WO2022041534A1 - 适用于hdi板的电解铜箔用添加剂及电解铜箔生产工艺 - Google Patents

适用于hdi板的电解铜箔用添加剂及电解铜箔生产工艺 Download PDF

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WO2022041534A1
WO2022041534A1 PCT/CN2020/132528 CN2020132528W WO2022041534A1 WO 2022041534 A1 WO2022041534 A1 WO 2022041534A1 CN 2020132528 W CN2020132528 W CN 2020132528W WO 2022041534 A1 WO2022041534 A1 WO 2022041534A1
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concentration
copper foil
electrolytic
additive
copper
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PCT/CN2020/132528
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French (fr)
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江泱
杨帅国
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九江德福科技股份有限公司
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    • C—CHEMISTRY; METALLURGY
    • C25—ELECTROLYTIC OR ELECTROPHORETIC PROCESSES; APPARATUS THEREFOR
    • C25D—PROCESSES FOR THE ELECTROLYTIC OR ELECTROPHORETIC PRODUCTION OF COATINGS; ELECTROFORMING; APPARATUS THEREFOR
    • C25D1/00—Electroforming
    • C25D1/04—Wires; Strips; Foils
    • C—CHEMISTRY; METALLURGY
    • C25—ELECTROLYTIC OR ELECTROPHORETIC PROCESSES; APPARATUS THEREFOR
    • C25D—PROCESSES FOR THE ELECTROLYTIC OR ELECTROPHORETIC PRODUCTION OF COATINGS; ELECTROFORMING; APPARATUS THEREFOR
    • C25D3/00—Electroplating: Baths therefor
    • C25D3/02—Electroplating: Baths therefor from solutions
    • C25D3/38—Electroplating: Baths therefor from solutions of copper

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  • the invention relates to the technical field of electrolytic copper foil, in particular to an additive for electrolytic copper foil suitable for HDI boards and a production process for electrolytic copper foil.
  • HDI boards With the continuous development of high-density and high-precision electronic products, thinning, small volume and good packaging, the high-density integration technology contained in HDI boards can make the design of end products more miniaturized, and also meet the requirements of higher electronic performance and efficiency. Standard, currently popular electronic products, such as mobile phones, digital (camera), notebook computers, automotive electronics, many use HDI boards. With the upgrading of electronic products and changes in market demand, HDI boards are developing very rapidly. , but the HDI board processing technology is complex, multiple laminations, high-density interconnection between layers, multiple buried holes, blind holes, multiple thermal processing of copper foil and substrate, and poor toughness of general electrolytic copper foil, which will lead to Broken copper foil.
  • the present invention proposes an additive for electrolytic copper foil suitable for HDI board and a production process for electrolytic copper foil, which can overcome the above-mentioned deficiencies of the prior art.
  • An additive for electrolytic copper foil suitable for HDI board is sodium polydithiodipropane sulfonate (SPS) containing brightener, N,N-dimethyl-dithiocarbonyl propane sulfonate (DPS) ) and an aqueous solution of gelatin, the concentration of brightener SPS in the aqueous solution is 2-3 g/L, the concentration of DPS is 0.5-1.5 g/L, and the concentration of gelatin is 3-4 g/L.
  • SPS sodium polydithiodipropane sulfonate
  • DPS N,N-dimethyl-dithiocarbonyl propane sulfonate
  • the molecular weight of the gelatin is 20,000.
  • a production process of electrolytic copper foil comprises the following steps:
  • S1 liquid preparation process add copper rods or copper blocks into the copper-dissolving tank, react with pure water and dilute sulfuric acid to generate copper sulfate solution;
  • the generated copper sulfate solution is sent to the clean liquid tank after being filtered, the electrolyte solution is obtained after adjusting the clean liquid concentration, the electrolytic solution is sent to the electrolytic cell, the additive is added in the electrolytic cell, and then electrolytic production is carried out,
  • the current density was 65A/m 2
  • the flow rate of the electrolyte was 35m 3 /h
  • the flow rate of the additive was 30-40mL/min.
  • the production process also comprises the following steps:
  • S3 surface treatment process the green foil produced in the electrolysis process is subjected to surface treatment.
