电刷镀SiC/Ni-P复合镀层工艺及腐蚀性能研究
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摘要
电刷镀技术属于特种电镀技术，是电镀技术的新发展。由于该项技术具有操作设备简单、电流密度大、镀层沉积速度快、质量好、适应性强等优点，因此在表面工程中获得了广泛的应用。复合镀层是复合材料领域中一个新的研究方向，也是表面工程技术中较为活跃的研究热点之一。因此，采用电刷镀工艺制备复合镀层具有广阔的应用前景。
本文首先研究了制备Ni-P合金刷镀层的各项工艺参数，确定了镀液的组成，分析了影响刷镀层中P含量和镀层沉积速度的主要因素。在此基础之上，通过在镀液中加入SiC微粒和表面活性剂，并适当调整操作工艺参数，获得了SiC / Ni-P复合刷镀层。SiC微粒的粒径大小、含量及其分布是影响复合刷镀层质量的重要因素。通过金相显微镜和扫描电镜等方法观察了SiC / Ni-P复合刷镀层的显微组织和表面形貌，通过EDS、XRD等分析手段测定了复合刷镀层的成分和结构。试验结果表明：通过合理的镀液配方设计和操作工艺参数，可以获得基体镀层具有非晶态结构的、SiC微粒含量为17.8%(vol)且分布较为均匀的复合刷镀层。同时发现SiC / Ni-P复合刷镀层比Ni-P合金刷镀层表面更加平整、光滑，组织更加致密，镀层表面的微裂纹数量及其长度都明显减少，表明SiC微粒的加入能够使刷镀层的晶粒细化，并且显著降低了刷镀层的内应力。
30个周期的中性盐雾腐蚀试验结果表明，SiC / Ni-P复合镀层比Ni-P、Ni刷镀层具有更好的耐腐蚀性能。其原因可以归结为以下三个方面：首先，由于SiC微粒的加入减轻了镀层中微裂纹的倾向，提高了镀层的致密度；其次，随着作为腐蚀过程中阳极区域的微裂纹区面积的显著减少，阴极/阳极的面积比相应增大，整个腐蚀过程将由阳极过程所控制，高的阴极/阳极面积比所导致的阳极极化使腐蚀速度明显降低；再者，腐蚀产物以及SiC微粒在比较细小的微裂纹处的形成和聚集将更容易堵塞腐蚀介质进入到镀层内部的腐蚀通道，这也起到一定的保护作用。所有上述因素均使复合刷镀层的耐腐蚀性能有所提高。
当氧化温度在400℃~800℃之间时，复合刷镀层的抗高温氧化能力要优于Ni-P合金刷镀层；800℃、氧化100h的试验结果表明：Ni-P和SiC / Ni-P复合刷镀层的氧化动力学曲线基本呈抛物线型，显示氧化过程主要由扩散步骤控制着反
应速度。就相同试验时间的氧化增重量而言，SiC / Ni-P复合刷镀层具有较好的抗高温氧化性能，这可能是由于复合镀层中高耐热性的SiC微粒在高温氧化过程中对镀层表面形成的氧化产物存在着固定和附着的作用，使氧化产物不容易发生脱落，从而提高了复合镀层的抗高温氧化能力。另外，复合镀层的表面微裂纹等缺陷数量比较少，减少了镀层中氧的传输与扩散通道，这也会相应地提高复合刷镀层的抗高温氧化能力。
Brush plating is a kind of specific method and new development of electroplating technique. It requires some simple operating equipment and high current density, offers portability, suitability, high speed and quality deposites and coatings. Therefore, the kind of technique has been widespreadly applicated in Surface Engineering. Composite coatings is a new study orientation in the filed of composite materials, is also a study hotspot in Surface Engineering technique. Therefore, the application of composite coatings obtained by brush plating technique will be used widely.
