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WO2018180988A1 - 圧延銅箔の表面処理液及び表面処理方法並びに圧延銅箔の製造方法 - Google Patents

圧延銅箔の表面処理液及び表面処理方法並びに圧延銅箔の製造方法 Download PDF

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Publication number
WO2018180988A1
WO2018180988A1 PCT/JP2018/011707 JP2018011707W WO2018180988A1 WO 2018180988 A1 WO2018180988 A1 WO 2018180988A1 JP 2018011707 W JP2018011707 W JP 2018011707W WO 2018180988 A1 WO2018180988 A1 WO 2018180988A1
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WO
WIPO (PCT)
Prior art keywords
copper foil
rolled copper
mass
surface treatment
hydrogen peroxide
Prior art date
Application number
PCT/JP2018/011707
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English (en)
French (fr)
Japanese (ja)
Inventor
昌彌 曽根
裕嗣 松永
聡 玉井
Original Assignee
三菱瓦斯化学株式会社
Priority date (The priority date is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the date listed.)
Filing date
Publication date
Application filed by 三菱瓦斯化学株式会社 filed Critical 三菱瓦斯化学株式会社
Priority to KR1020197027199A priority Critical patent/KR102568740B1/ko
Priority to JP2019509711A priority patent/JP7074127B2/ja
Priority to CN201880021257.1A priority patent/CN110462103A/zh
Publication of WO2018180988A1 publication Critical patent/WO2018180988A1/ja

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    • C—CHEMISTRY; METALLURGY
    • C23—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; CHEMICAL SURFACE TREATMENT; DIFFUSION TREATMENT OF METALLIC MATERIAL; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL; INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL
    • C23F—NON-MECHANICAL REMOVAL OF METALLIC MATERIAL FROM SURFACE; INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL; MULTI-STEP PROCESSES FOR SURFACE TREATMENT OF METALLIC MATERIAL INVOLVING AT LEAST ONE PROCESS PROVIDED FOR IN CLASS C23 AND AT LEAST ONE PROCESS COVERED BY SUBCLASS C21D OR C22F OR CLASS C25
    • C23F1/00—Etching metallic material by chemical means
    • C23F1/10—Etching compositions
    • C23F1/14—Aqueous compositions
    • C23F1/16—Acidic compositions
    • C23F1/18—Acidic compositions for etching copper or alloys thereof
    • Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
    • Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
    • Y02E—REDUCTION OF GREENHOUSE GAS [GHG] EMISSIONS, RELATED TO ENERGY GENERATION, TRANSMISSION OR DISTRIBUTION
    • Y02E60/00—Enabling technologies; Technologies with a potential or indirect contribution to GHG emissions mitigation
    • Y02E60/10—Energy storage using batteries

