镁合金表面有机涂层和化学镀层的研究
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摘要
本实验研究了镁合金的有机涂层和化学镀层的制备和涂层性能。本研究取得了以下有价值的研究成果:
1.锌系磷化膜具有微观多孔结构可使有机涂层嵌入其中。采用锌系磷化技术作为有机涂层的预处理技术可以确保镁合金和有机涂层之间具有良好的结合力。研究表明,有机涂层的性能与磷化膜中磷锌矿的结晶取向、耐蚀性和润湿性有关,复合磷化膜越致密、耐蚀性、耐酸碱腐蚀性和润湿性越好,则有机涂层的结合力和耐蚀性等性能就越好。
2.提出了适合镁合金的有机涂层工艺。分别采用“钼酸盐复合磷化膜+电泳漆+面涂层工艺”和“钼酸盐复合磷化膜+粉末喷涂工艺”,在镁合金上制备了两种有机涂层,对涂层的全面质量检验结果表明它们能够国标的要求。3.镁合金试样在化学镀镍前首先在铬酸和硝酸溶液中进行铬化处理,然后将其浸在氟化氢溶液中使其表面生成氟化镁保护膜,采用硫酸镍为主盐的镀液在AZ91D镁合金上直接化学镀Ni-P合金,镀层致密无孔,具有一定耐蚀性。
4.采用无铬的磷酸盐复合磷化膜对镁合金进行前处理,然后在硫酸盐中镀光亮镍磷合金。试验发现磷化液中的间硝基苯磺酸钠可使镁合金表面的微阴极区增加,使成膜速度加快,并使磷化膜的细致。在含有间硝基苯磺酸钠的磷化液中得到的磷化膜上可获得致密均匀,无孔隙的Ni-P镀层,Ni-P层表现出良好的结合力和耐腐蚀能力。
5.采用含有钼酸盐的磷化膜作为化学镀Ni-P的底层,磷化液中钼酸盐添加剂可使磷化膜上的单质锌含量增加。在AZ91D镁合金磷化膜上化学镀Ni-P涂层其表现出很好的性能。盐雾实验结果显示其抵抗腐蚀的时间长达150小时。Ni-P涂层表面硬度大约为670Hv,当其在180°C加热两小时后硬度增加到大约935Hv。
6.在镁合金上制备了Ni-P/Ni-W-P化学镀双层膜。镀层的极化曲线和盐
Magnesium alloy has low density, high strength-to-weight ratio and othergood physical and mechanical characteristics. However, the application ofmagnesium alloys has been limited due to their undesirable properties includingpoor corrosion and low wear resistance. Thus, the formation of anticorrosion andhigh wear-resistance coatings on the surface of Mg or Mg alloys is necessary inpractical applications. Since magnesium is one of the most electrochemicallyactive metal, ordinary coatings, such as nickel, copper and zinc coatings, can onlyprovide a physical barrier to corrosion attack of magnesium substrate. So, anycoatings on magnesium alloys should be as uniform, adherent and porosity free aspossible.
The preparing technologies, characteristics and anticorrosion mechanismshave been investigated in the paper. In the paper zinc phosphating process wereused to replace chromate treatment for the pretreatment of magnesium alloy.The relations among the characteristics of organic coating and themicrostructure, composition, phase structure and wettability of phosphate filmwere studied. It is shown that molybdate complex zinc phosphate film exhibits theoptimal anticorrosion characteristics and can be used as the base for electro-coatand powder coating of magnesium alloy.
The complex zinc phosphate film is also suitable to be the base film of theelectroless nickel deposit because there are nanocrystalline zinc particlesdispersed the phosphate film, which can provide the active particles for nickelnucleus. The anticorrosion characteristics of multilayer electroless deposit (Ni-P/Ni-W-P) are much better than single electroless nickel deposit.
