CN105839099B - A kind of nickel plating surface chromium-free passivating treatment agent and treatment process - Google Patents
A kind of nickel plating surface chromium-free passivating treatment agent and treatment process Download PDFInfo
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Abstract
本发明属于钝化剂领域，公开了一种镀镍表面无铬钝化处理剂及处理工艺。所述无铬钝化处理剂由以下重量份的组分组成：氢氧化钠或氢氧化钾3～15份、水溶性过硫酸盐10～30份、水溶性硅酸盐1～10份、水溶性磷酸盐0～25份、水溶性钨酸盐0～25份、碳酸钠1～10份，去离子水20～85份。本发明的钝化处理剂无铬环保，不含挥发性酸或有机物，钝化过程中无挥发无气味，对生产环境友好。经本发明钝化剂处理后的钝化膜在提高对镀镍表面耐蚀性与抗氧化性的同时，保证镀镍层仍具备较好的导电性与焊接性能。The invention belongs to the field of passivation agents and discloses a chromium-free passivation treatment agent and a treatment process for nickel-plated surfaces. The chromium-free passivation treatment agent is composed of the following components in parts by weight: 3-15 parts of sodium hydroxide or potassium hydroxide, 10-30 parts of water-soluble persulfate, 1-10 parts of water-soluble silicate, water-soluble 0-25 parts of neutral phosphate, 0-25 parts of water-soluble tungstate, 1-10 parts of sodium carbonate, and 20-85 parts of deionized water. The passivation treatment agent of the present invention is chromium-free and environmentally friendly, does not contain volatile acid or organic matter, has no volatilization and odor during the passivation process, and is friendly to the production environment. The passivation film treated with the passivator of the invention improves the corrosion resistance and oxidation resistance of the nickel-plated surface while ensuring that the nickel-plated layer still has good electrical conductivity and welding performance.
Description
技术领域technical field
本发明属于钝化剂领域，具体涉及一种镀镍表面无铬钝化处理剂及处理工艺。The invention belongs to the field of passivating agents, and in particular relates to a chromium-free passivating treatment agent and a treatment process for nickel-plated surfaces.
背景技术Background technique
由于化学镀镍和电镀镍具有优良的硬度、耐磨性、耐蚀性、导电性及特殊磁学性等综合性能，所以广泛应用于汽车、石油、航天、机械装备、计算机及电子通信等重要领域。但是在大气或腐蚀环境下，镀镍表面容易形成镍的氧化物或硫化物，这层氧化物使镀层表面失去金属光泽、发黄变暗或出现斑点，严重影响镀层的外观效果。对于PCB领域，这层氧化物不仅增加了镀镍层表面的接触电阻，还降低了镀镍层的焊接性能，影响引线键合的强度和可靠性，容易造成焊接件的脱落。通常会对镀镍层表面进行钝化处理，以提高镀层的耐蚀性及抗氧化性，才能投入生产使用。Because electroless nickel plating and electroplating nickel have excellent comprehensive properties such as hardness, wear resistance, corrosion resistance, electrical conductivity and special magnetic properties, they are widely used in important industries such as automobiles, petroleum, aerospace, mechanical equipment, computers and electronic communications. field. However, in the atmospheric or corrosive environment, nickel oxides or sulfides are easily formed on the surface of nickel plating. This layer of oxides will cause the surface of the coating to lose its metallic luster, turn yellow and darken, or appear spots, which seriously affect the appearance of the coating. For the PCB field, this layer of oxide not only increases the contact resistance of the surface of the nickel plating layer, but also reduces the soldering performance of the nickel plating layer, affects the strength and reliability of the wire bonding, and easily causes the soldering parts to fall off. Passivation treatment is usually performed on the surface of the nickel plating layer to improve the corrosion resistance and oxidation resistance of the plating layer before it can be put into production.
铬酸盐钝化是传统的镀镍表面钝化处理技术，通过在镀层表面一层致密的铬酸盐钝化膜有效地提高镀层的耐蚀性及抗氧化性。但是六价铬对人体健康及生态环境都有极大的危害，致使铬酸盐钝化处理技术逐渐受到限制。欧盟RoHS指令规定将于2017年全面禁止含六价铬的电子产品进入欧洲境内进行销售，所以无铬钝化处理技术取代铬酸盐钝化处理技术已是大势所催。Chromate passivation is a traditional nickel plating surface passivation treatment technology, which can effectively improve the corrosion resistance and oxidation resistance of the coating through a dense chromate passivation film on the surface of the coating. However, hexavalent chromium is extremely harmful to human health and the ecological environment, which has gradually restricted the chromate passivation treatment technology. The EU RoHS Directive stipulates that electronic products containing hexavalent chromium will be completely banned from entering Europe for sale in 2017, so the chromium-free passivation treatment technology has replaced the chromate passivation treatment technology.
