CN105063582B - An ionic liquid chemical copper plating method - Google Patents

An ionic liquid chemical copper plating method Download PDF

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CN105063582B
CN105063582B CN 201510437116 CN201510437116A CN105063582B CN 105063582 B CN105063582 B CN 105063582B CN 201510437116 CN201510437116 CN 201510437116 CN 201510437116 A CN201510437116 A CN 201510437116A CN 105063582 B CN105063582 B CN 105063582B
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ionic liquid
copper plating
solution
electroless
parts
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CN105063582A (en )
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何波
林均秀
胡文成
徐玉珊
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珠海元盛电子科技股份有限公司
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Abstract

本发明公开一种以简单、绿色环保的离子液体作为镀溶液的离子液体化学镀铜的方法。 The present invention discloses a simple process green ionic liquid as an ionic liquid of the copper plating solution. 该方法包括:(1)作为化学镀溶液的离子液体的配制;(2)对印制电路板进行预处理,然后将电路板置于步骤(1)制得的化学镀溶液中,在50~80°之间进行化学镀铜;本发明利用离子液体来作为化学镀铜的溶液能够极大地降低溶液的挥发性,减少对人体的伤害及对环境的污染,同时,使用过后的离子液体容易降解,不会对环境造成污染,离子液体无味、不易燃、易与产物分离、易回收、可反复循环利用。 The method comprises: (1) electroless plating solution is formulated as an ionic liquid; (2) pretreatment of the printed circuit board, and the board to step (1) prepared electroless plating solution at 50 ~ electroless copper plating between 80 °; according to the present invention uses ionic liquids as the electroless copper plating solution can greatly reduce the volatility of the solution, to reduce the harm to human body and environmental pollution, at the same time, after the use of ionic liquids readily degraded , will not pollute the environment, the ionic liquid odorless, nonflammable, easily separated from the product, easily recycled, can be repeatedly recycled. 本发明可用于电路板印制领域。 The present invention can be used in the field of printed circuit boards.

Description

_种禹子液体化学镀铜的方法 Yu sub _ seed copper plating method of the liquid

技术领域 FIELD

[0001] 本发明涉及一种离子液体化学镀铜的方法。 [0001] The present invention relates to an ionic liquid copper plating method. 具体而言,涉及包含化学镀铜的离子液体配制和印制板的孔金属化。 More specifically, it relates to ionic liquids comprising copper plating formulation and PCB metallization of apertures.

背景技术 Background technique

[0002] 化学镀铜因为经济、简单而成为表面处理的主要技术之一。 [0002] electroless copper because of economic, simple to become one of the major technology surface treatment. 化学镀铜在化学镀中占有十分重要的地位,目前已经广泛应用于非金属电镀的底层、印制板的孔金属化和电子仪器的电磁屏蔽层等各个方面。 Electroless copper plating occupies a very important position, has been widely applied to the underlying plating of non-metallic, the various aspects of the PCB hole metallization and electronic instruments like electromagnetic shielding layer. 印制板孔金属化技术是印制板制造技术的关键之一,化学镀铜可以显著缩短加工周期,降低生产成本,金属化孔可靠性强,铜孔内镀层厚度非常均匀且不存在应力。 PCB hole metallization is one of the key technology PCB manufacturing techniques, the copper plating can significantly shorten the processing cycle, reduce production costs, reliability metallized hole, the hole copper plating thickness is very uniform and there is no stress. 用此种工艺方法很容易做出高精度的印制板。 Such a process for easily made with high precision PCB.