Definitions

  • the present invention relates to a surface treatment solution for rolled copper foil, a surface treatment method for rolled copper foil using the same, and a method for producing rolled copper foil.
  • Rolled copper foil is used for flexible printed circuit boards (FPC), and has recently been rolled to reduce transmission loss in the high-frequency region, as well as to achieve higher density, thinner thickness, and finer / fine pitch. It is desired to treat copper foil smoothly.
  • FPC flexible printed circuit boards
  • Patent Document 1 a method using azoles, halogen ions and silver ions is known (Patent Document 1).
  • Patent Document 1 a method using azoles, halogen ions and silver ions.
  • etching progresses along the crystal grain boundary, and crater-like etching and pits occur, making it difficult to smooth the surface.
  • the rolled copper foil is known to have excellent flexibility, and the crystal orientation is controlled so that a cubic texture after recrystallization annealing develops in order to improve the flexibility.
  • crystal grains having locally different crystal grain orientations exist in the uniform crystal structure, and the etching rate of the part is different from the surrounding etching rate. It is considered that crater-like etching and pits are formed on the surface (for example, see Patent Documents 2 and 3).
  • Non-Patent Document 1 Non-Patent Document 1
  • the present invention relates to a surface treatment solution and a surface treatment method suitable for surface treatment of a rolled copper foil, and a method for producing the rolled copper foil.
  • the present inventors have found that the above problems can be solved by a surface treatment liquid having a specific composition in which hydrogen peroxide and sulfuric acid are mixed in a specific molar ratio and an alcohol-based additive is added. That is, the present invention is as follows.
  • Hydrogen peroxide (A), sulfuric acid (B), alcohol (C) and phenylurea (D) are contained, and the molar ratio of hydrogen peroxide (A) / sulfuric acid (B) is 0.3-3.
  • this invention is as follows.
  • Hydrogen peroxide (A), sulfuric acid (B), alcohol (C) and phenylurea (D) are contained, and the molar ratio of hydrogen peroxide (A) / sulfuric acid (B) is 0.3-3.
  • the manufacturing method of rolled copper foil including processing a rolled copper foil surface by making a process liquid contact the rolled copper foil surface and dissolving the rolled copper foil surface.
  • [5a] Content of the hydrogen peroxide (A) and phenylurea (D) is within the following ranges, respectively: Hydrogen peroxide (A): 0.5-3.0% by mass Phenylurea (D): 0.005 to 0.3% by mass
  • Phenylurea (D): 0.005 to 0.3% by mass The method for producing a rolled copper foil according to any one of [1a] to [4a].
  • [7a] Hydrogen peroxide (A), sulfuric acid (B), alcohol (C) and phenylurea (D) are contained, and the molar ratio of hydrogen peroxide (A) / sulfuric acid (B) is 0.3-3.
  • Rolling in which the content of sulfuric acid (B) is in the range of 0.5 to 15.0% by mass and the content of alcohol (C) is in the range of 0.1 to 5.0% by mass A surface treatment method for a rolled copper foil, comprising dissolving the surface of the rolled copper foil using a surface treatment solution for copper foil.
  • [11a] Content of the hydrogen peroxide (A) and phenylurea (D) is within the following ranges, respectively: Hydrogen peroxide (A): 0.5-3.0% by mass Phenylurea (D): 0.005 to 0.3% by mass
  • Phenylurea (D): 0.005 to 0.3% by mass The surface treatment method for rolled copper foil according to any one of [7a] to [10a].
  • [14a] Content of the hydrogen peroxide (A) and phenylurea (D) is within the following ranges, respectively: Hydrogen peroxide (A): 0.5-3.0% by mass Phenylurea (D): 0.005 to 0.3% by mass
  • a rolled copper foil having excellent smoothness can be obtained by using the processing solution for rolled copper foil of the present invention.
  • a flexible printed circuit film capable of reducing transmission loss in a high frequency region, increasing the density, reducing the thickness, and further reducing the size and fine pitch is manufactured. be able to.
  • FIG. 10 is a surface observation image by SEM (magnification 1000 times) of Examples 10 to 14.
  • FIG. 6 is a surface observation image by SEM (magnification 1000 times) of Comparative Examples 1 to 6.
  • the method for producing a rolled copper foil of the present invention comprises hydrogen peroxide (A), sulfuric acid (B), alcohol (C) and phenylurea (D), and the molar ratio of hydrogen peroxide (A) / sulfuric acid (B).
  • the ratio is in the range of 0.3 to 3.0
  • the sulfuric acid (B) is in the range of 0.5 to 15.0% by mass
  • the alcohol (C) is in the range of 0.1 to 5.0% by mass.
  • a surface treatment liquid is brought into contact with the rolled copper foil surface to dissolve the rolled copper foil surface, thereby treating the rolled copper foil surface.