发明内容Contents of the invention
为了解决现有技术的缺点和不足之处，本发明的首要目的在于提供一种镀镍表面无铬钝化处理剂。该钝化处理剂在不影响镀层导电性、焊接性以及外观的前提下，实现的镀层耐蚀性和抗氧化性的显著提高。In order to solve the shortcomings and deficiencies of the prior art, the primary purpose of the present invention is to provide a chromium-free passivation treatment agent for nickel-plated surfaces. The passivation treatment agent significantly improves the corrosion resistance and oxidation resistance of the coating without affecting the conductivity, weldability and appearance of the coating.
本发明的另一目的在于提供一种采用上述无铬钝化处理剂对镀镍表面进行处理的工艺。Another object of the present invention is to provide a process for treating the nickel-plated surface by using the above-mentioned chromium-free passivation treatment agent.
本发明目的通过以下技术方案实现：The object of the invention is achieved through the following technical solutions:
一种镀镍表面无铬钝化处理剂，所述无铬钝化处理剂由以下重量份的组分组成：氢氧化钠或氢氧化钾3～15份、水溶性过硫酸盐10～30份、水溶性硅酸盐1～10份、水溶性磷酸盐0～25份、水溶性钨酸盐0～25份、碳酸钠1～10份，去离子水20～85份。A chromium-free passivation treatment agent for nickel-plated surfaces. The chromium-free passivation treatment agent consists of the following components in parts by weight: 3-15 parts of sodium hydroxide or potassium hydroxide, and 10-30 parts of water-soluble persulfate 1-10 parts of water-soluble silicate, 0-25 parts of water-soluble phosphate, 0-25 parts of water-soluble tungstate, 1-10 parts of sodium carbonate, 20-85 parts of deionized water.
上述处理剂中，所述水溶性过硫酸盐作为强氧化剂，优选地，所述水溶性过硫酸盐选自过硫酸钾或过硫酸钠。In the above treating agent, the water-soluble persulfate is used as a strong oxidizing agent, preferably, the water-soluble persulfate is selected from potassium persulfate or sodium persulfate.
上述处理剂中，所述水溶性硅酸盐作为成膜剂，优选地，所述水溶性硅酸盐是指硅酸钠。In the above treatment agent, the water-soluble silicate is used as a film-forming agent, preferably, the water-soluble silicate refers to sodium silicate.
上述处理剂中，所述水溶性磷酸盐和水溶性钨酸盐作为辅助成膜剂，优选地，所述水溶性磷酸盐是指磷酸钠，所述水溶性钨酸盐是指钨酸钠。Among the above treatment agents, the water-soluble phosphate and water-soluble tungstate are used as auxiliary film-forming agents, preferably, the water-soluble phosphate refers to sodium phosphate, and the water-soluble tungstate refers to sodium tungstate.
作为一种优选方案，所述无铬钝化处理剂由以下重量份的组分组成：氢氧化钠10份、过硫酸钾20份、硅酸钠5份、磷酸钠10份、碳酸钠3份、去离子水52份。As a preferred version, the chromium-free passivation treatment agent is composed of the following components by weight: 10 parts of sodium hydroxide, 20 parts of potassium persulfate, 5 parts of sodium silicate, 10 parts of sodium phosphate, and 3 parts of sodium carbonate , 52 parts of deionized water.
作为一种优选方案，所述无铬钝化处理剂由以下重量份的组分组成：氢氧化钠10份、过硫酸钾20份、硅酸钠5份、钨酸钠15份、碳酸钠3份、去离子水47份。As a preferred version, the chromium-free passivation treatment agent is composed of the following components by weight: 10 parts of sodium hydroxide, 20 parts of potassium persulfate, 5 parts of sodium silicate, 15 parts of sodium tungstate, 3 parts of sodium carbonate parts, 47 parts of deionized water.