[0003] 化学镀铜溶液种类繁多,镀液一般由铜盐、还原剂、配位体、稳定剂和其他添加剂组成。 [0003] a wide variety of electroless copper plating solution, plating solution generally consists of copper, a reducing agent, the ligand, stabilizers and other additives. 其中还原剂一般为甲醛、次磷酸钠和硼氢化钠为还原剂。 Wherein the reducing agent is typically formaldehyde, sodium borohydride and sodium hypophosphite as a reducing agent. 其中常见的还原剂为甲醛,然而甲醛具有挥发性和毒性,对人体和周围的环境均有严重影响。 One of the common reducing agent is formaldehyde, formaldehyde, volatile and toxic, however, have a serious impact on the human body and the surrounding environment. 常见的方法是用次磷酸钠来代替甲醛,主要是用柠檬酸钠作为络合剂,但是其镀铜速度低。 The common method is to use sodium hypophosphite instead of formaldehyde, mainly with sodium citrate as a complexing agent, but the low speed plating.

[0004] 根据现有文献报道,化学镀铜溶液中的甲醛对生态环境有危害,并且有致癌的潜在危险,同时化学镀铜溶液中的络合剂(如EDTA等)不易进行生物降解,废水处理困难,除此之外,化学镀铜溶液的稳定性较差,操作稍有不慎就会出现溶液分解,需对其进行严格的监控和维护,成本极高。 [0004] According to the prior literature, electroless copper plating solution of formaldehyde environment hazards, and potential carcinogenic risk, while electroless copper plating solution of a complexing agent (e.g., EDTA) easily biodegrade waste processing difficulties, in addition, less stable copper plating solution, there will be a little careless operation decomposition solution, the need to be strict monitoring and maintenance, high costs. 因此寻找一种高效、环保的方法进行化学镀铜成为了研究的热点。 So to find an efficient, environmentally friendly method of electroless copper plating has become a hot research.

发明内容 SUMMARY

[0005] 本发明旨在改善上述问题,提出了一种以简单、绿色环保的离子液体作为镀溶液的离子液体化学镀铜的方法。 [0005] The present invention aims to improve the above problem, a simple, green ionic liquid ionic liquid electroless plating solution as copper plating method.

[0006] 本发明所述方法所采用的技术方案是:该方法包括以下步骤: [0006] The method aspect of the present invention is employed: the method comprising the steps of:

[0007] (1)作为化学镀溶液的离子液体的配制; [0007] (1) Preparation of electroless plating solution as an ionic liquid;

[0008] (2)对印制电路板进行预处理,然后将电路板置于步骤(1)制得的化学镀溶液中,在50〜80°C之间进行化学镀铜。 [0008] (2) pretreatment of the printed circuit board, and the board to step (1) prepared electroless plating solution, electroless copper plating between 50~80 ° C.

[0009] 进一步地,所述步骤(1)的具体步骤为: [0009] Further, the step (1) is the specific steps:

[0010] a、按摩尔比为1:2取氯化胆碱和尿素放入烧杯中,置于控温磁力搅拌器上保持恒温60 °C加热,磁力搅拌0 · 5小时; [0010] a, a molar ratio of 1: 2 to take choline chloride and urea into a beaker placed on a magnetic stirrer to maintain constant temperature 60 ° C was heated with magnetic stirring 0 · 5 hours;

[0011] b、待烧杯中形成均匀透明溶液后,将氯化铜、配位剂、还原剂和催化剂依次分别加入离子液体中,每次加入一种试剂之前溶液均要均匀透明,保温60°C磁力搅拌1小时,其中,按质量份数计,当步骤(1)获得的透明溶液为100份时,所述氯化铜为1〜3份,配位剂为2〜6份,还原剂为3〜7份,催化剂为0.1〜0.4份。 [0011] b, after the formation of a uniform transparent solution to be beaker, cupric chloride, complexing agent, reducing agent and catalyst were added in the ionic liquid, respectively, each time before adding a reagent solution have to be a uniform transparent, heat 60 ° when C magnetically stirred for 1 hour, wherein the mass fraction of the total, when the step (1) a clear solution was obtained 100 parts of said copper chloride as 1 ~ 3 parts of 2 ~ 6 parts of complexing agent, a reducing agent is 3~7 parts, the catalyst is 0.1~0.4 parts.