  • the surface treatment liquid having the above composition is brought into contact with the surface of the rolled copper foil to dissolve the surface of the rolled copper foil.
  • a rolled copper foil having excellent properties can be obtained.
  • the surface treatment solution for rolled copper foil used in the present invention contains hydrogen peroxide (A), sulfuric acid (B), alcohol (C) and phenylurea (D). These will be described in detail below.
  • Hydrogen peroxide (A) in the present invention is a component that functions as an oxidizing agent for copper.
  • the hydrogen peroxide (A) used in the present invention is not limited, and a commercially available aqueous hydrogen peroxide solution can be used.
  • a 60% industrial / electronic industry grade product manufactured by Mitsubishi Gas Chemical Co., Ltd. is preferably used. can do.
  • the concentration of hydrogen peroxide (A) in the surface treatment liquid is preferably 0.5 to 3.0% by mass, more preferably 0.6 to 2.5% by mass, and particularly preferably 0.8. It is -2.0 mass%. When the concentration of hydrogen peroxide is in the above range, a good copper surface state and a suitable copper dissolution rate can be obtained.
  • the molar ratio of hydrogen peroxide (A) / sulfuric acid (B) is 0.3 to 3.0, preferably 0.4 to 3.0, and more preferably 0.5 to 3. 0.
  • the molar ratio of hydrogen peroxide (A) / sulfuric acid (B) is particularly preferably 0.5 to 0.9.
  • the sulfuric acid (B) in the present invention is a component that functions as an etching agent for copper oxidized by hydrogen peroxide.
  • the sulfuric acid (B) used by this invention For example, 95% special grade reagent made from Wako Pure Chemical Industries Ltd. can be used conveniently.
  • the concentration of sulfuric acid (B) in the surface treatment liquid is 0.5 to 15.0 mass%, preferably 0.6 to 15.0 mass%, and more preferably 1.0 to 5.0 mass%. %. By being in this range, a good copper surface state and a suitable copper dissolution rate can be obtained.
  • the alcohol (C) in the present invention includes all common alcohols, and is a component that improves the smoothness of the rolled copper foil surface.
  • Specific examples of the alcohol (C) include monohydric alcohols such as methanol, ethanol and propanol, dihydric alcohols such as ethylene glycol and propylene glycol, trihydric alcohols and glycol ethers such as polyethylene glycol. Two or more of these can be used in combination.
  • the concentration of the alcohol (C) in the surface treatment liquid is 0.1 to 5.0% by mass, preferably 0.5 to 5.0% by mass. By being in this range, a smooth surface state of the rolled copper foil can be obtained.
  • Phenylurea (D) in the present invention is a component that improves the stability of hydrogen peroxide.
  • limiting in the phenylurea (D) used by this invention For example, Wako Pure Chemical Industries Ltd. phenylurea can be used conveniently.
  • the concentration of phenylurea (D) in the surface treatment liquid is preferably 0.005 to 0.3% by mass, more preferably 0.005 to 0.15% by mass, and still more preferably 0.005 to 0.3% by mass. 0.1% by mass. By being in this range, decomposition of hydrogen peroxide can be suppressed.
  • the smoothness of the surface of rolled copper foil can be made more excellent by adjusting the amount ratio of phenylurea (D) as appropriate.
  • the surface treatment liquid of the present invention can further contain water and other commonly used additives as long as the effects of the present invention are not impaired.
  • a known etching rate adjusting agent such as an alkali, organic carboxylic acid, organic amine compound, or a copper ion supply source may be added as necessary to stabilize the etching rate.
  • the water is preferably one from which metal ions, organic impurities, particle particles, and the like have been removed by distillation, ion exchange treatment, filter treatment, various adsorption treatments, etc., more preferably pure water, and particularly preferably ultrapure water. .
  • the surface treatment solution for rolled copper foil is prepared by uniformly stirring hydrogen peroxide (A), sulfuric acid (B), alcohol (C), phenylurea (D) and other components as required.
  • the surface of the rolled copper foil is treated by bringing the surface treatment liquid into contact with the surface of the rolled copper foil to dissolve the surface of the rolled copper foil.
  • the smoothness of the rolled copper foil surface can be made excellent by processing the rolled copper foil surface using the said surface treatment liquid.
  • the method for bringing the surface treatment liquid into contact with the surface of the rolled copper foil is not particularly limited, and a known method such as dipping or spraying can be employed.
  • the surface treatment liquid for rolled copper foil of this invention can be used for the surface treatment method of the well-known rolled copper foil by immersion, spraying, etc.