  • step S3 includes the following steps:
  • the concentration of sulfuric acid in the pickling tank is 130 ⁇ 135g/L, and the temperature is 20 ⁇ 30°C;
  • S32 is roughened, the copper concentration in the roughening tank is 15-20g/L, the sulfuric acid concentration is 135-155g/L, and the temperature is 30-40°C;
  • the copper concentration in the curing tank is 60-75g/L, the sulfuric acid concentration is 100-110g/L, and the temperature is 45-50°C;
  • the concentration of nickel in the blackening treatment tank is 2 ⁇ 3g/L
  • the concentration of zinc is 5 ⁇ 6g/L
  • the concentration of K 4 P 2 O 7 is 100 ⁇ 120g/L
  • the pH value is 10 ⁇ 11
  • S35 is anti-oxidation, and the chromium concentration in the anti-oxidation treatment tank is 2.5 ⁇ 3.5g/L, the pH is 11 ⁇ 12, and the temperature is 20 ⁇ 30°C.
  • the content of copper in the electrolyte is 90-95 g/L
  • the content of sulfuric acid is 130-150 g/L
  • the temperature of the electrolyte is 54-57°C.
  • the 12-105 ⁇ m electrolytic copper foil produced by using the additive for electrolytic copper foil suitable for HDI board of the present invention has stable peak profile, consistent lattice size, normal temperature tensile strength ⁇ 400MPa, high temperature tensile strength Strength ⁇ 200MPa, elongation at room temperature ⁇ 10%, elongation at high temperature ⁇ 15%, folding endurance ⁇ 3000 times, high airborne strength, good copper foil toughness, thus solving the problem of copper foil rupture during HDI sheet processing.
  • Fig. 1 is the SEM image of the electrolytic copper foil prepared in Example 1 of the present invention.
  • Fig. 2 is the SEM image of the electrolytic copper foil prepared in Example 2 of the present invention.
  • Example 3 is a SEM image of the electrolytic copper foil prepared in Example 3 of the present invention.
  • An additive for electrolytic copper foil suitable for HDI board is an aqueous solution with SPS concentration of 2g/L, DPS concentration of 0.5g/L and gelatin concentration of 3g/L, and the molecular weight of gelatin is 20000.
  • S1 liquid preparation process add the cleaned or degreasing copper rod or copper block into the copper melting tank, and chemically react with pure water and dilute sulfuric acid under the conditions of steam heating and fan oxygenation to generate copper sulfate solution;
  • the copper sulfate solution generated by the above-mentioned reaction is sent to the clean liquid tank after filtering, and the clean liquid concentration is adjusted, and the copper content is 90g/L, and the sulfuric acid content is 130g/L, and the temperature is 54 °C.
  • send to The electrolytic cell adding the additive in the electrolytic cell, the flow rate of the additive is 30mL/min, and then electrolyzed production; the process conditions for controlling the electrolytic green foil are the current density 65A/m 2 , and the flow rate of the electrolyte is 35m 3 / h;
  • S32 is roughened, the copper concentration is 15g/L, the sulfuric acid concentration is 135g/L, and the temperature is 30°C;
  • the nickel concentration is 2g/L
  • the zinc concentration is 5g/L
  • the K 4 P 2 O 7 concentration is 100g/L
  • the pH value is controlled at 10
  • the temperature is 35°C;
  • S35 is anti-oxidative, the chromium concentration is 2.5g/L, the pH value is controlled at 11, and the temperature is 20°C.
  • the SEM image of the prepared electrolytic copper foil is shown in FIG. 1 .
  • An additive for electrolytic copper foil suitable for HDI board has an aqueous solution of SPS concentration of 2.5g/L, DPS concentration of 0.5g/L and gelatin concentration of 3.5g/L, and the molecular weight of gelatin is 20000.
  • the production process of the 18 ⁇ m electrolytic copper foil prepared by the above-mentioned additives includes the following steps:
  • S1 liquid preparation process add the cleaned or degreasing copper rod or copper block into the copper melting tank, and chemically react with pure water and dilute sulfuric acid under the conditions of steam heating and fan oxygenation to generate copper sulfate solution;
  • the copper sulfate solution generated above is sent to the clean liquid tank after being filtered, and the concentration of the clean liquid is adjusted, the copper content is 93g/L, the sulfuric acid content is 130g/L, and the temperature is 55°C.