[0012] 进一步地,所述氯化铜的浓度为5g/L〜15g/L。 [0012] Further, the concentration of copper chloride 5g / L~15g / L.

[0013] 进一步地,所述配位剂为酒石酸钠,其浓度为10g/L〜30g/L。 [0013] Furthermore, the complexing agent is sodium tartrate, at a concentration of 10g / L~30g / L.

[0014] 进一步地,所述还原剂为次磷酸钠,其浓度为15g/L〜35g/L。 [0014] Further, the reducing agent is sodium hypophosphite, a concentration of 15g / L~35g / L.

[00Ί5]更进一步地,所述催化剂是镍、钴、铁的金属盐,浓度为0.5g/L〜2g/L。 [00Ί5] Furthermore, the catalyst is a nickel, cobalt, iron salts, at a concentration of 0.5g / L~2g / L.

[0016] 本发明的有益效果是:本发明采用离子液体作为化学镀铜的溶液,而离子液体具有易降解,挥发性小,通过改变离子种类即可调节离子液体的溶解性等特点,在化学镀铜中,利用离子液体来作为化学镀铜的溶液能够极大地降低溶液的挥发性,减少对人体的伤害及对环境的污染,同时,使用过后的离子液体容易降解,不会对环境造成污染,离子液体无味、不易燃、易与产物分离、易回收、可反复循环利用,是一种简单、绿色环保的溶液,由其制得的印制板质量稳定,且印制质量好,孔金属化均匀。 [0016] Advantageous effects of the present invention are: the present invention uses an ionic liquid as the electroless copper plating solution, the ionic liquid has readily degradable, low volatility, solubility of the ionic liquid can be adjusted by varying the ion species, etc., in chemical copper, the use of ionic liquids as a copper plating solution can greatly reduce the volatility of the solution, to reduce the harm to human body and environmental pollution, at the same time, the ionic liquid is easily degraded after use, will not pollute the environment , ionic liquids odorless, nonflammable, easily separated from the product, easily recycled, can be repeatedly recycled, is a simple, green solution was obtained therefrom PCB stable quality, and good quality printing, porous metal of uniform.

具体实施方式 detailed description

[0017] 下面根据发明方法通过具体实施例来详细说明。 [0017] The following method according to the invention described in detail through specific embodiments. 以下实施实例只是为了更好地将本发明技术原理阐释清楚,并不代表本发明只限制使用该实施实例。 The following examples are embodiments in order to better explain the technical principles of the present invention clearly do not represent the present invention is limited only to use the example embodiment.

[0018] 实施例一: [0018] Example a:

[0019] 按摩尔比为1:2取氯化胆碱和尿素放入烧杯中,置于控温磁力搅拌器上保持恒温60 °C加热,磁力搅拌0.5小时。 [0019] molar ratio of 1: 2 to take choline chloride and urea into a beaker placed on a magnetic stirrer to maintain constant temperature 60 ° C was heated with magnetic stirring for 0.5 hours. 待烧杯中形成均匀透明溶液后,将氯化铜5g/L、配位剂I Og/L、还原剂15g//L和催化剂0.5g/L依次分别加入离子液体中,每次加入试剂之前溶液均要均匀透明,保温60°C磁力搅拌1小时。 After forming a uniform transparent solution to be beaker, cupric chloride 5g / L, a complexing agent I Og / L, the reducing agent and catalyst 15g // L 0.5g / L of ionic liquid were added sequentially, before the addition of each reagent solution to have a uniform transparent insulation 60 ° C magnetically stirred for 1 hour. 将预处理过的印制电路板放入配制好的溶液中进行化学镀铜实验,实验温度为50 °C。 The pretreated printed circuit board into the prepared solution for electroless copper plating experiments a temperature of 50 ° C.

