化学沉积镍基合金/纳米TiO_2复合镀层结构与性能研究
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摘要
纳米二氧化钛是一种光催化活性很高的半导体材料，具有很好的实用价值。人们采用各种方法，以提高光催化效果。纳米TiO_2悬浮体系存在纳米TiO_2难以分离与回收的问题，限制了其使用。采用化学沉积方法，用金属镀层包覆纳米TiO_2，可以实现对其固载。化学镀镍磷二元合金镀层具有优良的物理和化学性能，在工程上获得了广泛的应用。化学镀镍磷二元合金体系中加入第三组分，可以使镀层的性能得到很大的提高。在化学镀溶液中加入不溶性颗粒，使之产生共沉积而形成同时具有基质金属和固体微粒两类物质综合性能的复合镀层。由于纳米粒子具有特殊的物理和化学性能，将纳米量级的不溶微粒取代微米颗粒形成纳米复合镀层从而使化学镀层复合了纳米材料的特异功能,如提高硬度、耐磨性和耐蚀性。本文尝试采用电泳－化学沉积两步工艺，提高了复合镀层中纳米颗粒含量。
采用溶胶－凝胶方法成功制备了锌掺杂纳米TiO_2，光降解甲基橙溶液实验表明，掺杂浓度为0.8%时，经过500℃热处理后的Zn-TiO_2样品的光催化活性最高。对掺Zn量为0.8%的纳米TiO_2粉末进行渗氮处理，实验表明，Zn和N共掺杂的TiO_2的光催化性能最好，说明Zn与N有协同提高TiO_2光催化性能的作用。
镀液组分和操作条件对化学沉积Ni-Zn-P合金的沉积速度和镀层成分均有影响，随着镀液中硫酸锌含量提高，沉积速度下降，镀层中锌含量提高,磷含量下降；随着镀液中次亚磷酸钠含量提高，沉积速度提高，镀层中磷含量提高；随着镀液pH值提高，沉积速度提高，磷含量减少，锌含量提高；随着镀液温度提高，沉积速度提高。镀态下化学沉积Ni-Zn-P合金由非晶态的相和镍的固溶体存在。热处理至400℃时出现Ni_3P相而且已基本完全晶化，至600℃时出现Ni_5Zn_(12)相。在500℃时显微硬度达到最大值HV1210。冲蚀实验结果表明，在流动腐蚀介质中化学沉积Ni-Zn-P合金层质量损失随介质流动速度提高，冲击角度的减小而增加。
所获得化学沉积Ni-Sn-P沉积层为非晶态镍锡磷合金。随着镀液中四氯化锡和次亚磷酸钠含量的提高，沉积速度呈上升趋势，镀层中Sn的含量呈增加趋势，P的含量呈下降趋势；pH值在3-6范围内，随着镀液pH值增加，沉积速度成上升趋势；随着镀液温度的提高，沉积速度升高，镀层中磷含量呈下降趋势。冲蚀实验表明，随着冲蚀时间的延长，流体速度的提高，沉积层质量损失不断增加。在冲击角度为60°时，沉积层质量损失存在最大值。
通过在化学沉积Ni-Zn-P合金溶液中加入纳米TiO_2粒子，可以获得Ni-Zn-P-TiO_2复合镀层，最佳工艺条件下TiO_2的包覆量为10.76wt%。在相同状态下，化学沉积Ni-Zn-P-TiO_2纳米复合镀层的显微硬度值均高于化学镀Ni-Zn-P合金的硬度。经400℃1小时热处理，复合镀层具有最大的硬度值。化学沉积Ni-Zn-P-TiO_2纳米复合镀层经300℃热处理后质量损失最低，有最好的耐蚀性能。冲蚀实验结果表明，随着介质冲击角度减小，介质流速增加，镀层质量损失增加。在流动介质中化学沉积Ni-Zn-P-TiO_2纳米复合镀层的耐冲蚀性能优于化学沉积Ni-Zn-P合金镀层。
采用电泳沉积工艺获得纳米二氧化钛涂层，经随后进行的化学镀获得Ni-P/纳米TiO_2复合镀层。镀态下Ni-P/纳米TiO_2复合镀层是由结晶态和非晶态Ni-P合金及锐钛矿型纳米TiO_2组成的。在相同状态下，由于纳米颗粒的增强效应，复合镀层的显微硬度均高于镍磷合金镀层。由于纳米二氧化钛颗粒均匀的分布在镍磷化学镀层中，使Ni-P/纳米TiO_2复合镀层抗腐蚀性能大大加强。用甲基橙溶液进行的光催化反应表明，Ni-P/纳米TiO_2复合镀层具有较好的光催化效果。
Nano titanium dioxide is a kind of semi-conductor having good photo catalytic activity andpractical value. Various kinds of methods were employed to improve its photo catalytic activity. Itsapplication fields were restricted because of the difficulties of separating and recycling nano titaniumdioxide powders. Nano titanium dioxide particles can be loaded by electroless deposited coatings.Electroless plating Ni-P binary alloys have been achieved extensive application in industry, for thecoatings process excellent physical and chemical properties. Recent researches show that, byintroducing another constituent in the electroless deposited nickel-based binary alloys, the nickelbased ternary alloys can be obtained with the improved properties and performance. To add insolubleparticles in electroless plating bath and make them co-deposited with electroless deposited alloys, wecan obtain composite coatings which have excellent properties. As the nano-particles have quantumsize effect, small size effect, surface and interface effects, they have special physical and chemicalproperties. Nano composite coatings have specific functions such as hardenability, good wearresistance and good corrosion resistance. In this paper, Ni-P-nanometer TiO_2composite coatingswere prepared by electrophoretically deposite and electroless plating Ni-P alloy to improve thecontent of nano TiO_2particles in the coatings.