  • the additive is added to the electrolytic cell, and the flow rate of the additive is 35 mL/min, and then electrolytic production is performed; the process conditions for controlling the electrolytic green foil are a current density of 70 A/m 2 and a flow rate of the electrolyte solution of 40 m 3 /h;
  • S32 is roughened, the copper concentration is 15g/L, the sulfuric acid concentration is 135g/L, and the temperature is 30°C;
  • S34 is blackened, the concentration of nickel is 2g/L, the concentration of zinc is 5g/L, the concentration of K 4 P 2 O 7 is 100g/L, the pH value is controlled at 10, and the temperature is 35°C;
  • S35 is anti-oxidation
  • the concentration of chromium is 2.5g/L
  • the pH value is controlled at 11
  • the temperature is 20°C.
  • the SEM image of the prepared electrolytic copper foil is shown in FIG. 2 .
  • An additive for electrolytic copper foil suitable for HDI board is an aqueous solution with a concentration of SPS of 3g/L, a concentration of DPS of 1.5g/L, a concentration of gelatin of 4g/L, and the molecular weight of gelatin is 20,000.
  • the production process of preparing 35 ⁇ m electrolytic copper foil with the above-mentioned additives includes the following steps:
  • S1 liquid preparation process add the cleaned or degreasing copper rod or copper block into the copper melting tank, and chemically react with pure water and dilute sulfuric acid under the conditions of steam heating and fan oxygenation to generate copper sulfate solution;
  • the copper sulfate solution generated by above-mentioned reaction is sent to the clean liquid tank after filtration, adjust the clean liquid concentration, copper content 95g/L, sulfuric acid content 150g/L, temperature 55 °C, is sent to electrolyzer after adjustment, Add the additive in the electrolytic cell, and the flow rate of the additive is 40mL/min, and then electrolytic production is performed; the process conditions for controlling the electrolytic green foil are the current density of 75A/m 2 and the flow rate of the electrolyte solution of 45m 3 /h;
  • S32 is roughened, the copper concentration is 15g/L, the sulfuric acid concentration is 135g/L, and the temperature is 30°C;
  • the concentration of nickel is 2g/L
  • the concentration of zinc is 5g/L
  • the concentration of K 4 P 2 O 7 is 100g/L
  • the pH value is controlled at 10
  • the temperature is 35 °C
  • S35 is anti-oxidation
  • the concentration of chromium is 2.5g/L
  • the pH value is controlled at 11
  • the temperature is 20°C.
  • the SEM image of the prepared electrolytic copper foil is shown in FIG. 3 .
  • Copper foil specification Normal temperature tensile strength Room temperature elongation Normal temperature tensile strength Room temperature elongation Folding times 12 ⁇ m specification (Example 1) 420MPa 10% 230MPa 15% ⁇ 3000 times 18 ⁇ m specification (Example 2) 410MPa 12% 220MPa 18% ⁇ 3000 times 35 ⁇ m specification (Example 3) 400MPa 16% 220MPa 25% ⁇ 3000 times
  • the copper sulfate solution is obtained through the process of dissolving copper solution, and then the prepared electrolyte is filtered through the tank liquid, and the parameters of cupric acid are adjusted, and the present invention is added to the electrolytic tank.
  • the semi-finished product that is, the raw foil, is produced through the electrolysis process, and finally the finished copper foil is produced through the surface treatment process.

