镁合金化学转化及化学转化膜上化学镀镍的研究
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摘要
目前,化学转化与化学镀镍技术都是镁合金表面处理研究的热点。本文在研究镁合金化学转化工艺的基础上,把两种工艺结合起来,成功地在AZ91D镁合金表面制备了具有良好耐蚀性、致密性的化学转化-化学镀镍复合涂层。
针对AZ91D镁合金开发了磷酸-高锰酸体系、钨酸-硅酸体系两类转化膜的制备方法。通过正交优化试验确定了两个转化液的配方。即磷酸-高锰酸体系:17.5g/L Na_2WO_4、4g/L Na_2SiO_3、0.5g/L KMnO_4、1g/L Na_2MoO_4;钨酸-硅酸体系:5g/L Na_3PO_4、15g/L NH_4H_2PO_4、1g/L KMnO_4、0.5g/L (NH_4)_6Mo_7O_(24)以及适量添加剂。由SEM可观察到转化膜的表面成“干枯河床”状。XRD分析表明,本实验中钨酸钠-硅酸钠体系转化膜的相成分主要为MgO、MgSiO_3、Mg_2SiO_4等化合物;磷酸–高锰酸盐体系转化膜的相成分主要为Mg、Al_(12)Mg_(17)和无定形相。处理液中存在的元素,在相应的膜层中基本都能找到其对应的氧化物或化合物。电化学测试表明,钨酸钠-硅酸钠体系转化膜较基体的腐蚀电位正移了0.45V;磷酸–高锰酸盐体系转化膜较基体的腐蚀电位正移了0.73V;同时自腐蚀电流降低了,两种转化膜均提高了镁合金的耐蚀性。
在化学转化膜上采用低浓度Sn2+敏化、离子Pd2+活化工艺对化学转化膜表面进行碱性化学镀镍的镀前预处理,获得了较好的效果。通过正交优化得到在转化膜上化学镀镍的最佳工艺为:30g/L硫酸镍、28g/L次磷酸钠、20 g/L柠檬酸钠、10 g/L氟化铵、0.4mg/L硫脲、pH 8.5–9.0、温度85℃。由SEM可观察到镀层的截面形貌,镀层与转化膜成紧密的“锯齿”状结合。XRD分析表明,镀层的相成分主要为Ni、Ni_5P_2、Ni_3P_2、MgO等。电化学测试表明,对转化膜进行化学镀镍之后,体系反应的是镀镍层的腐蚀信息。复合涂层的自腐蚀电位较基体提高了0.93V,极化曲线的钝化电位区间增加了,自腐蚀电流密度则升高了约一个数量级。表明化学镀镍对转化膜的封孔作用,进一步提高了镀层的耐蚀性。
The technologys of chemical conversion coating and electroless deposit nickel phosphorus alloy are the research hotspots of magnesium surface treatment at present. In this dissertation, based on the study of chemical conversion coating process, a smooth composite coating had been prepared on AZ91D magnesium alloy by chemical conversion coating and electroless depositing Ni-P alloy. The composite coating had very compact interior structure and high anti-corrosion capability, and it could provide more perfect protection for magnesium alloy from corroding.
Two new conversion coating system for the corrosion protection of die-casting AZ91D magnesium alloy were studied in this dissertation. One was composed of 17.5g/LNa_2WO_4,4g/LNa_2SiO_3,0.5g/L KMnO_4,1g/L Na_2MoO_4;the other was composed o f 5g/L Na_3PO_4,15g/L NH_4H_2PO_4,1g/L KMnO_4,0.5g/L (NH_4)_6Mo_7O_(24) and a little additive. The thickness,surface look,structure and the phase constitution of conversion film were studied by scan electron microscope(SEM) and X-ray diffraction(XRD).The results showed that the compositions of the conversion coating made by the first system were MgO,MgSiO_3,Mg_2SiO_4 and some other things. While the coating made by the second system were made up of Mg,Al_(12)Mg_(17) and some non-crystal structure.The elements in the solution could be found in the coating as their oxides or compounds.The researchs of dynamic potential polarization showed that the corrosion current potential of the coating got by the two system separately increase 0.45V and 0.75V.The corrosion resistance of the films got by the two system was all obviously improved and the self-corrosion current density decreased.
The low concentration Sn~(2+) sensitization and Pd~(2+) activation process were used to pretreat the chemical conversion coatings, then a crystal structure Ni-P coating could be prepared on it in alkaline electroless plating solution. The orthogonal test optimization experiments were applied to obtain a good alkaline electroless plating Ni-P alloy process,as follows: 30g/LNiSO_4·6H_2O,28g/LNa_H_2PO2·H_2O,10g/LNH_4F, 20g/LNa_2C_4H_6O_6·2H_2O,pH is 8.5-9.0,temperature is 85℃.The thickness,surface look,structure and the phase constitution of conversion film were studied by scan electron microscope(SEM) and X-ray diffraction(XRD). The results showed that the conversion coating was non-crystal structuer, and the composions were made up of Ni, Ni_5P_2, Ni_3P_2, MgO and eta.The study of electrochemistry test showed the system reflected the corrosion information of the nickelplate coating.The self-corrosion current potential of the composite plate increased 0.93V, and the deactivated electric potential sector of polarization curve increased, and the self-corrosion current density increased a order of magnitude. The sealed hole function of electroless deposit nickel phosphorus alloy, further enhanced the corrosion resistance of the coating.