In the paper, Ni-P alloy brush plating coatings were firstly obtained. The electrolyte composition and operating process parameters were analyzed and decided. Some main influence factors on P content and quality of Ni-P coatings were discussed. Based on these, SiC / Ni-P composite brush plating coatings were co-deposited by adding some SiC particle and surfactants into the Ni-P electrobath and rightly adjusting operating process parameters. The SiC particle size and its content and distribution state were some important factors for the quality of SiC / Ni-P composite coatings. The microstructure and surface morphology of SiC / Ni-P coatings were observed with metalloscope and SEM, its element composition and structure were investigated by EDS and XRD. These test results showed that SiC / Ni-P composite coatings with 17.8vol% and uniformity of SiC particle and amorphous structure of Ni-P alloy matrix could be prepared by appropriately modulating the solution composition and operating process parameters. Compared with the Ni-P coatings, the surface of SiC / Ni-P composite coatings was much leveler, much smoother and more homogeneous. The quantity and length of microscopic crack were evidently less than those of Ni-P alloy coatings. These results showed that SiC particle could make crystalline be refiner and reduce significantly the internal stress of SiC / Ni-P composite brush plating coatings.
The 30 period neutral salt spray corrosion test results showed that the corrosion resistance of SiC / Ni-P composite coatings was superior to that of Ni-P and Ni brush
plating coatings. There were several reasons as following for this. First, the trend of
microscopic crack was reduced when SiC particle was added into the Ni-P coatings, so the compactness of SiC / Ni-P composite brush plating coatings was improved; Second, during the corrosion course the microscopic crack area as corrosion anodic was reduced, correspondly the cathode/anodic area ratio would be augmented, thus the whole corrosion course was controlled by anodic process. The anodic polarization which was caused from large ratio of cathode/anodic area reduced markedly the corrosion velocity. Finally, Some corrosion products which formed and collected in the microscopic crack zone blocked the corrosion routeways by which corrosion medium could enter into the interior of SiC / Ni-P composite coatings. All factors above mentioned improved the corrosion resistance of SiC / Ni-P composite brush plating coatings.
When SiC / Ni-P and Ni-P brush plating coatings were oxidized from 400℃ to 800℃ for 2h, the experiment results showed that the oxidation resistance of composite coatings was superior to that of Ni-P coatings. When the two kinds of coatings were oxidized at 800℃ for 100h, the experiment results showed that their oxidation kinetics curves followed closely a parabolic oxidation law, indicating that the oxidation reaction was controlled by diffusion. During the same oxidation time as far as the weight change of oxidation product concerned, the results showed the SiC / Ni-P composite brush plating coatings had better oxidation resistance than Ni-P alloy coatings. The oxidation product might be fixed and adhesived by the SiC particle during the oxidation process. Therefore the oxidation product did not easily fall off and the oxidation resistance of SiC / Ni-P coatings were improved. In addition, the quantity of microscopic crack and other flaw on the surface of SiC / Ni-P c
本文首先研究了制备Ni-P合金刷镀层的各项工艺参数，确定了镀液的组成，分析了影响刷镀层中P含量和镀层沉积速度的主要因素。在此基础之上，通过在镀液中加入SiC微粒和表面活性剂，并适当调整操作工艺参数，获得了SiC / Ni-P复合刷镀层。SiC微粒的粒径大小、含量及其分布是影响复合刷镀层质量的重要因素。通过金相显微镜和扫描电镜等方法观察了SiC / Ni-P复合刷镀层的显微组织和表面形貌，通过EDS、XRD等分析手段测定了复合刷镀层的成分和结构。试验结果表明：通过合理的镀液配方设计和操作工艺参数，可以获得基体镀层具有非晶态结构的、SiC微粒含量为17.8%(vol)且分布较为均匀的复合刷镀层。同时发现SiC / Ni-P复合刷镀层比Ni-P合金刷镀层表面更加平整、光滑，组织更加致密，镀层表面的微裂纹数量及其长度都明显减少，表明SiC微粒的加入能够使刷镀层的晶粒细化，并且显著降低了刷镀层的内应力。
30个周期的中性盐雾腐蚀试验结果表明，SiC / Ni-P复合镀层比Ni-P、Ni刷镀层具有更好的耐腐蚀性能。其原因可以归结为以下三个方面：首先，由于SiC微粒的加入减轻了镀层中微裂纹的倾向，提高了镀层的致密度；其次，随着作为腐蚀过程中阳极区域的微裂纹区面积的显著减少，阴极/阳极的面积比相应增大，整个腐蚀过程将由阳极过程所控制，高的阴极/阳极面积比所导致的阳极极化使腐蚀速度明显降低；再者，腐蚀产物以及SiC微粒在比较细小的微裂纹处的形成和聚集将更容易堵塞腐蚀介质进入到镀层内部的腐蚀通道，这也起到一定的保护作用。所有上述因素均使复合刷镀层的耐腐蚀性能有所提高。
当氧化温度在400℃~800℃之间时，复合刷镀层的抗高温氧化能力要优于Ni-P合金刷镀层；800℃、氧化100h的试验结果表明：Ni-P和SiC / Ni-P复合刷镀层的氧化动力学曲线基本呈抛物线型，显示氧化过程主要由扩散步骤控制着反