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  • Engineering & Computer Science (AREA)
  • Chemical Kinetics & Catalysis (AREA)
  • Electrochemistry (AREA)
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Abstract

一种适用于HDI板的电解铜箔用添加剂及电解铜箔生产工艺，所述添加剂为含有光亮剂SPS、DPS和明胶的水溶液，所述水溶液中光亮剂SPS的浓度为2～3g/L，DPS的浓度为0.5～1.5g/L，明胶的浓度为3～4g/L。该适用于HDI板的电解铜箔用添加剂生产出的12～105μm电解铜箔，轮廓峰值稳定、晶格大小一致、常温抗拉强度≥400MPa，高温抗拉强度≥200MPa，常温延伸率≥10％，高温延伸率≥15％，耐折次数≥3000次，机载强度高、铜箔韧性好，解决了HDI板材在加工过程中的铜箔断裂问题。

Description

适用于HDI板的电解铜箔用添加剂及电解铜箔生产工艺 技术领域
本发明涉及电解铜箔技术领域，具体来说，涉及一种适用于HDI板的电解铜箔用添加剂及电解铜箔生产工艺。
背景技术
随着电子产品不断向高密度、高精度发展，轻薄化、容积小、封装性好，HDI板中蕴含的高密度集成技术可以使终端产品设计更加小型化，也满足电子性能和效率的更高标准，目前流行的电子产品，如手机、数码(摄)像机、笔记本电脑、汽车电子，很多都要是使用HDI板，随着电子产品的更新换代和市场需求的改变，HDI板的发展非常迅速，但HDI板加工技术复杂，多次层压，层与层之间高密互连，多次埋孔、盲孔，铜箔与基材多次热加工，一般的电解铜箔韧性差，会导致铜箔断裂。
发明内容
针对相关技术中的上述技术问题，本发明提出一种适用于HDI板的电解铜箔用添加剂及电解铜箔生产工艺，能够克服现有技术的上述不足。
为实现上述技术目的，本发明的技术方案是这样实现的：
一种适用于HDI板的电解铜箔用添加剂，所述添加剂为含有光亮剂聚二硫二丙烷磺酸钠(SPS)、N,N-二甲基-二硫代羰基丙烷磺酸钠(DPS)和明胶的水溶液，所述水溶液中光亮剂SPS的浓度为2～3g/L，DPS的浓度为0.5～1.5g/L，明胶的浓度为3～4g/L。
优选地，所述明胶的分子量为20000。
根据本发明的另一方面，提供了一种电解铜箔生产工艺，该生产工艺包括以下步骤：
S1制液工序：将铜杆或铜块加入溶铜罐中，与纯水、稀硫酸反应生成硫酸铜溶液；
S2电解工序：将生成的硫酸铜溶液经过滤后送至净液罐，调整净液浓度 后得到电解液，将电解液送至电解槽，在电解槽中加入所述添加剂，然后进行电解生产，电流密度为65A/m 2，电解液的流量为35m 3/h，添加剂流量为30～40mL/min。
进一步地，所述生产工艺还包括以下步骤：
S3表面处理工序：将电解工序生产出的生箔进行表面处理。
进一步地，所述步骤S3包括以下步骤：
S31酸洗，酸洗槽中硫酸浓度为130～135g/L，温度为20～30℃；
S32粗化，粗化槽中铜浓度为15～20g/L，硫酸浓度为135～155g/L，温度为30～40℃；
S33固化，固化槽中铜浓度为60～75g/L，硫酸浓度为100～110g/L，温度为45～50℃；
S34黑化，黑化处理槽中镍的浓度为2～3g/L，锌浓度为5～6g/L，K 4P 2O 7浓度为100～120g/L，pH值为10～11，温度为35～45℃；
S35防氧化，防氧化处理槽中铬浓度为2.5～3.5g/L，pH为11～12，温度为20～30℃。
优选地，在电解生产过程中，电解液中铜含量为90～95g/L，硫酸含量为130～150g/L，电解液温度为54～57℃。
本发明的有益效果：通过使用本发明的适用于HDI板的电解铜箔用添加剂生产出的12～105μm电解铜箔，轮廓峰值稳定、晶格大小一致、常温抗拉强度≥400MPa，高温抗拉强度≥200MPa，常温延伸率≥10％，高温延伸率≥15％，耐折次数≥3000次，机载强度高、铜箔韧性好，从而解决了HDI板材在加工过程中的铜箔断裂问题。
