representing the area coefficient. It is a graph.
- FIG. 2 is a graph showing the relationship between measured adhesive strength and R in Production Examples 1 to 11.
- 5 is a graph in which the axis is measured adhesion strength (kgfZcm) and the horizontal axis is R ( ⁇ m).
- FIG. 3 is a graph showing a calibration curve R.
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JP2004110486A JP2005292057A (ja) | 2004-04-02 | 2004-04-02 | 銅箔粗化面の接着強度の評価方法 |
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Cited By (2)
Publication number | Priority date | Publication date | Assignee | Title |
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CN103476198A (zh) * | 2012-06-06 | 2013-12-25 | 三菱瓦斯化学株式会社 | 印刷电路板用铜箔及其制法以及使用该铜箔的印刷电路板 |
CN109917007A (zh) * | 2019-04-18 | 2019-06-21 | 广东工业大学 | 一种复合材料胶接界面结合强度的检测方法及设备 |
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CN111257220B (zh) * | 2020-02-26 | 2023-06-06 | 上海景瑞阳实业有限公司 | 一种判断腻子粉粘接强度的方法 |
JP7310753B2 (ja) * | 2020-08-20 | 2023-07-19 | 新東工業株式会社 | 接合強度の推定方法、及び接合強度の推定装置 |
Citations (2)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
JPH08111582A (ja) * | 1994-10-07 | 1996-04-30 | Hitachi Chem Co Ltd | 被接着物の粗面化処理方法 |
JPH08313428A (ja) * | 1995-05-16 | 1996-11-29 | Toyota Motor Corp | 薄膜密着強度評価方法 |
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2004
- 2004-04-02 JP JP2004110486A patent/JP2005292057A/ja active Pending
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- 2005-03-31 TW TW94110268A patent/TWI289420B/zh not_active IP Right Cessation
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Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
JPH08111582A (ja) * | 1994-10-07 | 1996-04-30 | Hitachi Chem Co Ltd | 被接着物の粗面化処理方法 |
JPH08313428A (ja) * | 1995-05-16 | 1996-11-29 | Toyota Motor Corp | 薄膜密着強度評価方法 |
Cited By (3)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
CN103476198A (zh) * | 2012-06-06 | 2013-12-25 | 三菱瓦斯化学株式会社 | 印刷电路板用铜箔及其制法以及使用该铜箔的印刷电路板 |
CN109917007A (zh) * | 2019-04-18 | 2019-06-21 | 广东工业大学 | 一种复合材料胶接界面结合强度的检测方法及设备 |
CN109917007B (zh) * | 2019-04-18 | 2021-07-06 | 广东工业大学 | 一种复合材料胶接界面结合强度的检测方法及设备 |
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JP2005292057A (ja) | 2005-10-20 |
TWI289420B (en) | 2007-11-01 |
TW200538008A (en) | 2005-11-16 |
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