作为一种优选方案，所述无铬钝化处理剂由以下重量份的组分组成：氢氧化钠10份、过硫酸钾20份、硅酸钠5份、碳酸钠3份、去离子水62份。As a preferred version, the chromium-free passivation treatment agent consists of the following components by weight: 10 parts of sodium hydroxide, 20 parts of potassium persulfate, 5 parts of sodium silicate, 3 parts of sodium carbonate, 62 parts of deionized water share.
一种采用上述无铬钝化处理剂对镀镍表面进行处理的工艺，包括如下步骤：将刚施镀完的镀镍工件立即浸入到上述无铬钝化处理剂中，在30～90℃条件下反应15～45min，取出后热水清洗，烘干，即可在镀镍表面得到一层钝化膜。A process for treating nickel-plated surfaces with the above-mentioned chromium-free passivation treatment agent, comprising the following steps: immediately immerse the nickel-plated workpiece just after plating into the above-mentioned chromium-free passivation treatment agent, React for 15 to 45 minutes, take it out, wash it with hot water, and dry it to get a passivation film on the nickel-plated surface.
本发明无铬钝化剂的作用机理为在含强氧化剂过硫酸盐的碱性溶液中，镀层表面的金属Ni被氧化形成Ni(OH)2和NiOOH，溶液中的硅酸根会与Ni(OH)2、NiOOH脱水缩合，并经过多次的硅酸缩聚反应，最终在镀镍表面形成一层聚硅酸薄膜。所以，本发明无铬钝化剂制备出的钝化膜层为双层结构，有利于阻挡腐蚀离子对基体的进攻，具有优异的耐蚀性及抗氧化性。The mechanism of action of the chromium-free passivator of the present invention is that in the alkaline solution containing strong oxidant persulfate, the metal Ni on the coating surface is oxidized to form Ni(OH) 2 and NiOOH, and the silicate in the solution will react with Ni(OH) ) 2. NiOOH is dehydrated and condensed, and after many times of silicic acid polycondensation reactions, a layer of polysilicate film is finally formed on the nickel-plated surface. Therefore, the passivation film prepared by the chromium-free passivator of the present invention has a double-layer structure, which is beneficial to blocking the attack of corrosion ions on the substrate, and has excellent corrosion resistance and oxidation resistance.
本发明具有如下优点及有益效果：The present invention has following advantage and beneficial effect:
(1)本发明的钝化剂成分简单环保，不含六价铬等有毒物质，不含挥发性酸或有机物，钝化过程中钝化液无挥发无气味，对生产环境友好；(1) The composition of the passivating agent of the present invention is simple and environmentally friendly, does not contain toxic substances such as hexavalent chromium, does not contain volatile acids or organic substances, and the passivating solution has no volatilization and odor during the passivation process, and is friendly to the production environment;
(2)本发明的钝化剂可循环使用，反复添加补充，且废液易于处理；(2) The passivating agent of the present invention can be recycled, repeatedly added and supplemented, and the waste liquid is easy to handle;
(3)经本发明的钝化剂处理后，镀镍表面的耐蚀性和抗氧化性都有显著提高，从电化学腐蚀测试数据及盐雾实验结果来看，该钝化剂有希望取代传统的铬酸盐钝化剂成为新型环保钝化剂；(3) After being treated with the passivating agent of the present invention, the corrosion resistance and oxidation resistance of the nickel-plated surface are significantly improved. From the electrochemical corrosion test data and salt spray test results, the passivating agent is expected to replace The traditional chromate passivation agent becomes a new environment-friendly passivation agent;
(4)本发明的钝化剂生成的钝化膜为十纳米左右厚度的透明薄膜，不影响镀镍层原有的金属光泽；在该钝化膜的保护下镀镍层仍具备较好的导电性与焊接性。(4) the passivation film that the passivation agent of the present invention generates is a transparent film with a thickness of about ten nanometers, which does not affect the original metallic luster of the nickel-plated layer; under the protection of the passivation film, the nickel-plated layer still possesses better Conductivity and solderability.
具体实施方式Detailed ways
下面结合实施例对本发明作进一步详细的描述，但本发明的实施方式不限于此。The present invention will be further described in detail below in conjunction with examples, but the embodiments of the present invention are not limited thereto.
实施例1Example 1
本实施例的一种镀镍表面无铬钝化处理剂，按照以下组分的重量份数配制而成：氢氧化钠10份、过硫酸钾20份、硅酸钠5份、磷酸钠10份、碳酸钠3份，去离子水52份。A kind of nickel-plated surface chromium-free passivation treatment agent of the present embodiment is formulated according to the parts by weight of the following components: 10 parts of sodium hydroxide, 20 parts of potassium persulfate, 5 parts of sodium silicate, 10 parts of sodium phosphate , 3 parts of sodium carbonate, 52 parts of deionized water.