In the present work, the technology of organic coating and the electrolessNi-P deposition on AZ91D magnesium alloy was proposed. Several contributionsshoald be mentioned in the follows1. Characteristics of organic coating of magnesium alloy are related with phasestructure, anticorrosion characteristics and wettability of phosphate films.The denser of the phosphate film and the more content of (311) phases ofhopeite, the better of the anticorrosion and acid resistance and alkaliresistance and wettability of phosphate films;and the better of the adhesionand resist corrosion of the organic coating on magnesium alloy.2. The anticorrosion performance of the organic coatings based thenon-chromate phosphate coating was proved better by the salt spray test andadhesion and appearance performance. A new environment-friendly surfacetreatment method for magnesium alloy parts was provided in the study. Thetechnology of “ molybdenum modified zinc phosphate coating+electro-coat+paint” and “molybdenum modified zinc phosphate coating+powder paintof magnesium alloy were developed. They can satisfy many kinds ofinternational and national quality standards.3. Direct electroless Ni plating of magnesium alloy was obtained from nickelsulfate plating for the first time. The magnesium alloy samples were etchedfirst in a solution of chromate and nitric acid and than soaked in HF solutionto form a conversion film before electroless nickel deposition. But chromiumcompounds are carcinogenic substance, which should abstain to use.4. The non-chromium zinc phosphate coating was used as pretreatment coatingof electroless Ni–P deposits obtained from the acid bath containing nickelsulphate for the first time. The microstructure of the phosphate coatings wasobserved by using SEM and the phase compositions were analyzed by theusing XRD. Chemical compositions in the phosphating coating wereZn3(PO4)2·4H2O and Zn. Metal zinc in the phosphating coating becomes thecatalytic particles for the nickel deposition. The addition of sodium
metanitrobenzene sulphonate greatly increased the micro cathode sites of thephosphate coating and made the coatings fine greatly. It was proved that theelectroless Ni–P deposits plus phosphating coating obtained from the bathcontaining sodium metanitrobenzene sulphonate exhibited good anticorrosionperformance.5. In this study, AZ91D magnesium alloy samples were pretreated in a zincphosphating bath to obtain a phosphate coating. Then, the electroless Ni-Pdeposition on the phosphate coating was undertaken by using the plating bathcontaining sulfate nickel. The phosphate coating on the AZ91D magnesiumalloy was obtained from the bath containing mainly phosphoric acid and zincoxide. There was zinc in the phosphate coatings and the addition of Na2MoO4in the phosphating bath resulted in the increase of zinc in the coating. Theexistence of metallic zinc in the phosphate coating makes it possible to be asthe pretreatment layer for further electroless Ni-P deposition. The Ni-Pcoatings with dense and fine microstructure were obtained on the phosphatecoatings on AZ91D alloy obtained from the phosphating bath with additionof 2.0~2.5g/L Na2MoO4.The Ni-P plus phosphate coatings on the AZ91Dmagnesium alloy exhibited good performance. Salt spray test showed thatthey could withstand about 150 hours without corrosion. The surfacehardness of the Ni-P coating is about 670Hv, and its hardness was increasedto about 915Hv through the heat treatment of 2 hours at temperature of180°C.6. An available method to obtain electrless Ni-P/Ni-W-P coatings on AZ91Dmagnesium alloy was discussed. The microstructure of the coating wasanalyzed by scanning electron microscope (SEM) and X-ray diffractmeter(XRD). The corrosion resistance of the coatings was estimated byelectrochemical polarization measurements and 10%HCl solutionimmergence test. The electrless Ni-P/Ni-W-P coatings can stand in 10%HClsolution for 170 minutes without corrosion. The hardness of the coating is
622HKV, and the coating has good adhesions. With the proof of theexperiment, this technique can offer reliable protection for AZ91Dmagnesium alloy.
1.锌系磷化膜具有微观多孔结构可使有机涂层嵌入其中。采用锌系磷化技术作为有机涂层的预处理技术可以确保镁合金和有机涂层之间具有良好的结合力。研究表明,有机涂层的性能与磷化膜中磷锌矿的结晶取向、耐蚀性和润湿性有关,复合磷化膜越致密、耐蚀性、耐酸碱腐蚀性和润湿性越好,则有机涂层的结合力和耐蚀性等性能就越好。
2.提出了适合镁合金的有机涂层工艺。分别采用“钼酸盐复合磷化膜+电泳漆+面涂层工艺”和“钼酸盐复合磷化膜+粉末喷涂工艺”,在镁合金上制备了两种有机涂层,对涂层的全面质量检验结果表明它们能够国标的要求。3.镁合金试样在化学镀镍前首先在铬酸和硝酸溶液中进行铬化处理,然后将其浸在氟化氢溶液中使其表面生成氟化镁保护膜,采用硫酸镍为主盐的镀液在AZ91D镁合金上直接化学镀Ni-P合金,镀层致密无孔,具有一定耐蚀性。
4.采用无铬的磷酸盐复合磷化膜对镁合金进行前处理,然后在硫酸盐中镀光亮镍磷合金。试验发现磷化液中的间硝基苯磺酸钠可使镁合金表面的微阴极区增加,使成膜速度加快,并使磷化膜的细致。在含有间硝基苯磺酸钠的磷化液中得到的磷化膜上可获得致密均匀,无孔隙的Ni-P镀层,Ni-P层表现出良好的结合力和耐腐蚀能力。
5.采用含有钼酸盐的磷化膜作为化学镀Ni-P的底层,磷化液中钼酸盐添加剂可使磷化膜上的单质锌含量增加。在AZ91D镁合金磷化膜上化学镀Ni-P涂层其表现出很好的性能。盐雾实验结果显示其抵抗腐蚀的时间长达150小时。Ni-P涂层表面硬度大约为670Hv,当其在180°C加热两小时后硬度增加到大约935Hv。
6.在镁合金上制备了Ni-P/Ni-W-P化学镀双层膜。镀层的极化曲线和盐
Magnesium alloy has low density, high strength-to-weight ratio and othergood physical and mechanical characteristics. However, the application ofmagnesium alloys has been limited due to their undesirable properties includingpoor corrosion and low wear resistance. Thus, the formation of anticorrosion andhigh wear-resistance coatings on the surface of Mg or Mg alloys is necessary inpractical applications. Since magnesium is one of the most electrochemicallyactive metal, ordinary coatings, such as nickel, copper and zinc coatings, can onlyprovide a physical barrier to corrosion attack of magnesium substrate. So, anycoatings on magnesium alloys should be as uniform, adherent and porosity free aspossible.