附图说明
为了更清楚地说明本发明实施例或现有技术中的技术方案，下面将对实施例中所需要使用的附图作简单地介绍，显而易见地，下面描述中的附图仅仅是本发明的一些实施例，对于本领域普通技术人员来讲，在不付出创造性劳动的前提下，还可以根据这些附图获得其他的附图。
图1是本发明实施例1制备的电解铜箔的SEM图；
图2是本发明实施例2制备的电解铜箔的SEM图；
图3是本发明实施例3制备的电解铜箔的SEM图。
具体实施方式
下面将结合本发明实施例中的附图，对本发明实施例中的技术方案进行清楚、完整地描述，显然，所描述的实施例仅仅是本发明一部分实施例，而不是全部的实施例。基于本发明中的实施例，本领域普通技术人员所获得的所有其他实施例，都属于本发明保护的范围。
实施例1
一种适用于HDI板的电解铜箔用添加剂，该添加剂为SPS浓度为2g/L、DPS浓度为0.5g/L、明胶浓度为3g/L的水溶液，明胶的分子量为20000。
采用上述添加剂制备12μm电解铜箔，具体包括如下步骤：
S1制液工序：将清洗或除油的铜杆或铜块加入溶铜罐中，与纯水、稀硫酸，在蒸汽加热、风机增氧的条件下发生化学反应，生成硫酸铜溶液；
S2电解工序：将上述反应生成的硫酸铜溶液，经过滤后送至净液罐，调整净液浓度，铜含量为90g/L，硫酸含量为130g/L，温度为54℃，调整后送至电解槽，在电解槽中加入所述添加剂，所述添加剂的流量为30mL/min，然后进行电解生产；控制电解生箔的工艺条件为电流密度65A/m 2，电解液的流量为35m 3/h；
S3表面处理工序：将电解工序生产出的生箔进行表面处理：
S31酸洗，硫酸浓度为130g/L，温度为20℃；
S32粗化，铜浓度为15g/L，硫酸浓度为135g/L，温度为30℃；
S33固化，铜浓度为60g/L，硫酸浓度为100g/L，温度为45℃；
S34黑化，镍浓度为2g/L，锌浓度为5g/L，K 4P 2O 7浓度为100g/L，pH值控制在10，温度为35℃；
S35防氧化，铬浓度为2.5g/L，pH值控制在11，温度为20℃。
制备得到的电解铜箔的SEM图如图1所示。
实施例2
一种适用于HDI板的电解铜箔用添加剂，该添加剂SPS浓度为2.5g/L、DPS浓度为0.5g/L、明胶浓度为3.5g/L的水溶液，明胶的分子量为20000。
采用上述添加剂制备的18μm电解铜箔的生产工艺包括如下步骤：
S1制液工序：将清洗或除油的铜杆或铜块加入溶铜罐中，与纯水、稀硫酸，在蒸汽加热、风机增氧的条件下发生化学反应，生成硫酸铜溶液；
S2电解工序：将上述生成的硫酸铜溶液，经过滤后送至净液罐，调整净液浓度，铜含量93g/L，硫酸含量130g/L，温度55℃，调整扣送至电解槽，在电解槽中加入所述添加剂，添加剂流量为35mL/min，然后进行电解生产；控制电解生箔的工艺条件为电流密度70A/m 2，电解液的流量为40m 3/h；
S3表面处理工序：将电解工序生产出的生箔进行表面处理：
S31酸洗，硫酸浓度为130g/L，温度为20℃；
S32粗化，铜浓度为15g/L，硫酸浓度为135g/L，温度为30℃；
S33固化，铜浓度为60g/L，硫酸浓度为100g/L，温度为45℃；
S34黑化，镍的浓度为2g/L，锌浓度为5g/L，K 4P 2O 7浓度为100g/L，pH值控制在10，温度为35℃；
S35防氧化，铬的浓度为2.5g/L，pH值控制在11，温度为20℃。
制备得到的电解铜箔的SEM图如图2所示。
实施例3
一种适用于HDI板的电解铜箔用添加剂，该添加剂为SPS的浓度为3g/L，DPS的浓度1.5g/L，明胶的浓度为4g/L的水溶液，明胶的分子量为20000。
采用上述添加剂制备35μm电解铜箔的生产工艺包括如下步骤：
S1制液工序：将清洗或除油的铜杆或铜块加入溶铜罐中，与纯水、稀硫酸，在蒸汽加热、风机增氧的条件下发生化学反应，生成硫酸铜溶液；
