CN101818368A - Electrodeposit nickel plating solution for deformation zinc alloy and electrodeposit nickel plating method thereof - Google Patents
Electrodeposit nickel plating solution for deformation zinc alloy and electrodeposit nickel plating method thereof Download PDFInfo
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Abstract
本发明公开了一种变形锌合金的电沉积镀镍溶液及其电沉积镀镍方法。本发明的电沉积镀镍溶液的溶剂为去离子水，溶质包含110～130g/L的六水合硫酸镍、10～15g/L的氯化钠、30～35g/L的硼酸、80～170g/L的柠檬酸钠。本发明的电沉积镀镍方法是在进行电沉积之前，将本发明的电沉积镀镍溶液的pH值调节为4.8～6.9，保持电沉积镀镍溶液的温度为20～30℃，阴极电流密度为0.8～1.5安培/分米2。本发明的电沉积镀镍溶液不含氰化物、无污染而且稳定性好；使用本发明的电沉积镀镍方法所得镀层表面无条纹，在金相显微镜下观察无裂纹，在150℃下热震无起泡剥落现象，涂膏表面变色面积不超过10％。
The invention discloses an electrodeposition nickel plating solution for deformed zinc alloy and an electrodeposition nickel plating method thereof. The solvent of the electrodeposition nickel plating solution of the present invention is deionized water, and the solute includes 110-130g/L nickel sulfate hexahydrate, 10-15g/L sodium chloride, 30-35g/L boric acid, 80-170g/L L of Sodium Citrate. The electrodeposition nickel-plating method of the present invention is before carrying out electrodeposition, the pH value of the electrodeposition nickel-plating solution of the present invention is adjusted to 4.8～6.9, the temperature that keeps the electrodeposition nickel-plating solution is 20～30 ℃, the cathodic current density It is 0.8-1.5 amperes/ dm2 . The electrodeposited nickel plating solution of the present invention does not contain cyanide, is pollution-free and has good stability; the surface of the coating obtained by using the electrodeposited nickel plating method of the present invention has no streaks, no cracks observed under a metallographic microscope, and thermal shock at 150 ° C. There is no blistering and peeling phenomenon, and the discoloration area of the pasted surface does not exceed 10%.
Description
技术领域technical field
本发明涉及变形锌合金的表面处理领域，尤其是涉及一种变形锌合金的电沉积镀镍溶液及其电沉积镀镍方法。The invention relates to the field of surface treatment of deformed zinc alloys, in particular to an electrodeposition nickel plating solution and an electrodeposition nickel plating method for deformed zinc alloys.
背景技术Background technique
锌合金是以锌为基加入其他元素组成的合金。锌合金的主要添加元素有铝，铜和镁等。按制造工艺，锌合金可分为铸造锌合金和变形锌合金。与传统的铸造锌合金相比，变形锌合金具有更高的蠕变强度和低温塑性，主要用于生产各种形状的锌材，是黄铜的替代材料，在电子、通讯、五金、制笔、卫浴等行业有广泛应用。Zinc alloy is an alloy composed of zinc as the base and other elements. The main additive elements of zinc alloy are aluminum, copper and magnesium. According to the manufacturing process, zinc alloy can be divided into cast zinc alloy and deformed zinc alloy. Compared with traditional cast zinc alloys, wrought zinc alloys have higher creep strength and low-temperature plasticity, and are mainly used to produce zinc materials of various shapes. , sanitary ware and other industries are widely used.
通常，对锌合金进行表面处理可以加强锌合金的耐腐蚀性能和装饰性能。对变形锌合金而言，由于铝含量较高以及使用挤压成型的加工过程，具有较高的化学活性，因此同样需要使用表面处理的方法加强其耐腐蚀性能和装饰性能。Generally, surface treatment of zinc alloys can enhance the corrosion resistance and decorative properties of zinc alloys. For wrought zinc alloys, due to the high aluminum content and the high chemical activity of the extrusion molding process, it is also necessary to use surface treatment methods to enhance its corrosion resistance and decorative properties.
