铝、镁合金化学镀镍机理与工艺研究
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摘要
由于镁合金和铝合金是轻质工程材料，并具有许多优良性能，如密度小，强度高，易于压力加工等特点，在军工、汽车、航空航天，摩托和电子通讯等行业中得到广泛的应用，成为一种常用的结构材料。但是铝、镁合金具有一个共同的特点是它们的化学活性较高，硬度低，耐蚀耐磨性差等，这些弱点影响了该材料发挥其优势。通常需要采用表面处理技术以改进其制件的表面性能来提高其耐蚀耐磨性能。通过化学镀镍可以提高铝，镁合金表面硬度，耐腐蚀，耐磨性，并可赋予铝，镁合金表面许多功能特性，如焊接性，可抛光性等。
本论文研究了不同前处理方法对AZ91D镁合金化学镀镍镀层性能的影响，确立了适合于化学镀镍的环保前处理工艺；探讨了开发的绿色前处理工艺的界面反应机理；研究了化学镀镍的主要影响因素；同时研究了镀液中的化学反应速率动力学方程。对铝合金研究在中等温下进行直接化学镀镍(70°C)的工艺及反应机理，研究镁合金硫酸镍主盐的化学镀镍镀液，降低生产成本，提高镀液的稳定性。通过加入活化剂(KF)和调整主配合剂来提高化学镀镍的速度。开发低成本长寿命的硫酸镍主盐的铝，镁合金化学镀镍溶液，并对其反应机理和工艺进行了剖析。
采用重量法，扫描电子显微镜(SEM)，X-射线衍射(XRD)，发射扫描电子(FSEM)，X-射线探测器(EDX)，环境扫描电镜(ESEM)和电化学测试等检测方法，对铝，镁合金的前处理后的表面形貌和成分，镀层表面形貌，镀层断面形貌，镀镍层进行表征。通过氯化钠溶液的浸泡实验来测定镀层的孔隙率，评定镀层的致密性。应用电化学开路电势—时间曲线和镀层阳极极化曲线来分析活化剂和不同配合剂的作用效果，解释其反应机理。研究结果表明：
1.（1）经HNO_3+CrO_3酸洗→HF活化的前处理，（2）HNO_3+H_3PO_4酸洗→K_4P_2O_7活化→NH_4HF_2活化的前处理所得镁合金基底能够获得合适的氟化膜表面粘附物质，有效地防止镁合金基底在镀液中的腐蚀。（3）经过HNO_3+CrO_3酸洗后→K_4P_2O_7活化→浸锌的前处理工艺，最好能能形成一层致密的锌膜，这层金属锌膜既能防止基底上的镁腐蚀，又能提高表面的电沉积和化学沉积的活性。三种不同前处理后获得的镁合金基底表面粗糙，且形成了不同程度的刻蚀粗糙度，能够增强镀层与基底的结合力。
2.经过HNO_3+H_3PO_4酸洗→K_4P_2O_7活化→NH_4HF_2溶液二次活化处理，获得的镁合金基底表面有着适当的F/O比值(1.2:1)，能够为镍的初始沉积提供适当的活性点，适当比例的氟化膜能有效的防止镀液中的氢离子腐蚀和镍离子的置换反应，避免对镁基体的腐蚀和形成无结合力的镀层。这样的表面处理获得的化学镀镍层具有良好的耐蚀性和结合力。该前处理溶液中没有铬盐，是一种低毒性的较为环保的镁合金表面处理方法。
3.采用硫酸镍主盐的化学镀液，其镀液中主盐、还原剂浓度一般维持在20~28g·dm~(-3)。化学镀镍在60℃开始施镀，在80~90℃镀液才能正常工作。当施镀次数超过三次后，沉积速度降至8.127μm·h~(-1)，硫酸镍浓度降至16.56g·dm~(-3)。需要补充主盐和还原剂才能进行正常的化学镀镍，镀液需要维护。
4.铝合金化学镀镍溶液中加入活化剂后，会使基体表面的氧化物溶解，露出更多铝合金基材，使其电极电势出现负移，适宜浓度(2～4g·dm~(-3))的活化剂可以加快化学诱发沉积镍的速度，实现6063铝合金在中温条件下直接化学镀镍，提高化学沉积的速度，改善镀层的综合性能。但过高浓度(>4g·dm~(-3))的活化剂会对镀层产生严重的腐蚀作用。
5.采用氨基乙酸为主配合剂，进行铝合金化学镀镍时，提高了镀速，获得了致密的化学镀镍层，其镀层的耐蚀性能明显改善，镀层在腐蚀介质中腐蚀电势提高，腐蚀电流降低，耐色变性也得到了明显的提高。化学镀镍的沉积速度随氨基乙酸质量浓度的增加而下降。活化剂浓度为2g·dm~(-3)，氨基乙酸浓度为8g·dm~(-3)时，能得到的综合性能良好的Ni P镀层。
Aluminum and magnesium alloys are widely uesd in many fields: military,automobile, aerospace, mechanical and electronic components, etc, because they havemany attrative properties, such as: low density, high intensity and easy to pressureprocessing, etc. However, aluminum and magnesium alloys have some commonshortcomings. Aluminum and magnesium alloys are intrinsically high reactive, andare easily oxidized to form oxidation film in the dry air. They have poor corrosionresistance and wearability, low hardness, which are actually one of the main obstaclesto the application of aluminum and magnesium alloys in practical environments.Electroless nickel