上述镀镍表面无铬钝化处理剂按以下步骤制成：The above-mentioned nickel-plated surface chromium-free passivation treatment agent is made according to the following steps:
(1)将氢氧化钠倒入去离子水中，在常温常压下搅拌直至完全溶解；(1) Sodium hydroxide is poured into deionized water, and stirred at normal temperature and pressure until completely dissolved;
(2)将磷酸钠、硅酸钠和碳酸钠倒入步骤(1)得到的溶液，在常温常压下搅拌直至完全溶解；(2) Sodium phosphate, sodium silicate and sodium carbonate are poured into the solution obtained in step (1), and stirred at normal temperature and pressure until completely dissolved;
(3)将过硫酸钾倒入步骤(2)得到的溶液，在常温常压下搅拌直至完全溶解，得到所述无铬钝化处理剂。(3) Pour potassium persulfate into the solution obtained in step (2), and stir at normal temperature and pressure until completely dissolved to obtain the chromium-free passivation treatment agent.
采用上述无铬钝化处理剂对镀镍表面进行处理的工艺，包括如下步骤：The process of treating the nickel-plated surface by using the above-mentioned chromium-free passivation treatment agent comprises the following steps:
将钝化处理剂加热到70℃，并在这个温度下保温。把刚施镀完的镀镍工件完全浸入钝化液中，在70℃下反应30min，取出后用70℃热水清洗工件表面，然后在100℃烘箱内烘干处理20min，即可在镀镍表面得到一层钝化膜。Heat the passivation agent to 70°C and keep it warm at this temperature. Fully immerse the nickel-plated workpiece just finished plating in the passivation solution, react at 70°C for 30 minutes, take it out, wash the surface of the workpiece with hot water at 70°C, and then dry it in an oven at 100°C for 20 minutes, then the nickel-plated A passivation film is obtained on the surface.
实施例2Example 2
本实施例的一种镀镍表面无铬钝化处理剂，按照以下组分的重量份数配制而成：氢氧化钠10份、过硫酸钾20份、硅酸钠5份、钨酸钠15份、碳酸钠3份，去离子水47份。A chromium-free passivation treatment agent for nickel-plated surfaces of this embodiment is prepared according to the parts by weight of the following components: 10 parts of sodium hydroxide, 20 parts of potassium persulfate, 5 parts of sodium silicate, and 15 parts of sodium tungstate 3 parts, 3 parts of sodium carbonate, 47 parts of deionized water.
上述镀镍表面无铬钝化处理剂按以下步骤制成：The above-mentioned nickel-plated surface chromium-free passivation treatment agent is made according to the following steps:
(1)将氢氧化钠倒入去离子水中，在常温常压下搅拌直至完全溶解；(1) Sodium hydroxide is poured into deionized water, and stirred at normal temperature and pressure until completely dissolved;
(2)将钨酸钠、硅酸钠和碳酸钠倒入步骤(1)得到的溶液，在常温常压下搅拌直至完全溶解；(2) Pour sodium tungstate, sodium silicate and sodium carbonate into the solution obtained in step (1), and stir at normal temperature and pressure until completely dissolved;
(3)将过硫酸钾倒入步骤(2)得到的溶液，在常温常压下搅拌直至完全溶解，得到所述无铬钝化处理剂。(3) Pour potassium persulfate into the solution obtained in step (2), and stir at normal temperature and pressure until completely dissolved to obtain the chromium-free passivation treatment agent.
采用上述无铬钝化处理剂对镀镍表面进行处理的工艺，包括如下步骤：The process for treating the nickel-plated surface by using the above-mentioned chromium-free passivation treatment agent comprises the following steps:
将钝化处理剂加热到70℃，并在这个温度下保温。把刚施镀完的镀镍工件完全浸入钝化液中，在70℃下反应30min，取出后用70℃热水清洗工件表面，然后在100℃烘箱内烘干处理20min，即可在镀镍表面得到一层钝化膜。Heat the passivation agent to 70°C and keep it warm at this temperature. Fully immerse the nickel-plated workpiece just finished plating in the passivation solution, react at 70°C for 30 minutes, take it out, wash the surface of the workpiece with hot water at 70°C, and then dry it in an oven at 100°C for 20 minutes, then the nickel-plated A passivation film is obtained on the surface.