传统方法中，一般使用氰化物作为铜电镀工艺的成份而在锌合金表面电镀铜，但是由于镀敷溶液中含有的氰化物具有毒性，将污染环境且危害健康，所以正在被其他无毒的镀敷溶液取代。目前，适用于镁合金表面电镀的中性镀镍工艺在锌合金表面都得到了发展，中性镀镍工艺具有环境友好无污染的优点，在一定程度上能够替代氰化物镀铜工艺而用于锌合金表面电镀。但是，目前锌合金表面的中性镀镍工艺主要集中应用于压铸成型的铸造锌合金，另外，中性镀镍的镀液成分和工艺条件并不适合于变形锌合金，存在镀层出现裂纹，将会影响本身镀层性能和后续镀种，以及镀液稳定性差，维护困难等问题。In the traditional method, cyanide is generally used as a component of the copper electroplating process to electroplate copper on the surface of zinc alloy, but because the cyanide contained in the plating solution is toxic, it will pollute the environment and endanger health, so it is being used by other non-toxic plating. Apply solution instead. At present, the neutral nickel plating process suitable for electroplating on the surface of magnesium alloy has been developed on the surface of zinc alloy. Zinc alloy surface plating. However, the current neutral nickel plating process on the surface of zinc alloys is mainly applied to cast zinc alloys formed by die casting. In addition, the composition and process conditions of the neutral nickel plating solution are not suitable for deformed zinc alloys, and there are cracks in the coating, which will It will affect the performance of its own coating and subsequent plating, as well as poor stability of the plating solution and difficult maintenance.
因此，针对目前变形锌合金表面处理的现状，急需寻找一种适合于变形锌合金，而且环保稳定的表面处理工艺。Therefore, in view of the current status of surface treatment of wrought zinc alloys, it is urgent to find a surface treatment process suitable for wrought zinc alloys that is environmentally friendly and stable.
发明内容Contents of the invention
本发明所要解决的技术问题是针对上述技术现状而提供一种变形锌合金的电沉积镀镍溶液及其电沉积镀镍方法。The technical problem to be solved by the present invention is to provide an electrodeposition nickel plating solution and an electrodeposition nickel plating method for wrought zinc alloy in view of the above-mentioned technical status.
本发明解决上述技术问题所采用的技术方案为：The technical solution adopted by the present invention to solve the problems of the technologies described above is:
一种变形锌合金的电沉积镀镍溶液，溶剂为去离子水，溶质的各组分及其浓度如下：A kind of electrodeposition nickel-plating solution of deformation zinc alloy, solvent is deionized water, each component of solute and concentration thereof are as follows:
六水合硫酸镍 110～130g/L；Nickel sulfate hexahydrate 110～130g/L;
氯化钠 10～15g/L；Sodium chloride 10～15g/L;
硼酸 30～35g/L；Boric acid 30～35g/L;
柠檬酸钠 80～170g/L。
一种变形锌合金的电沉积镀镍方法，包括如下步骤：A method for electrodeposition nickel plating of deformed zinc alloys, comprising the steps of:
步骤1：配制电沉积镀镍溶液，该电沉积镀镍溶液的组分及其浓度如下：Step 1: prepare the electro-deposition nickel plating solution, the components and concentrations of the electrodeposition nickel-plating solution are as follows:
六水合硫酸镍 110～130g/L；Nickel sulfate hexahydrate 110～130g/L;
氯化钠 10～15g/L；Sodium chloride 10～15g/L;
硼酸 30～35g/L；Boric acid 30～35g/L;
柠檬酸钠 80～170g/L；
步骤2：使用氢氧化钠溶液调节步骤1得到的电沉积镀镍溶液的pH值为4.8～6.9，然后过滤；保持电沉积镀镍溶液的温度为20～30℃；Step 2: Using sodium hydroxide solution to adjust the pH value of the electrodeposition nickel plating solution obtained in step 1 to 4.8 to 6.9, and then filter; keep the temperature of the electrodeposition nickel plating solution at 20 to 30°C;
步骤3：将经除油的变形锌合金浸入电沉积镀镍溶液中，设定阴极电流密度为0.8～1.5安培/分米2，进行电沉积镀镍。Step 3: immerse the degreased deformed zinc alloy in the electro-deposition nickel-plating solution, set the cathode current density at 0.8-1.5 ampere/ dm2 , and perform electro-deposition nickel-plating.