S2电解工序：将上述反应生成的硫酸铜溶液，经过滤后送至净液罐，调整净液浓度，铜含量95g/L，硫酸含量150g/L，温度55℃，调整后送至电解槽，在电解槽中加入所述添加剂，添加剂流量为40mL/min，然后进行电解生产；控制电解生箔的工艺条件为电流密度75A/m 2，电解液的流量为45m 3/h；
S3表面处理工序：将上述生产出的生箔，经表面处理：
S31酸洗，硫酸浓度为130g/L，温度为20℃；
S32粗化，铜浓度为15g/L，硫酸浓度为135g/L，温度为30℃；
S33固化，铜浓度为60g/L，硫酸浓度为100g/L，温度为45℃；
S34黑化，镍的浓度为2g/L、锌浓度为5g/L，K 4P 2O 7浓度为100g/L，pH 值控制在10，温度为35℃，
S35防氧化，铬的浓度为2.5g/L，pH值控制在11，温度为20℃。
制备得到的电解铜箔的SEM图如图3所示。
实施例1-3制备的电解铜箔规格物性如表1所示。
表1电解铜箔物性测试结果
铜箔规格 常温抗拉强度 常温延伸率 常温抗拉强度 常温延伸率 耐折次数
12μm规格(实施例1) 420MPa 10％ 230MPa 15％ ≥3000次
18μm规格(实施例2) 410MPa 12％ 220MPa 18％ ≥3000次
35μm规格(实施例3) 400MPa 16％ 220MPa 25％ ≥3000次
综上所述，借助于本发明的上述技术方案，通过溶铜制液工序得到硫酸铜溶液，然后将制好的电解液经槽液过滤、铜酸参数的调配，在电解槽中加入本发明的添加剂，再经电解工序生产出半成品，即生箔，最后经过表面处理工序生产出成品铜箔，得到的成品铜箔轮廓峰值稳定、晶格大小一致、常温抗拉强度≥400MPa，高温抗拉强度≥200MPa，常温延伸率≥10％，高温延伸率≥15％，耐折次数≥3000次，机载强度高、铜箔韧性好，从而解决了HDI板材在加工过程中的铜箔断裂问题。
以上所述仅为本发明的较佳实施例而已，并不用以限制本发明，凡在本发明的精神和原则之内，所作的任何修改、等同替换、改进等，均应包含在本发明的保护范围之内。

Claims (6)

  1. 一种适用于HDI板的电解铜箔用添加剂，其特征在于，所述添加剂为含有光亮剂SPS、DPS和明胶的水溶液，所述水溶液中光亮剂SPS的浓度为2～3g/L，DPS的浓度为0.5～1.5g/L，明胶的浓度为3～4g/L。
  2. 根据权利要求1所述的适用于HDI板的电解铜箔用添加剂，其特征在于，所述明胶的分子量为20000。
  3. 一种采用权利要求1或2所述添加剂的电解铜箔生产工艺，其特征在于，包括以下步骤：
    S1制液工序：将铜杆或铜块加入溶铜罐中，与纯水、稀硫酸反应生成硫酸铜溶液；
    S2电解工序：将生成的硫酸铜溶液经过滤后送至净液罐，调整净液浓度后得到电解液，将电解液送至电解槽，在电解槽中加入所述添加剂，然后进行电解生产，电流密度为65A/m 2，电解液的流量为35m 3/h，添加剂流量为30～40mL/min。
  4. 根据权利要求3所述的电解铜箔生产工艺，其特征在于，进一步包括以下步骤：
    S3表面处理工序：将电解工序生产出的生箔进行表面处理。
  5. 根据权利要求4所述的电解铜箔生产工艺，其特征在于，所述步骤S3包括以下步骤：
    S31酸洗，酸洗槽中硫酸浓度为130～135g/L，温度为20～30℃；
    S32粗化，粗化槽中铜浓度为15～20g/L，硫酸浓度为135～155g/L，温度为30～40℃；
    S33固化，固化槽中铜浓度为60～75g/L，硫酸浓度为100～110g/L，温度为45～50℃；
    S34黑化，黑化处理槽中镍的浓度为2～3g/L，锌浓度为5～6g/L，K 4P 2O 7浓度为100～120g/L，pH值为10～11，温度为35～45℃；
    S35防氧化，防氧化处理槽中铬浓度为2.5～3.5g/L，pH为11～12，温度为20～30℃。
  6. 根据权利要求3所述的电解铜箔生产工艺，其特征在于，在电解生产过程中，电解液中铜含量为90～95g/L，硫酸含量为130～150g/L，电解液温度为54～57℃。
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