  • the rolled copper foil used in the present invention is a generally known rolled copper foil, which is produced by repeating plastic processing and heat treatment of a copper or copper alloy ingot with a rolling roll, and has high flexibility and high crystal orientation. It is a copper foil having properties.
  • the use temperature of the surface treatment liquid is not limited, but is usually 20 to 50 ° C., preferably 25 to 40 ° C., more preferably 25 to 35 ° C.
  • the higher the use temperature of the surface treatment solution the faster the dissolution rate of copper.
  • the temperature exceeds 50 ° C. the decomposition of hydrogen peroxide becomes undesirably severe.
  • the treatment time of the surface of the rolled copper foil with the surface treatment liquid is not limited, but is usually 1 to 600 seconds, preferably 5 to 300 seconds, more preferably 10 to 180 seconds, and particularly preferably 15 to 120 seconds.
  • the dissolution rate of the rolled copper foil by the surface treatment liquid is not limited, but the etching rate (E / R) is usually 0.4 to 4.0 ⁇ m / min, for example, under the treatment condition of 35 ° C., preferably 1 0.0 to 3.5 ⁇ m / min, and 1.5 to 3.0 ⁇ m / min is particularly preferable because the etching time can be shortened.
  • the rolled copper foil of the present invention surface-treated with the surface treatment liquid is excellent in surface smoothness, and therefore can be suitably used for flexible printed wiring boards and the like.
  • SEM scanning electron microscope
  • the brightness of the rolled copper foil before and after the surface treatment was determined using the standard deviation by setting the single-threshold value of the contrast of the concave and convex portions on the surface of the copper foil to 47, using the histogram as the series, and using the standard deviation.
  • the relationship is satisfied, and the smoothness is excellent.
  • the numerical value (%) represented by the above formula is more preferably ⁇ 5% or less, and further preferably ⁇ 10% or less.
  • ⁇ (Luminance of copper foil after treatment) ⁇ (luminance of untreated copper foil) ⁇ / (luminance of untreated copper foil) ⁇ 100% ⁇ (Brightness of copper foil after treatment) ⁇ 28.4 ⁇ /28.4 ⁇ 100% -10% or less: “Excellent” Less than -10% to -5% or less: “Good” -Less than -5% to less than 0% 0% or more: “Not possible”.
  • Etching rate [ ⁇ m / min] (mass before treatment [g] ⁇ 1 mass after treatment [g]) / (treatment area [m 2 ] ⁇ ⁇ specific gravity of copper> 8.92 [g / cm 3 ] )
  • Example 1 Hydrogen peroxide (A) 2.00 g (Mitsubishi Gas Chemical Co., Ltd. 60% hydrogen peroxide), sulfuric acid (B) 8.42 g (Wako Pure Chemical Industries, Ltd. 95% special grade reagent), alcohol (C) 1.00 g (polyethylene glycol 600 (PEG 600) (Wako first grade) manufactured by Wako Pure Chemical Industries, Ltd.), 0.06 g of phenylurea (D) (produced by Wako Pure Chemical Industries, Ltd.), and copper sulfate pentahydrate 23 .60 g (manufactured by Wako Pure Chemical Industries, Ltd.) was weighed, and ultrapure water was added so that the total mass became 200 g, followed by stirring until uniform to prepare a surface treatment solution for rolled copper foil.
  • PEG 600 polyethylene glycol 600
  • D phenylurea
  • D copper sulfate pentahydrate 23 .60 g
  • the rolled copper foil HA-V2 foil cut into a 30 mm square was etched using a surface treatment solution at a stirring speed of 200 rpm and a liquid temperature of 30 ° C., and subjected to a 3 ⁇ m etching process by immersion stirring.
  • the results are shown in Table 1 and FIG.
  • the luminance measurement result is smaller than 28.4 of the untreated substrate, and FIG. 2 shows that the surface is not etched into a crater shape, so that the smoothness is good.
  • Examples 2 to 9 The operation was performed in the same manner as in Example 1 except that the composition was changed to the composition shown in Table 1. The results are shown in Table 1 and FIG. The luminance measurement result is smaller than 28.4 of the untreated substrate, and FIG. 2 shows that the surface is not etched into a crater shape, so that the smoothness is good.
  • Example 10 to 14 The operation was performed in the same manner as in Example 1 except that the composition was changed to the composition shown in Table 1. The results are shown in Table 1 and FIG. The luminance measurement result is smaller than 28.4 of the untreated substrate, and it can be seen from FIG. 3 that the surface is not etched into a crater shape, so that the smoothness is good.
  • Example 6 An experiment was performed in the same manner as in Example 1 except that the composition was changed to the composition shown in Table 3 (Example of Patent Document 1). The results are shown in Table 3 and FIG. Although the surface is not etched into a crater shape from FIG. 4, it can be seen that good smoothness cannot be obtained because the luminance measurement result is larger than 28.4 of the untreated substrate.
  • the rolled copper foil obtained by the production method of the present invention is excellent in surface smoothness, it can be suitably used for a flexible printed wiring board (FPC) or the like.