plating is one of the effective surface modifications for aluminum,magnesium and its alloys. It not only improves the wear resistance and corrosionresistance, but also improve the hardness, wear resistance and electrical contactperformance. Electroless nickel plating has widely been applied in many industries.Ni-P coating exhibits all sort of new functions, such as magnetic property, lubricationperformance, etc. Therefore, the performances of electroless nickel plating coatingson AZ91D magnesium alloys obtained via different pretreatments have been studiedin this dissertation. We aim to develop an appropriate, environmental-friendlypretreatment technique for meeting the needs of industrial production. The interfacereaction mechanism of the environmental-friendly pretreatment was analyzed. Themain factors of electroless nickel plating were studied. At the same time, thedynamics equation of the acidic electroless plating on magnesium alloys was studied.In addition, the reaction mechanism and process of direct electroless nickel plating on6063aluminum alloy in temperature (70℃) were studied. The additive (fluoridecompound) was used and the main complexing agent was adjusted in the plating bathto improve the deposition rate of the electroless nickel plating. As far as aluminumand magnesium alloys are concerned, the main salts of electroless plating solutionsmostly focus attentions on basic nickel carbonate or nickel acetate, which result inhigh-cost, low-efficiency, instability of electroless plating solutions and littleapplications. There have important theoretic and practical signification of theelectroless plating on aluminum and magnesium alloys. Additionally, the platingmechanism and process are studied, by using low-cost, long-life NiSO_4·6H2O as themain salt.
In this dissertation, the electroless nickel plating on aluminum, and magnesiumalloys was studied in detail by means of weight method, Scanning ElectronMicroscope (SEM), X-ray Diffraction (XRD), Energy Dispersed X-ray spectrometer(EDX) Environmental Scanning Electron Microscope (ESEM) and electrochemistrymethods, etc. These measurement techniques were applied in the investigations ofpre-treatment process, the surface morphology and the cross section views of thecoatings, the analysis of the coating surface, the coating porosity and its evaluationmethod, the new electroless plating process，and so on.