Zinc doped nano TiO_2particles were prepared by sol-gel method. The test of light degradatingmethyl orange showed that, the highest photo catalytic occurred when the concentration of zinc inTiO_2particle was0.8wt%and had been calcined at500℃.The TiO_2particles containing0.8wt%zinc were nitrided. The test of light degradating methyl orange showed that, the TiO_2particles dopedwith zinc and nitron have excellent photo catalytic property. This showed that zinc and nitron canimprove photo catalytic property of nano titanium dioxide simultaneously.
The composition and operating conditions have great effect on the deposition rate andconstituent of electroless deposited Ni-Zn-P alloys. With the bath content of ZnSO4increased, thedeposition rate and the content of P in the coating decreased. With the bath content of NaH2PO2increased, the deposition rate and the content of phosphorus in the coating increased. With pH valueand temperature of the bath increased, the deposition rate increased and the content of phosphorus inthe coating decreased. The electroless deposited Ni-Zn-P alloy is composed with amorphour phaseand solid solution of nickel. Ni_3P phase appears and the coating is crystallized completely when ithas been heated to400℃. The Ni_5Zn_(12)phase appears when it has been heated to600℃.The greatestmicrohardness value appears when it has been heated to500℃. The results of erosion test show that,the mass loss of electroless deposited Ni-Zn-P alloy increased with corrosive medium flow rateincreased and erosion angle decreased.
The results show that the electroless deposited Ni-Sn-P ternary alloy is amorphous. Thedeposition rate and the tin content in the coating increase, but the phosphorus content in the coatingdecreases with increasing the stannic chloride and sodium hypophosphite contents in the bath. Thedeposition rate increases with the pH value of the bath in the range of3to6. Mass loss of the coatingincreases with increasing the erosion time and the flow velocity of erosion solution, which has itsmaximum value as the coating impacted at an angle of60°.
Electroless deposited Ni-Zn-P-TiO_2nano-composite coatings were prepared by adding nanoTiO_2particles into electroless plating bath. The content of TiO_2in the composite coatings is10.76wt%at the optium technological conditions.The hardness values of electroless depositedNi-Zn-P-TiO_2nano-composite coatings are higher than that of electroless plating Ni-Zn-P alloy atthe same conditions. The composite coatings have the highest hardness value when they are heattreated at400℃for one hour. The results of erosion test show that, the mass loss of coatings areincreasing with corrosive medium flow rate increasing and erosion angle decreasing. Electrolessdeposited Ni-Zn-P-TiO_2nano-composite coatings have better anti errosion property than Ni-Zn-Palloy coatings.