实施例3Example 3
本实施例的一种镀镍表面无铬钝化处理剂，按照以下组分的重量份数配制而成：氢氧化钠10份、过硫酸钾20份、硅酸钠5份、碳酸钠3份，去离子水62份。A kind of nickel-plated surface chromium-free passivation treatment agent of the present embodiment is formulated according to the parts by weight of the following components: 10 parts of sodium hydroxide, 20 parts of potassium persulfate, 5 parts of sodium silicate, 3 parts of sodium carbonate , 62 parts of deionized water.
上述镀镍表面无铬钝化处理剂按以下步骤制成：The above-mentioned nickel-plated surface chromium-free passivation treatment agent is made according to the following steps:
(1)将氢氧化钠倒入去离子水中，在常温常压下搅拌直至完全溶解；(1) Sodium hydroxide is poured into deionized water, and stirred at normal temperature and pressure until completely dissolved;
(2)将硅酸钠和碳酸钠倒入步骤(1)得到的溶液，在常温常压下搅拌直至完全溶解；(2) Sodium silicate and sodium carbonate are poured into the solution obtained in step (1), and stirred at normal temperature and pressure until fully dissolved;
(3)将过硫酸钾倒入步骤(2)得到的溶液，在常温常压下搅拌直至完全溶解，得到所述无铬钝化处理剂。(3) Pour potassium persulfate into the solution obtained in step (2), and stir at normal temperature and pressure until completely dissolved to obtain the chromium-free passivation treatment agent.
采用上述无铬钝化处理剂对镀镍表面进行处理的工艺，包括如下步骤：The process of treating the nickel-plated surface by using the above-mentioned chromium-free passivation treatment agent comprises the following steps:
将钝化处理剂加热到70℃，并在这个温度下保温。把刚施镀完的镀镍工件完全浸入钝化液中，在70℃下反应30min，取出后用70℃热水清洗工件表面，然后在100℃烘箱内烘干处理20min，即可在镀镍表面得到一层钝化膜。Heat the passivation agent to 70°C and keep it warm at this temperature. Fully immerse the nickel-plated workpiece just finished plating in the passivation solution, react at 70°C for 30 minutes, take it out, wash the surface of the workpiece with hot water at 70°C, and then dry it in an oven at 100°C for 20 minutes, then the nickel-plated A passivation film is obtained on the surface.
将实施例1、2、3和未经钝化处理的化学镀镍成品进行性能对比测试。电化学腐蚀测试采用三电极体系，腐蚀液为3.5wt.％NaCl水溶液，测试温度为室温(25℃)，参比电极为Ag/AgCl/sat.KCl。盐雾实验按照GB/T 10125-1997进行中性盐雾实验。结果如表1所示：Embodiment 1, 2, 3 and the electroless nickel-plated finished product without passivation treatment were carried out performance comparison test. The electrochemical corrosion test adopts a three-electrode system, the corrosion solution is 3.5wt.% NaCl aqueous solution, the test temperature is room temperature (25°C), and the reference electrode is Ag/AgCl/sat.KCl. Salt spray test The neutral salt spray test is carried out according to GB/T 10125-1997. The results are shown in Table 1:
表1Table 1
由表1结果可以看出，通过本发明的钝化剂处理后的镀镍表面的耐蚀性和抗氧化性都有显著提高，从电化学腐蚀测试数据及盐雾实验结果来看，本发明的钝化剂不影响镀镍层原有的金属光泽。As can be seen from the table 1 results, the corrosion resistance and oxidation resistance of the nickel-plated surface after the passivating agent treatment of the present invention are all significantly improved, from the electrochemical corrosion test data and salt spray test results, the present invention The passivating agent does not affect the original metallic luster of the nickel plating layer.
上述实施例为本发明较佳的实施方式，但本发明的实施方式并不受上述实施例的限制，其它的任何未背离本发明的精神实质与原理下所作的改变、修饰、替代、组合、简化，均应为等效的置换方式，都包含在本发明的保护范围之内。The above-mentioned embodiment is a preferred embodiment of the present invention, but the embodiment of the present invention is not limited by the above-mentioned embodiment, and any other changes, modifications, substitutions, combinations, Simplifications should be equivalent replacement methods, and all are included in the protection scope of the present invention.
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