为优化上述技术方案，采取的措施还包括：In order to optimize the above technical solutions, the measures taken also include:
上述步骤1中配置电沉积镀镍溶液的过程如下：The process of configuring the electrodeposition nickel plating solution in the above-mentioned step 1 is as follows:
(1)柠檬酸钠加去离子水溶解；(1) Sodium citrate is dissolved in deionized water;
(2)六水合硫酸镍、氯化钠加去离子水溶解；(2) Nickel sulfate hexahydrate, sodium chloride add deionized water to dissolve;
(3)硼酸加热去离子水溶解；(3) Boric acid is heated and dissolved in deionized water;
(4)把(2)溶液倒入(1)溶液中，搅拌均匀；(4) Pour (2) solution into (1) solution and stir evenly;
(5)将(3)溶液倒入(4)溶液中，搅拌均匀。(5) Pour (3) solution into (4) solution and stir evenly.
上述步骤2中的氢氧化钠溶液的浓度为10mol/L。The concentration of the sodium hydroxide solution in the above step 2 is 10mol/L.
与现有技术相比，本发明一种变形锌合金的电沉积镀镍溶液不含氰化物，对环境无污染，并且稳定性好，使用周期长；使用本发明的镀镍方法所得镀层表面无条纹，在金相显微镜下观察无裂纹，在150℃下热震无起泡剥落现象，涂覆在镀层表面用于测孔隙的膏状物(以下简称涂膏)的表面变色面积不超过10％。Compared with the prior art, the electrodeposited nickel plating solution of a deformed zinc alloy of the present invention does not contain cyanide, has no pollution to the environment, and has good stability and long service life; Streaks, no cracks observed under a metallographic microscope, no blistering and peeling under thermal shock at 150°C, the surface discoloration area of the paste (hereinafter referred to as paste) coated on the surface of the coating for measuring pores does not exceed 10% .
附图说明Description of drawings
图1是对应本发明实施例的电沉积镀镍溶液中pH值与柠檬酸钠含量，电沉积镀镍溶液的稳定性与镀镍后镀层特点示意图。Fig. 1 is a schematic diagram of the pH value and sodium citrate content in the electrodeposited nickel plating solution corresponding to the embodiment of the present invention, the stability of the electrodeposited nickel plating solution and the characteristics of the coating after nickel plating.
具体实施方式Detailed ways
以下结合附图实施例对本发明作进一步详细描述。The present invention will be further described in detail below in conjunction with the accompanying drawings and embodiments.
本发明一种变形锌合金的电沉积镀镍溶液的溶剂为去离子水，溶质的各组分及其浓度如下：The solvent of the electrodeposition nickel-plating solution of a kind of deformation zinc alloy of the present invention is deionized water, and each component of solute and concentration thereof are as follows:
六水合硫酸镍 110～130g/L；Nickel sulfate hexahydrate 110～130g/L;
氯化钠 10～15g/L；Sodium chloride 10～15g/L;
硼酸 30～35g/L；Boric acid 30～35g/L;
柠檬酸钠 80～170g/L。
上述一种变形锌合金的电沉积镀镍溶液的配制过程如下：The preparation process of the electrodeposited nickel plating solution of above-mentioned a kind of deformation zinc alloy is as follows:
(1)把上述配方中的柠檬酸钠加去离子水溶解；(1) Add the sodium citrate in the above formula to dissolve in deionized water;
(2)把上述配方中的六水合硫酸镍、氯化钠加去离子水溶解；(2) Nickel sulfate hexahydrate, sodium chloride in the above-mentioned formula are added and dissolved in deionized water;
(3)把上述配方中的硼酸加热去离子水溶解；(3) Boric acid in the above formula is heated and dissolved in deionized water;
(4)把(2)溶液倒入(1)溶液中，搅拌均匀；(4) Pour (2) solution into (1) solution and stir evenly;
(5)把(3)溶液倒入(4)溶液中，搅拌均匀；(5) Pour (3) solution into (4) solution, stir evenly;
图1是对应本发明的电沉积镀镍溶液中pH值与柠檬酸钠含量，电沉积镀镍溶液的稳定性与镀镍后镀层特点示意图。Fig. 1 is the pH value and sodium citrate content in the electro-deposition nickel-plating solution of the present invention, the stability of the electro-deposition nickel-plating solution and the characteristic diagram of the coating after nickel plating.