应速度。就相同试验时间的氧化增重量而言，SiC / Ni-P复合刷镀层具有较好的抗高温氧化性能，这可能是由于复合镀层中高耐热性的SiC微粒在高温氧化过程中对镀层表面形成的氧化产物存在着固定和附着的作用，使氧化产物不容易发生脱落，从而提高了复合镀层的抗高温氧化能力。另外，复合镀层的表面微裂纹等缺陷数量比较少，减少了镀层中氧的传输与扩散通道，这也会相应地提高复合刷镀层的抗高温氧化能力。
Brush plating is a kind of specific method and new development of electroplating technique. It requires some simple operating equipment and high current density, offers portability, suitability, high speed and quality deposites and coatings. Therefore, the kind of technique has been widespreadly applicated in Surface Engineering. Composite coatings is a new study orientation in the filed of composite materials, is also a study hotspot in Surface Engineering technique. Therefore, the application of composite coatings obtained by brush plating technique will be used widely.
In the paper, Ni-P alloy brush plating coatings were firstly obtained. The electrolyte composition and operating process parameters were analyzed and decided. Some main influence factors on P content and quality of Ni-P coatings were discussed. Based on these, SiC / Ni-P composite brush plating coatings were co-deposited by adding some SiC particle and surfactants into the Ni-P electrobath and rightly adjusting operating process parameters. The SiC particle size and its content and distribution state were some important factors for the quality of SiC / Ni-P composite coatings. The microstructure and surface morphology of SiC / Ni-P coatings were observed with metalloscope and SEM, its element composition and structure were investigated by EDS and XRD. These test results showed that SiC / Ni-P composite coatings with 17.8vol% and uniformity of SiC particle and amorphous structure of Ni-P alloy matrix could be prepared by appropriately modulating the solution composition and operating process parameters. Compared with the Ni-P coatings, the surface of SiC / Ni-P composite coatings was much leveler, much smoother and more homogeneous. The quantity and length of microscopic crack were evidently less than those of Ni-P alloy coatings. These results showed that SiC particle could make crystalline be refiner and reduce significantly the internal stress of SiC / Ni-P composite brush plating coatings.
The 30 period neutral salt spray corrosion test results showed that the corrosion resistance of SiC / Ni-P composite coatings was superior to that of Ni-P and Ni brush
plating coatings. There were several reasons as following for this. First, the trend of
microscopic crack was reduced when SiC particle was added into the Ni-P coatings, so the compactness of SiC / Ni-P composite brush plating coatings was improved; Second, during the corrosion course the microscopic crack area as corrosion anodic was reduced, correspondly the cathode/anodic area ratio would be augmented, thus the whole corrosion course was controlled by anodic process. The anodic polarization which was caused from large ratio of cathode/anodic area reduced markedly the corrosion velocity. Finally, Some corrosion products which formed and collected in the microscopic crack zone blocked the corrosion routeways by which corrosion medium could enter into the interior of SiC / Ni-P composite coatings. All factors above mentioned improved the corrosion resistance of SiC / Ni-P composite brush plating coatings.
When SiC / Ni-P and Ni-P brush plating coatings were oxidized from 400℃ to 800℃ for 2h, the experiment results showed that the oxidation resistance of composite coatings was superior to that of Ni-P coatings. When the two kinds of coatings were oxidized at 800℃ for 100h, the experiment results showed that their oxidation kinetics curves followed closely a parabolic oxidation law, indicating that the oxidation reaction was controlled by diffusion. During the same oxidation time as far as the weight change of oxidation product concerned, the results showed the SiC / Ni-P composite brush plating coatings had better oxidation resistance than Ni-P alloy coatings. The oxidation product might be fixed and adhesived by the SiC particle during the oxidation process. Therefore the oxidation product did not easily fall off and the oxidation resistance of SiC / Ni-P coatings were improved. In addition, the quantity of microscopic crack and other flaw on the surface of SiC / Ni-P c
引文
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