The preparing technologies, characteristics and anticorrosion mechanismshave been investigated in the paper. In the paper zinc phosphating process wereused to replace chromate treatment for the pretreatment of magnesium alloy.The relations among the characteristics of organic coating and themicrostructure, composition, phase structure and wettability of phosphate filmwere studied. It is shown that molybdate complex zinc phosphate film exhibits theoptimal anticorrosion characteristics and can be used as the base for electro-coatand powder coating of magnesium alloy.
The complex zinc phosphate film is also suitable to be the base film of theelectroless nickel deposit because there are nanocrystalline zinc particlesdispersed the phosphate film, which can provide the active particles for nickelnucleus. The anticorrosion characteristics of multilayer electroless deposit (Ni-P/Ni-W-P) are much better than single electroless nickel deposit.
In the present work, the technology of organic coating and the electrolessNi-P deposition on AZ91D magnesium alloy was proposed. Several contributionsshoald be mentioned in the follows1. Characteristics of organic coating of magnesium alloy are related with phasestructure, anticorrosion characteristics and wettability of phosphate films.The denser of the phosphate film and the more content of (311) phases ofhopeite, the better of the anticorrosion and acid resistance and alkaliresistance and wettability of phosphate films;and the better of the adhesionand resist corrosion of the organic coating on magnesium alloy.2. The anticorrosion performance of the organic coatings based thenon-chromate phosphate coating was proved better by the salt spray test andadhesion and appearance performance. A new environment-friendly surfacetreatment method for magnesium alloy parts was provided in the study. Thetechnology of “ molybdenum modified zinc phosphate coating+electro-coat+paint” and “molybdenum modified zinc phosphate coating+powder paintof magnesium alloy were developed. They can satisfy many kinds ofinternational and national quality standards.3. Direct electroless Ni plating of magnesium alloy was obtained from nickelsulfate plating for the first time. The magnesium alloy samples were etchedfirst in a solution of chromate and nitric acid and than soaked in HF solutionto form a conversion film before electroless nickel deposition. But chromiumcompounds are carcinogenic substance, which should abstain to use.4. The non-chromium zinc phosphate coating was used as pretreatment coatingof electroless Ni–P deposits obtained from the acid bath containing nickelsulphate for the first time. The microstructure of the phosphate coatings wasobserved by using SEM and the phase compositions were analyzed by theusing XRD. Chemical compositions in the phosphating coating wereZn3(PO4)2·4H2O and Zn. Metal zinc in the phosphating coating becomes thecatalytic particles for the nickel deposition. The addition of sodium
metanitrobenzene sulphonate greatly increased the micro cathode sites of thephosphate coating and made the coatings fine greatly. It was proved that theelectroless Ni–P deposits plus phosphating coating obtained from the bathcontaining sodium metanitrobenzene sulphonate exhibited good anticorrosionperformance.5. In this study, AZ91D magnesium alloy samples were pretreated in a zincphosphating bath to obtain a phosphate coating. Then, the electroless Ni-Pdeposition on the phosphate coating was undertaken by using the plating bathcontaining sulfate nickel. The phosphate coating on the AZ91D magnesiumalloy was obtained from the bath containing mainly phosphoric acid and zincoxide. There was zinc in the phosphate coatings and the addition of Na2MoO4in the phosphating bath resulted in the increase of zinc in the coating. Theexistence of metallic zinc in the phosphate coating makes it possible to be asthe pretreatment layer for further electroless Ni-P deposition. The Ni-Pcoatings with dense and fine microstructure were obtained on the phosphatecoatings on AZ91D alloy obtained from the phosphating bath with additionof 2.0~2.5g/L Na2MoO4.The Ni-P plus phosphate coatings on the AZ91Dmagnesium alloy exhibited good performance. Salt spray test showed thatthey could withstand about 150 hours without corrosion. The surfacehardness of the Ni-P coating is about 670Hv, and its hardness was increasedto about 915Hv through the heat treatment of 2 hours at temperature of180°C.6. An available method to obtain electrless Ni-P/Ni-W-P coatings on AZ91Dmagnesium alloy was discussed. The microstructure of the coating wasanalyzed by scanning electron microscope (SEM) and X-ray diffractmeter(XRD). The corrosion resistance of the coatings was estimated byelectrochemical polarization measurements and 10%HCl solutionimmergence test. The electrless Ni-P/Ni-W-P coatings can stand in 10%HClsolution for 170 minutes without corrosion. The hardness of the coating is
622HKV, and the coating has good adhesions. With the proof of theexperiment, this technique can offer reliable protection for AZ91Dmagnesium alloy.
引文
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