从图1可以看出，当本发明的电沉积镀镍溶液中pH值与柠檬酸钠含量的交叉点分别位于A区、B区、C区和D区时，电沉积镀镍溶液与电沉积镀镍后得到的镀层具有如下的特点：As can be seen from Fig. 1, when the intersection point of pH value and sodium citrate content in the electrodeposition nickel-plating solution of the present invention is positioned at A district, B district, C district and D district respectively, when electro-deposition nickel-plating solution and electrodeposition The coating obtained after nickel plating has the following characteristics:
A区：电沉积镀镍溶液稳定性差，出现浑浊沉淀现象。Area A: Electrodeposited nickel plating solution has poor stability and turbid precipitation occurs.
B区：电沉积镀层表面出现条纹，外观不合格。Area B: Streaks appear on the surface of the electrodeposited coating, and the appearance is unqualified.
C区：电沉积镀层表面无条纹，在金相显微镜下观察无裂纹，在150℃下热震无起泡剥落现象，涂膏表面变色面积不超过10％。Zone C: There are no streaks on the surface of the electrodeposited coating, no cracks observed under a metallographic microscope, no blistering and peeling off under thermal shock at 150°C, and the discoloration area of the paste surface does not exceed 10%.
D区：镀层表面无条纹，在金相显微镜下观察有裂纹，在150℃下热震出现起泡剥落现象，涂膏表面变色面积超过10％。Zone D: There are no streaks on the surface of the coating, but there are cracks observed under a metallographic microscope. Bubbles and peeling appear in thermal shock at 150°C, and the discoloration area of the paste surface exceeds 10%.
由此可以得出，当本发明的电沉积镀镍溶液位于C区时(pH值为4.8～6.9)，对变形锌合金进行电沉积镀镍后，变形锌合金表面得到性能良好的镀层。It can be concluded that, when the electrodeposited nickel plating solution of the present invention is located in zone C (pH value is 4.8-6.9), after the deformed zinc alloy is subjected to electrodeposited nickel plating, the surface of the deformed zinc alloy is coated with good performance.
实施例1：Example 1:
一种变形锌合金的电沉积镀镍溶液的各组分及其含量如下：Each component and content thereof of the electrodeposition nickel-plating solution of a kind of wrought zinc alloy are as follows:
六水合硫酸镍 110g/L；Nickel sulfate hexahydrate 110g/L;
氯化钠 12g/L；Sodium chloride 12g/L;
硼酸 30g/L；Boric acid 30g/L;
柠檬酸钠 80g/L。Sodium citrate 80g/L.
将以上各组分按照前述的配制过程配制电沉积镀镍溶液；使用10mol/L的氢氧化钠溶液调节该电沉积镀镍溶液的pH值为6.9；保持电沉积镀镍溶液的温度为30℃；将经除油的变形锌合金浸入电沉积镀镍溶液中，设定阴极电流密度为0.8安培/分米2，进行电沉积镀镍。所得镀层表面无条纹，在金相显微镜下观察无裂纹，在150℃下热震无起泡剥落现象，涂膏表面变色面积不超过10％。The above components are prepared according to the aforementioned preparation process to prepare an electrodeposition nickel plating solution; use 10mol/L sodium hydroxide solution to adjust the pH value of the electrodeposition nickel plating solution to 6.9; keep the temperature of the electrodeposition nickel plating solution at 30°C ; Immerse the degreased deformed zinc alloy in the electro-deposition nickel-plating solution, set the cathode current density to 0.8 ampere/decimeter 2 , and perform electro-deposition nickel-plating. The surface of the obtained coating has no streaks, no cracks observed under a metallographic microscope, no blistering and peeling phenomenon under thermal shock at 150° C., and the discoloration area of the pasted surface does not exceed 10%.