针对AZ91D镁合金开发了磷酸-高锰酸体系、钨酸-硅酸体系两类转化膜的制备方法。通过正交优化试验确定了两个转化液的配方。即磷酸-高锰酸体系:17.5g/L Na_2WO_4、4g/L Na_2SiO_3、0.5g/L KMnO_4、1g/L Na_2MoO_4;钨酸-硅酸体系:5g/L Na_3PO_4、15g/L NH_4H_2PO_4、1g/L KMnO_4、0.5g/L (NH_4)_6Mo_7O_(24)以及适量添加剂。由SEM可观察到转化膜的表面成“干枯河床”状。XRD分析表明,本实验中钨酸钠-硅酸钠体系转化膜的相成分主要为MgO、MgSiO_3、Mg_2SiO_4等化合物;磷酸–高锰酸盐体系转化膜的相成分主要为Mg、Al_(12)Mg_(17)和无定形相。处理液中存在的元素,在相应的膜层中基本都能找到其对应的氧化物或化合物。电化学测试表明,钨酸钠-硅酸钠体系转化膜较基体的腐蚀电位正移了0.45V;磷酸–高锰酸盐体系转化膜较基体的腐蚀电位正移了0.73V;同时自腐蚀电流降低了,两种转化膜均提高了镁合金的耐蚀性。
在化学转化膜上采用低浓度Sn2+敏化、离子Pd2+活化工艺对化学转化膜表面进行碱性化学镀镍的镀前预处理,获得了较好的效果。通过正交优化得到在转化膜上化学镀镍的最佳工艺为:30g/L硫酸镍、28g/L次磷酸钠、20 g/L柠檬酸钠、10 g/L氟化铵、0.4mg/L硫脲、pH 8.5–9.0、温度85℃。由SEM可观察到镀层的截面形貌,镀层与转化膜成紧密的“锯齿”状结合。XRD分析表明,镀层的相成分主要为Ni、Ni_5P_2、Ni_3P_2、MgO等。电化学测试表明,对转化膜进行化学镀镍之后,体系反应的是镀镍层的腐蚀信息。复合涂层的自腐蚀电位较基体提高了0.93V,极化曲线的钝化电位区间增加了,自腐蚀电流密度则升高了约一个数量级。表明化学镀镍对转化膜的封孔作用,进一步提高了镀层的耐蚀性。
The technologys of chemical conversion coating and electroless deposit nickel phosphorus alloy are the research hotspots of magnesium surface treatment at present. In this dissertation, based on the study of chemical conversion coating process, a smooth composite coating had been prepared on AZ91D magnesium alloy by chemical conversion coating and electroless depositing Ni-P alloy. The composite coating had very compact interior structure and high anti-corrosion capability, and it could provide more perfect protection for magnesium alloy from corroding.
Two new conversion coating system for the corrosion protection of die-casting AZ91D magnesium alloy were studied in this dissertation. One was composed of 17.5g/LNa_2WO_4,4g/LNa_2SiO_3,0.5g/L KMnO_4,1g/L Na_2MoO_4;the other was composed o f 5g/L Na_3PO_4,15g/L NH_4H_2PO_4,1g/L KMnO_4,0.5g/L (NH_4)_6Mo_7O_(24) and a little additive. The thickness,surface look,structure and the phase constitution of conversion film were studied by scan electron microscope(SEM) and X-ray diffraction(XRD).The results showed that the compositions of the conversion coating made by the first system were MgO,MgSiO_3,Mg_2SiO_4 and some other things. While the coating made by the second system were made up of Mg,Al_(12)Mg_(17) and some non-crystal structure.The elements in the solution could be found in the coating as their oxides or compounds.The researchs of dynamic potential polarization showed that the corrosion current potential of the coating got by the two system separately increase 0.45V and 0.75V.The corrosion resistance of the films got by the two system was all obviously improved and the self-corrosion current density decreased.
The low concentration Sn~(2+) sensitization and Pd~(2+) activation process were used to pretreat the chemical conversion coatings, then a crystal structure Ni-P coating could be prepared on it in alkaline electroless plating solution. The orthogonal test optimization experiments were applied to obtain a good alkaline electroless plating Ni-P alloy process,as follows: 30g/LNiSO_4·6H_2O,28g/LNa_H_2PO2·H_2O,10g/LNH_4F, 20g/LNa_2C_4H_6O_6·2H_2O,pH is 8.5-9.0,temperature is 85℃.The thickness,surface look,structure and the phase constitution of conversion film were studied by scan electron microscope(SEM) and X-ray diffraction(XRD). The results showed that the conversion coating was non-crystal structuer, and the composions were made up of Ni, Ni_5P_2, Ni_3P_2, MgO and eta.The study of electrochemistry test showed the system reflected the corrosion information of the nickelplate coating.The self-corrosion current potential of the composite plate increased 0.93V, and the deactivated electric potential sector of polarization curve increased, and the self-corrosion current density increased a order of magnitude. The sealed hole function of electroless deposit nickel phosphorus alloy, further enhanced the corrosion resistance of the coating.
引文
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