[0020] 实施例二: [0020] Example II:

[0021] 按摩尔比为1:2取氯化胆碱和尿素放入烧杯中,置于控温磁力搅拌器上保持恒温60 °C加热,磁力搅拌0.5小时。 [0021] molar ratio of 1: 2 to take choline chloride and urea into a beaker placed on a magnetic stirrer to maintain constant temperature 60 ° C was heated with magnetic stirring for 0.5 hours. 待烧杯中形成均匀透明溶液后,将氯化铜8g/L、配位剂15g/L、还原剂20g/L和催化剂lg/L依次分别加入离子液体中,每次加入试剂之前溶液均要均匀透明,保温60°C磁力搅拌1小时。 After forming a uniform transparent solution to be beaker, cupric chloride 8g / L, a complexing agent 15g / L, the reducing agent 20g / L catalyst and lg / L of ionic liquid were added sequentially, before each reagent solution were added uniformly to transparent insulation 60 ° C magnetically stirred for 1 hour. 将预处理过的印制电路板放入配制好的溶液中进行化学镀铜实验,实验温度为60 °C。 The pretreated printed circuit board into the prepared solution for electroless copper plating experiments a temperature of 60 ° C.

[0022] 实施例三: [0022] Example III:

[0023] 按摩尔比为1:2取氯化胆碱和尿素放入烧杯中,置于控温磁力搅拌器上保持恒温60°C加热,磁力搅拌0.5小时。 [0023] molar ratio of 1: 2 to take choline chloride and urea into a beaker placed on a magnetic stirrer to maintain constant temperature 60 ° C was heated with magnetic stirring for 0.5 hours. 待烧杯中形成均匀透明溶液后,将氯化铜12g/L、配位剂20g/L、还原剂30g/L和催化剂1.5g/L依次分别加入离子液体中,每次加入试剂之前溶液均要均匀透明,保温60°C磁力搅拌1小时。 After forming a uniform transparent solution to be beaker, cupric chloride 12g / L, a complexing agent 20g / L, the reducing agent 30g / L catalyst and 1.5g / L of ionic liquid were added successively, and the solution was added to the reagent prior to each uniform and transparent, heat 60 ° C magnetically stirred for 1 hour. 将预处理过的印制电路板放入配制好的溶液中进行化学镀铜实验,实验温度为70°C。 The pretreated printed circuit board into the prepared solution for electroless copper plating experiments a temperature of 70 ° C.

[0024] 实施例四: [0024] Example IV:

[0025] 按摩尔比为1:2取氯化胆碱和尿素放入烧杯中,置于控温磁力搅拌器上保持恒温60 °C加热,磁力搅拌0.5小时。 [0025] molar ratio of 1: 2 to take choline chloride and urea into a beaker placed on a magnetic stirrer to maintain constant temperature 60 ° C was heated with magnetic stirring for 0.5 hours. 待烧杯中形成均匀透明溶液后,将氯化铜15g/L、配位剂30g/L、还原剂35g/L和催化剂2g/L依次分别加入离子液体中,每次加入试剂之前溶液均要均匀透明,保温60°C磁力搅拌1小时。 After forming a uniform transparent solution to be beaker, cupric chloride 15g / L, a complexing agent 30g / L, the reducing agent 35g / L catalyst and 2g / L of ionic liquid were added sequentially, each solution were added to the reagent before uniformly transparent insulation 60 ° C magnetically stirred for 1 hour. 将预处理过的印制电路板放入配制好的溶液中进行化学镀铜实验,实验温度为60 °C。 The pretreated printed circuit board into the prepared solution for electroless copper plating experiments a temperature of 60 ° C.

[0026] 经过实验,上述实施例获得的测试性能指标如表1所示。 [0026] After the experiment, testing the performance metrics obtained above embodiments as shown in Table 1.