实施例2：Example 2:
一种变形锌合金的电沉积镀镍溶液的各组分及其含量如下：Each component and content thereof of the electrodeposition nickel-plating solution of a kind of wrought zinc alloy are as follows:
六水合硫酸镍 120g/L；Nickel sulfate hexahydrate 120g/L;
氯化钠 10g/L；Sodium chloride 10g/L;
硼酸 30g/L；Boric acid 30g/L;
柠檬酸钠 120g/L。Sodium citrate 120g/L.
将以上各组分按照前述的配制过程配制电沉积镀镍溶液；使用10mol/L的氢氧化钠溶液调节该电沉积镀镍溶液的pH值为6.0；保持电沉积镀镍溶液的温度为25℃；将经除油的变形锌合金浸入电沉积镀镍溶液中，设定阴极电流密度为1.0安培/分米2，进行电沉积镀镍。所得镀层表面无条纹，在金相显微镜下观察无裂纹，在150℃下热震无起泡剥落现象，涂膏表面变色面积不超过10％。The above components are prepared according to the aforementioned preparation process to prepare an electrodeposition nickel plating solution; use 10mol/L sodium hydroxide solution to adjust the pH value of the electrodeposition nickel plating solution to 6.0; keep the temperature of the electrodeposition nickel plating solution at 25°C ; Immerse the degreased deformed zinc alloy in the electro-deposition nickel-plating solution, set the cathode current density to 1.0 ampere/ dm2 , and perform electro-deposition nickel-plating. The surface of the obtained coating has no streaks, no cracks observed under a metallographic microscope, no blistering and peeling phenomenon under thermal shock at 150° C., and the discoloration area of the pasted surface does not exceed 10%.
实施例3：Example 3:
一种变形锌合金的电沉积镀镍溶液的各组分及其含量如下：Each component and content thereof of the electrodeposition nickel-plating solution of a kind of wrought zinc alloy are as follows:
六水合硫酸镍 130g/L；Nickel sulfate hexahydrate 130g/L;
氯化钠 15g/L；Sodium chloride 15g/L;
硼酸 35g/L；Boric acid 35g/L;
柠檬酸钠 170g/L。Sodium citrate 170g/L.
将以上各组分按照前述的配制过程配制电沉积镀镍溶液；使用10mol/L的氢氧化钠溶液调节该电沉积镀镍溶液的pH值为4.8；保持电沉积镀镍溶液的温度为20℃；将经除油的变形锌合金浸入电沉积镀镍溶液中，设定阴极电流密度为1.5安培/分米2，进行电沉积镀镍。所得镀层表面无条纹，在金相显微镜下观察无裂纹，在150℃下热震无起泡剥落现象，涂膏表面变色面积不超过10％。The above components are prepared according to the aforementioned preparation process for electro-deposition nickel plating solution; use 10mol/L sodium hydroxide solution to adjust the pH value of the electrodeposition nickel-plating solution to 4.8; keep the temperature of the electrodeposition nickel-plating solution at 20°C ; Immerse the degreased deformed zinc alloy in the electro-deposition nickel-plating solution, set the cathode current density to 1.5 amps/ dm2 , and perform electro-deposition nickel-plating. The surface of the obtained coating has no streaks, no cracks observed under a metallographic microscope, no blistering and peeling phenomenon under thermal shock at 150° C., and the discoloration area of the pasted surface does not exceed 10%.
实施例4：Example 4:
一种变形锌合金的电沉积镀镍溶液的各组分及其含量如下：Each component and content thereof of the electrodeposition nickel-plating solution of a kind of wrought zinc alloy are as follows:
六水合硫酸镍 115g/L；Nickel sulfate hexahydrate 115g/L;
氯化钠 12g/L；Sodium chloride 12g/L;
硼酸 35g/L；Boric acid 35g/L;
柠檬酸钠 100g/L。Sodium citrate 100g/L.