The effect of the applied electric field strength, electric current and deposition durations onelectrophoretically depositing were studied. Suitable technological parameters of electroless platingNi-P solution were obtained.The microstructure of the composite coating was analyzed by XRD andSEM. The microhardness values of the composite coatings were tested.The methyl orange solutionwas used as the reactant to evaluate the photocatalytic activity of the catalyst samples. The resultsshow that, nanometer TiO_2particles are distributed uniformly in the composite coating. Themicrohardness values of the composite coatings are higher than that of Ni-P alloy coatings. Thecomposite coating processes better photocatalytic activity.
采用溶胶－凝胶方法成功制备了锌掺杂纳米TiO_2，光降解甲基橙溶液实验表明，掺杂浓度为0.8%时，经过500℃热处理后的Zn-TiO_2样品的光催化活性最高。对掺Zn量为0.8%的纳米TiO_2粉末进行渗氮处理，实验表明，Zn和N共掺杂的TiO_2的光催化性能最好，说明Zn与N有协同提高TiO_2光催化性能的作用。
镀液组分和操作条件对化学沉积Ni-Zn-P合金的沉积速度和镀层成分均有影响，随着镀液中硫酸锌含量提高，沉积速度下降，镀层中锌含量提高,磷含量下降；随着镀液中次亚磷酸钠含量提高，沉积速度提高，镀层中磷含量提高；随着镀液pH值提高，沉积速度提高，磷含量减少，锌含量提高；随着镀液温度提高，沉积速度提高。镀态下化学沉积Ni-Zn-P合金由非晶态的相和镍的固溶体存在。热处理至400℃时出现Ni_3P相而且已基本完全晶化，至600℃时出现Ni_5Zn_(12)相。在500℃时显微硬度达到最大值HV1210。冲蚀实验结果表明，在流动腐蚀介质中化学沉积Ni-Zn-P合金层质量损失随介质流动速度提高，冲击角度的减小而增加。
所获得化学沉积Ni-Sn-P沉积层为非晶态镍锡磷合金。随着镀液中四氯化锡和次亚磷酸钠含量的提高，沉积速度呈上升趋势，镀层中Sn的含量呈增加趋势，P的含量呈下降趋势；pH值在3-6范围内，随着镀液pH值增加，沉积速度成上升趋势；随着镀液温度的提高，沉积速度升高，镀层中磷含量呈下降趋势。冲蚀实验表明，随着冲蚀时间的延长，流体速度的提高，沉积层质量损失不断增加。在冲击角度为60°时，沉积层质量损失存在最大值。
通过在化学沉积Ni-Zn-P合金溶液中加入纳米TiO_2粒子，可以获得Ni-Zn-P-TiO_2复合镀层，最佳工艺条件下TiO_2的包覆量为10.76wt%。在相同状态下，化学沉积Ni-Zn-P-TiO_2纳米复合镀层的显微硬度值均高于化学镀Ni-Zn-P合金的硬度。经400℃1小时热处理，复合镀层具有最大的硬度值。化学沉积Ni-Zn-P-TiO_2纳米复合镀层经300℃热处理后质量损失最低，有最好的耐蚀性能。冲蚀实验结果表明，随着介质冲击角度减小，介质流速增加，镀层质量损失增加。在流动介质中化学沉积Ni-Zn-P-TiO_2纳米复合镀层的耐冲蚀性能优于化学沉积Ni-Zn-P合金镀层。
采用电泳沉积工艺获得纳米二氧化钛涂层，经随后进行的化学镀获得Ni-P/纳米TiO_2复合镀层。镀态下Ni-P/纳米TiO_2复合镀层是由结晶态和非晶态Ni-P合金及锐钛矿型纳米TiO_2组成的。在相同状态下，由于纳米颗粒的增强效应，复合镀层的显微硬度均高于镍磷合金镀层。由于纳米二氧化钛颗粒均匀的分布在镍磷化学镀层中，使Ni-P/纳米TiO_2复合镀层抗腐蚀性能大大加强。用甲基橙溶液进行的光催化反应表明，Ni-P/纳米TiO_2复合镀层具有较好的光催化效果。
Nano titanium dioxide is a kind of semi-conductor having good photo catalytic activity andpractical value. Various kinds of methods were employed to improve its photo catalytic activity. Itsapplication fields were restricted because of the difficulties of separating and recycling nano titaniumdioxide powders. Nano titanium dioxide particles can be loaded by electroless deposited coatings.Electroless plating Ni-P binary alloys have been achieved extensive application in industry, for thecoatings process excellent physical and chemical properties. Recent researches show that, byintroducing another constituent in the electroless deposited nickel-based binary alloys, the nickelbased ternary alloys can be obtained with the improved properties and performance. To add insolubleparticles in electroless plating bath and make them co-deposited with electroless deposited alloys, wecan obtain composite coatings which have excellent properties. As the nano-particles have quantumsize effect, small size effect, surface and interface effects, they have special physical and chemicalproperties. Nano composite coatings have specific functions such as hardenability, good wearresistance and good corrosion resistance. In this paper, Ni-P-nanometer TiO_2composite coatingswere prepared by electrophoretically deposite and electroless plating Ni-P alloy to improve thecontent of nano TiO_2particles in the coatings.