[0027] 表1 [0027] TABLE 1

[0028] [0028]

Figure CN105063582BD00051

[0029] 由表1可知,本发明采用离子液体作为化学镀铜的溶液,其镀铜时间短,无挥发性气味产生,溶液体系和镀铜后的印制板体系均具有稳定的性能表现,在后续的溶液处理中,其极易降解,不会对环境造成任何的污染,也保证了人体免受伤害,其是一种全新的镀铜方法。 [0029] As apparent from Table 1, the present invention uses ionic liquids as the electroless copper plating solution, which plating time is short, no volatile odor generation, and the solution system has a stable copper PCB system performance, in the subsequent solution treatment, which can easily degrade and will not cause any pollution to the environment, but also to ensure that the human body from harm, which is a new copper plating method.

[0030] 上述实例对本发明做了详细的说明,但并不意味着本发明仅仅局限于这四种实例。 [0030] The above examples of the present invention has been described in detail, it is not intended that the invention be limited to these four examples. 在不脱离本发明技术原理的情况下,对其进行改进和变形在本发明权利要求和技术之内,也应属于本发明的保护范围。 Art without departing from the principle of the invention, its improvements and modifications within the claims of the invention and technologies should also fall within the scope of the present invention.

Claims (4)

  1. 1. 一种离子液体化学镀铜的方法,其特征在于,该方法包括以下步骤: (1) 作为化学镀溶液的离子液体的配制;按摩尔比为1:2取氯化胆碱和尿素放入烧杯中,置于控温磁力搅拌器上保持恒温60°C加热,磁力搅拌0.5小时;待烧杯中形成均匀透明溶液后,将氯化铜、配位剂、还原剂和催化剂依次分别加入离子液体中,每次加入一种试剂之前溶液均要均匀透明,保温60°C磁力搅拌1小时,其中,按质量份数计,当步骤(1)获得的透明溶液为100份时,所述氯化铜为1〜3份,配位剂为2〜6份,还原剂为3〜7份,催化剂为 A method for electroless copper plating of an ionic liquid, wherein the method comprises the steps of: (1) electroless plating solution is formulated as an ionic liquid; molar ratio of 1: 2 to take place choline chloride and urea into a beaker placed in a constant temperature 60 ° C heating temperature on a magnetic stirrer or a magnetic stirring for 0.5 hours; after the formation of a uniform transparent solution to be beaker, cupric chloride, complexing agent, reducing agent and catalyst were added successively ions liquid, before each addition of a reagent solution have to be a uniform transparent, heat 60 ° C magnetically stirred for 1 hour, wherein the fraction of the total mass, when a clear solution in step (1) is obtained when 100 parts of the chlorine 1~3 parts copper to complexing agent is 2 ~ 6 parts, parts of reducing agent is 3~7, the catalyst is
    0.1〜0.4份;所述催化剂是镍、钴、铁的金属盐,浓度为0.5g/L〜2g/L; (2) 对印制电路板进行预处理,然后将电路板置于步骤(1)制得的化学镀溶液中,在50 〜80°C之间进行化学镀铜;。 0.1~0.4 parts; the catalyst is a nickel, cobalt, iron salts, at a concentration of 0.5g / L~2g / L; (2) pretreatment of the printed circuit board, and the board to step (1 ) prepared electroless plating solution, electroless copper plating between 50 ~80 ° C;.
  2. 2. 根据权利要求1所述的一种离子液体化学镀铜的方法,其特征在于:所述氯化铜的浓度为5g/L 〜15g/L。 2. A method according ionic liquid chemical copper plating according to claim 1, wherein: the concentration of the copper chloride was 5g / L ~15g / L.
  3. 3. 根据权利要求1所述的一种离子液体化学镀铜的方法,其特征在于:所述配位剂为酒石酸钠,其浓度为l〇g/L〜30g/L。 The copper plating method of an ionic liquid chemical according to claim 1, wherein: said complexing agent is sodium tartrate, at a concentration of l〇g / L~30g / L.
  4. 4. 根据权利要求1所述的一种离子液体化学镀铜的方法,其特征在于:所述还原剂为次磷酸钠,其浓度为15g/L〜35g/L。 The copper plating method of an ionic liquid chemical according to claim 1, wherein: the reducing agent is sodium hypophosphite, a concentration of 15g / L~35g / L.
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