将以上各组分按照前述的配制过程配制电沉积镀镍溶液；使用10mol/L的氢氧化钠溶液调节该电沉积镀镍溶液的pH值为6.5；保持电沉积镀镍溶液的温度为25℃；将经除油的变形锌合金浸入电沉积镀镍溶液中，设定阴极电流密度为1.0安培/分米2，进行电沉积镀镍。所得镀层表面无条纹，在金相显微镜下观察无裂纹，在150℃下热震无起泡剥落现象，涂膏表面变色面积不超过10％。Prepare the above-mentioned components according to the aforementioned preparation process to prepare an electrodeposition nickel plating solution; use 10mol/L sodium hydroxide solution to adjust the pH value of the electrodeposition nickel plating solution to 6.5; keep the temperature of the electrodeposition nickel plating solution at 25°C ; Immerse the degreased deformed zinc alloy in the electro-deposition nickel-plating solution, set the cathode current density to 1.0 ampere/ dm2 , and perform electro-deposition nickel-plating. The surface of the obtained coating has no streaks, no cracks observed under a metallographic microscope, no blistering and peeling phenomenon under thermal shock at 150° C., and the discoloration area of the pasted surface does not exceed 10%.
实施例5：Example 5:
一种变形锌合金的电沉积镀镍溶液的各组分及其含量如下：Each component and content thereof of the electrodeposition nickel-plating solution of a kind of wrought zinc alloy are as follows:
六水合硫酸镍 125g/L；Nickel sulfate hexahydrate 125g/L;
氯化钠 15g/L；Sodium chloride 15g/L;
硼酸 33g/L；Boric acid 33g/L;
柠檬酸钠 150g/L。Sodium citrate 150g/L.
将以上各组分按照前述的配制过程配制电沉积镀镍溶液；使用10mol/L的氢氧化钠溶液调节该电沉积镀镍溶液的pH值为5.3；保持电沉积镀镍溶液的温度为20℃；将经除油的变形锌合金浸入电沉积镀镍溶液中，设定阴极电流密度为1.5安培/分米2，进行电沉积镀镍。所得镀层表面无条纹，在金相显微镜下观察无裂纹，在150℃下热震无起泡剥落现象，涂膏表面变色面积不超过10％。The above components are prepared according to the aforementioned preparation process to prepare an electrodeposition nickel plating solution; use 10mol/L sodium hydroxide solution to adjust the pH value of the electrodeposition nickel plating solution to 5.3; keep the temperature of the electrodeposition nickel plating solution at 20°C ; Immerse the degreased deformed zinc alloy in the electro-deposition nickel-plating solution, set the cathode current density to 1.5 amps/ dm2 , and perform electro-deposition nickel-plating. The surface of the obtained coating has no streaks, no cracks observed under a metallographic microscope, no blistering and peeling phenomenon under thermal shock at 150° C., and the discoloration area of the pasted surface does not exceed 10%.
本发明的最佳实施例已阐明，由本领域普通技术人员做出的各种变化或改型都不会脱离本发明的范围。The preferred embodiment of the present invention has been illustrated, and various changes or modifications may be made by those skilled in the art without departing from the scope of the present invention.
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| CN103540968A (en) * | 2013-09-24 | 2014-01-29 | 成都泛华航空仪表电器有限公司 | Process method for electroplating nickel on aluminum-copper composite material component |
| CN103966633A (en) * | 2013-02-01 | 2014-08-06 | 金华东威表面处理科技有限公司 | Nickel plating solution |
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| 《镀镍工艺基础》 20070131 陈天玉 其他类型镍盐镀镍 化学工艺出版社 271、272 1-4 , 第1版 1 * |
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| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103966633A (en) * | 2013-02-01 | 2014-08-06 | 金华东威表面处理科技有限公司 | Nickel plating solution |
| CN103966633B (en) * | 2013-02-01 | 2017-05-24 | 金华东威表面处理科技有限公司 | Nickel plating solution |
| CN103540968A (en) * | 2013-09-24 | 2014-01-29 | 成都泛华航空仪表电器有限公司 | Process method for electroplating nickel on aluminum-copper composite material component |
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