Experimental results showed that:
1. Three different pre-treatments were studied, and the surface properties of thepretreated magnesium alloys were characterized by means of SEM, EDX andelectrochemical method. The results showed that the different degrees of corrosionwere produced on the surface of magnesium alloys. There had some deep cavities onthe surface and a coarse surface was all formed. The coarse surface can augment themechanical occlusive force between the coatings and the substrates. A compactfluoride film was formed on the surface of the specimen via (1) HNO_3+CrO_3pickling→HF activation or (2) HNO_3+H_3PO_4pickling→K_4P_2O_7activation→NH_4HF_2activation. The fluoride film can hinder the magnesium alloys from furtherdissolution. A zinc film was produced on the substrate via (3) HNO_3+CrO_3pickling→K_4P_2O_7activation→zinc immersion, which can also effectively protect themagnesium alloys from corrosion.
2. After the surfaces of magnesium alloys were pretreated via HNO_3+H_3PO_4pickling→K_4P_2O_7activation→NH_4HF_2activation. There was suitable F/O (1.2:1)on the substrate surface, which can provide appropriate active points, and effectivelyprotect the magnesium alloys from corrosion in the bath. The Ni-P coating had goodappearance, good corrosion resistance and excellent adhesion. The usage of the toxicsubstances in this pretreatment was avoided. Therefore, it was a chromium-free, lowfluoride and environmental-friendly pretreatment technology.
3. In the electroless plating acidic solutions using NiSO_4·6H2O as the main salt,both nickel salt and reducing agent were generally maintained between20~28g·dm~(-3).The temperature of electroless nickel plating was controlled to be80℃~90℃. Thedeposition rate was reduced to8.127μm·h-1and the concentration of nickel sulfatewas reduced to16.56g·dm~(-3)after more than twice platings. We need to supplenmentthe main salt and reducing agent arc needed in order to carry out normal electrolessnickel plating bath.
4. Appropriate concentrations of additive can accelerate the rate of chemicallyinduced nickel deposition, and realize direct electroless nickel plating on6063aluminum alloy in medium temperature (70℃). The additive can play important rolesin accelerating the deposition rate and improving the comprehensive performance ofcoatings.
5. Aminoacetic acid as a main complexing agent in the bath can controlreasonable plating rate of electroless nickel plating, and produce high quality coatingwith high corrosion resistance, good adhesion. The resistance of color degenerationalso got obvious improvement. When the additive was adjusted to2g·dm~(-3)and theaminoacetic was controlled to8g·dm~(-3), the Ni–P coating with better comprehensiveperformance was obtained.
本论文研究了不同前处理方法对AZ91D镁合金化学镀镍镀层性能的影响，确立了适合于化学镀镍的环保前处理工艺；探讨了开发的绿色前处理工艺的界面反应机理；研究了化学镀镍的主要影响因素；同时研究了镀液中的化学反应速率动力学方程。对铝合金研究在中等温下进行直接化学镀镍(70°C)的工艺及反应机理，研究镁合金硫酸镍主盐的化学镀镍镀液，降低生产成本，提高镀液的稳定性。通过加入活化剂(KF)和调整主配合剂来提高化学镀镍的速度。开发低成本长寿命的硫酸镍主盐的铝，镁合金化学镀镍溶液，并对其反应机理和工艺进行了剖析。
采用重量法，扫描电子显微镜(SEM)，X-射线衍射(XRD)，发射扫描电子(FSEM)，X-射线探测器(EDX)，环境扫描电镜(ESEM)和电化学测试等检测方法，对铝，镁合金的前处理后的表面形貌和成分，镀层表面形貌，镀层断面形貌，镀镍层进行表征。通过氯化钠溶液的浸泡实验来测定镀层的孔隙率，评定镀层的致密性。应用电化学开路电势—时间曲线和镀层阳极极化曲线来分析活化剂和不同配合剂的作用效果，解释其反应机理。研究结果表明：