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  • Chemical & Material Sciences (AREA)
  • Chemical Kinetics & Catalysis (AREA)
  • General Chemical & Material Sciences (AREA)
  • Engineering & Computer Science (AREA)
  • Materials Engineering (AREA)
  • Mechanical Engineering (AREA)
  • Metallurgy (AREA)
  • Organic Chemistry (AREA)
  • ing And Chemical Polishing (AREA)
  • Electroplating Methods And Accessories (AREA)
  • Chemical Treatment Of Metals (AREA)
PCT/JP2018/011707 2017-03-31 2018-03-23 圧延銅箔の表面処理液及び表面処理方法並びに圧延銅箔の製造方法 WO2018180988A1 (ja)

Priority Applications (3)

Application Number Priority Date Filing Date Title
KR1020197027199A KR102568740B1 (ko) 2017-03-31 2018-03-23 압연동박의 표면처리액 및 표면처리방법 그리고 압연동박의 제조방법
JP2019509711A JP7074127B2 (ja) 2017-03-31 2018-03-23 圧延銅箔の表面処理液及び表面処理方法並びに圧延銅箔の製造方法
CN201880021257.1A CN110462103A (zh) 2017-03-31 2018-03-23 压延铜箔的表面处理液及表面处理方法以及压延铜箔的制造方法

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JP2017069910 2017-03-31
JP2017-069910 2017-03-31

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Cited By (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN113981447A (zh) * 2021-11-10 2022-01-28 纳然电子技术(苏州)有限公司 一种蚀刻液
CN115928071A (zh) * 2022-12-02 2023-04-07 江西荣晖电子有限公司 一种pcb用铜箔的前处理方法

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JPH01292890A (ja) * 1988-05-20 1989-11-27 Mitsubishi Gas Chem Co Inc 薄銅張回路基板の製造法
JPH0260189A (ja) * 1988-08-26 1990-02-28 Mitsubishi Gas Chem Co Inc 薄銅箔張回路基板の製造法
JP2012229460A (ja) * 2011-04-25 2012-11-22 Mitsubishi Gas Chemical Co Inc 銅または銅合金表面用処理剤
WO2013015322A1 (ja) * 2011-07-26 2013-01-31 三菱瓦斯化学株式会社 銅／モリブデン系多層薄膜用エッチング液

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JP4687852B2 (ja) * 2001-06-25 2011-05-25 三菱瓦斯化学株式会社 銅および銅合金の表面処理剤
WO2010074053A1 (ja) * 2008-12-26 2010-07-01 日鉱金属株式会社 電子回路用の圧延銅箔又は電解銅箔及びこれらを用いた電子回路の形成方法
JP5499517B2 (ja) 2009-05-21 2014-05-21 三菱瓦斯化学株式会社 金属表面処理方法
JP5778460B2 (ja) 2011-03-24 2015-09-16 Jx日鉱日石金属株式会社 圧延銅箔及びその製造方法、並びに銅張積層板
JP5127082B2 (ja) 2011-03-29 2013-01-23 Ｊｘ日鉱日石金属株式会社 圧延銅箔
JP6424559B2 (ja) * 2013-11-22 2018-11-21 三菱瓦斯化学株式会社 エッチング用組成物及びそれを用いたプリント配線板の製造方法
JP2015134953A (ja) * 2014-01-17 2015-07-27 Jx日鉱日石金属株式会社 表面処理銅箔、キャリア付銅箔、プリント配線板、プリント回路板、銅張積層板及びプリント配線板の製造方法
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JPH01292890A (ja) * 1988-05-20 1989-11-27 Mitsubishi Gas Chem Co Inc 薄銅張回路基板の製造法
JPH0260189A (ja) * 1988-08-26 1990-02-28 Mitsubishi Gas Chem Co Inc 薄銅箔張回路基板の製造法
JP2012229460A (ja) * 2011-04-25 2012-11-22 Mitsubishi Gas Chemical Co Inc 銅または銅合金表面用処理剤
WO2013015322A1 (ja) * 2011-07-26 2013-01-31 三菱瓦斯化学株式会社 銅／モリブデン系多層薄膜用エッチング液

Cited By (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN113981447A (zh) * 2021-11-10 2022-01-28 纳然电子技术(苏州)有限公司 一种蚀刻液
CN115928071A (zh) * 2022-12-02 2023-04-07 江西荣晖电子有限公司 一种pcb用铜箔的前处理方法

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KR20190133164A (ko) 2019-12-02
JPWO2018180988A1 (ja) 2020-02-06
TW201843349A (zh) 2018-12-16
JP7074127B2 (ja) 2022-05-24
TWI808075B (zh) 2023-07-11
CN110462103A (zh) 2019-11-15
KR102568740B1 (ko) 2023-08-21

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