Zinc doped nano TiO_2particles were prepared by sol-gel method. The test of light degradatingmethyl orange showed that, the highest photo catalytic occurred when the concentration of zinc inTiO_2particle was0.8wt%and had been calcined at500℃.The TiO_2particles containing0.8wt%zinc were nitrided. The test of light degradating methyl orange showed that, the TiO_2particles dopedwith zinc and nitron have excellent photo catalytic property. This showed that zinc and nitron canimprove photo catalytic property of nano titanium dioxide simultaneously.
The composition and operating conditions have great effect on the deposition rate andconstituent of electroless deposited Ni-Zn-P alloys. With the bath content of ZnSO4increased, thedeposition rate and the content of P in the coating decreased. With the bath content of NaH2PO2increased, the deposition rate and the content of phosphorus in the coating increased. With pH valueand temperature of the bath increased, the deposition rate increased and the content of phosphorus inthe coating decreased. The electroless deposited Ni-Zn-P alloy is composed with amorphour phaseand solid solution of nickel. Ni_3P phase appears and the coating is crystallized completely when ithas been heated to400℃. The Ni_5Zn_(12)phase appears when it has been heated to600℃.The greatestmicrohardness value appears when it has been heated to500℃. The results of erosion test show that,the mass loss of electroless deposited Ni-Zn-P alloy increased with corrosive medium flow rateincreased and erosion angle decreased.
The results show that the electroless deposited Ni-Sn-P ternary alloy is amorphous. Thedeposition rate and the tin content in the coating increase, but the phosphorus content in the coatingdecreases with increasing the stannic chloride and sodium hypophosphite contents in the bath. Thedeposition rate increases with the pH value of the bath in the range of3to6. Mass loss of the coatingincreases with increasing the erosion time and the flow velocity of erosion solution, which has itsmaximum value as the coating impacted at an angle of60°.
Electroless deposited Ni-Zn-P-TiO_2nano-composite coatings were prepared by adding nanoTiO_2particles into electroless plating bath. The content of TiO_2in the composite coatings is10.76wt%at the optium technological conditions.The hardness values of electroless depositedNi-Zn-P-TiO_2nano-composite coatings are higher than that of electroless plating Ni-Zn-P alloy atthe same conditions. The composite coatings have the highest hardness value when they are heattreated at400℃for one hour. The results of erosion test show that, the mass loss of coatings areincreasing with corrosive medium flow rate increasing and erosion angle decreasing. Electrolessdeposited Ni-Zn-P-TiO_2nano-composite coatings have better anti errosion property than Ni-Zn-Palloy coatings.
The effect of the applied electric field strength, electric current and deposition durations onelectrophoretically depositing were studied. Suitable technological parameters of electroless platingNi-P solution were obtained.The microstructure of the composite coating was analyzed by XRD andSEM. The microhardness values of the composite coatings were tested.The methyl orange solutionwas used as the reactant to evaluate the photocatalytic activity of the catalyst samples. The resultsshow that, nanometer TiO_2particles are distributed uniformly in the composite coating. Themicrohardness values of the composite coatings are higher than that of Ni-P alloy coatings. Thecomposite coating processes better photocatalytic activity.
引文
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