1.（1）经HNO_3+CrO_3酸洗→HF活化的前处理，（2）HNO_3+H_3PO_4酸洗→K_4P_2O_7活化→NH_4HF_2活化的前处理所得镁合金基底能够获得合适的氟化膜表面粘附物质，有效地防止镁合金基底在镀液中的腐蚀。（3）经过HNO_3+CrO_3酸洗后→K_4P_2O_7活化→浸锌的前处理工艺，最好能能形成一层致密的锌膜，这层金属锌膜既能防止基底上的镁腐蚀，又能提高表面的电沉积和化学沉积的活性。三种不同前处理后获得的镁合金基底表面粗糙，且形成了不同程度的刻蚀粗糙度，能够增强镀层与基底的结合力。
2.经过HNO_3+H_3PO_4酸洗→K_4P_2O_7活化→NH_4HF_2溶液二次活化处理，获得的镁合金基底表面有着适当的F/O比值(1.2:1)，能够为镍的初始沉积提供适当的活性点，适当比例的氟化膜能有效的防止镀液中的氢离子腐蚀和镍离子的置换反应，避免对镁基体的腐蚀和形成无结合力的镀层。这样的表面处理获得的化学镀镍层具有良好的耐蚀性和结合力。该前处理溶液中没有铬盐，是一种低毒性的较为环保的镁合金表面处理方法。
3.采用硫酸镍主盐的化学镀液，其镀液中主盐、还原剂浓度一般维持在20~28g·dm~(-3)。化学镀镍在60℃开始施镀，在80~90℃镀液才能正常工作。当施镀次数超过三次后，沉积速度降至8.127μm·h~(-1)，硫酸镍浓度降至16.56g·dm~(-3)。需要补充主盐和还原剂才能进行正常的化学镀镍，镀液需要维护。
4.铝合金化学镀镍溶液中加入活化剂后，会使基体表面的氧化物溶解，露出更多铝合金基材，使其电极电势出现负移，适宜浓度(2～4g·dm~(-3))的活化剂可以加快化学诱发沉积镍的速度，实现6063铝合金在中温条件下直接化学镀镍，提高化学沉积的速度，改善镀层的综合性能。但过高浓度(>4g·dm~(-3))的活化剂会对镀层产生严重的腐蚀作用。
5.采用氨基乙酸为主配合剂，进行铝合金化学镀镍时，提高了镀速，获得了致密的化学镀镍层，其镀层的耐蚀性能明显改善，镀层在腐蚀介质中腐蚀电势提高，腐蚀电流降低，耐色变性也得到了明显的提高。化学镀镍的沉积速度随氨基乙酸质量浓度的增加而下降。活化剂浓度为2g·dm~(-3)，氨基乙酸浓度为8g·dm~(-3)时，能得到的综合性能良好的Ni P镀层。
Aluminum and magnesium alloys are widely uesd in many fields: military,automobile, aerospace, mechanical and electronic components, etc, because they havemany attrative properties, such as: low density, high intensity and easy to pressureprocessing, etc. However, aluminum and magnesium alloys have some commonshortcomings. Aluminum and magnesium alloys are intrinsically high reactive, andare easily oxidized to form oxidation film in the dry air. They have poor corrosionresistance and wearability, low hardness, which are actually one of the main obstaclesto the application of aluminum and magnesium alloys in practical environments.Electroless nickel plating is one of the effective surface modifications for aluminum,magnesium and its alloys. It not only improves the wear resistance and corrosionresistance, but also improve the hardness, wear resistance and electrical contactperformance. Electroless nickel plating has widely been applied in many industries.Ni-P coating exhibits all sort of new functions, such as magnetic property, lubricationperformance, etc. Therefore, the performances of electroless nickel plating coatingson AZ91D magnesium alloys obtained via different pretreatments have been studiedin this dissertation. We aim to develop an appropriate, environmental-friendlypretreatment technique for meeting the needs of industrial production. The interfacereaction mechanism of the environmental-friendly pretreatment was analyzed. Themain factors of electroless nickel plating were studied. At the same time, thedynamics equation of the acidic electroless plating on magnesium alloys was studied.In addition, the reaction mechanism and process of direct electroless nickel plating on6063aluminum alloy in temperature (70℃) were studied. The additive (fluoridecompound) was used and the main complexing agent was adjusted in the plating bathto improve the deposition rate of the electroless nickel plating. As far as aluminumand magnesium alloys are concerned, the main salts of electroless plating solutionsmostly focus attentions on basic nickel carbonate or nickel acetate, which result inhigh-cost, low-efficiency, instability of electroless plating solutions and littleapplications. There have important theoretic and practical signification of theelectroless plating on aluminum and magnesium alloys. Additionally, the platingmechanism and process are studied, by using low-cost, long-life NiSO_4·6H2O as themain salt.
In this dissertation, the electroless nickel plating on aluminum, and magnesiumalloys was studied in detail by means of weight method, Scanning ElectronMicroscope (SEM), X-ray Diffraction (XRD), Energy Dispersed X-ray spectrometer(EDX) Environmental Scanning Electron Microscope (ESEM) and electrochemistrymethods, etc. These measurement techniques were applied in the investigations ofpre-treatment process, the surface morphology and the cross section views of thecoatings, the analysis of the coating surface, the coating porosity and its evaluationmethod, the new electroless plating process，and so on.
Experimental results showed that:
1. Three different pre-treatments were studied, and the surface properties of thepretreated magnesium alloys were characterized by means of SEM, EDX andelectrochemical method. The results showed that the different degrees of corrosionwere produced on the surface of magnesium alloys. There had some deep cavities onthe surface and a coarse surface was all formed. The coarse surface can augment themechanical occlusive force between the coatings and the substrates. A compactfluoride film was formed on the surface of the specimen via (1) HNO_3+CrO_3pickling→HF activation or (2) HNO_3+H_3PO_4pickling→K_4P_2O_7activation→NH_4HF_2activation. The fluoride film can hinder the magnesium alloys from furtherdissolution. A zinc film was produced on the substrate via (3) HNO_3+CrO_3pickling→K_4P_2O_7activation→zinc immersion, which can also effectively protect themagnesium alloys from corrosion.
2. After the surfaces of magnesium alloys were pretreated via HNO_3+H_3PO_4pickling→K_4P_2O_7activation→NH_4HF_2activation. There was suitable F/O (1.2:1)on the substrate surface, which can provide appropriate active points, and effectivelyprotect the magnesium alloys from corrosion in the bath. The Ni-P coating had goodappearance, good corrosion resistance and excellent adhesion. The usage of the toxicsubstances in this pretreatment was avoided. Therefore, it was a chromium-free, lowfluoride and environmental-friendly pretreatment technology.
3. In the electroless plating acidic solutions using NiSO_4·6H2O as the main salt,both nickel salt and reducing agent were generally maintained between20~28g·dm~(-3).The temperature of electroless nickel plating was controlled to be80℃~90℃. Thedeposition rate was reduced to8.127μm·h-1and the concentration of nickel sulfatewas reduced to16.56g·dm~(-3)after more than twice platings. We need to supplenmentthe main salt and reducing agent arc needed in order to carry out normal electrolessnickel plating bath.
4. Appropriate concentrations of additive can accelerate the rate of chemicallyinduced nickel deposition, and realize direct electroless nickel plating on6063aluminum alloy in medium temperature (70℃). The additive can play important rolesin accelerating the deposition rate and improving the comprehensive performance ofcoatings.
5. Aminoacetic acid as a main complexing agent in the bath can controlreasonable plating rate of electroless nickel plating, and produce high quality coatingwith high corrosion resistance, good adhesion. The resistance of color degenerationalso got obvious improvement. When the additive was adjusted to2g·dm~(-3)and theaminoacetic was controlled to8g·dm~(-3), the Ni–P coating with better comprehensiveperformance was obtained.
引文
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