Ni-P-纳米SiO_2化学复合镀层制备及耐蚀和冷凝性能强化研究
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摘要
在化学镀液中加入纳米颗粒,通过与金属共沉积可获得纳米颗粒复合化学镀层。纳米颗粒的引入,会给镀层带来意想不到的优异的功能特性。本文在研究化学镀Ni-P工艺的基础上,将采用溶胶法制备的纳米Si02添加到化学镀液中得到纳米Si02颗粒复合化学镀层,并对复合镀层的生长机理、微观结构、晶化动力学及强化耐蚀和冷凝传热性能进行了系统研究,主要研究内容及创新成果如下：
(1).把Bockris方程用于化学镀Ni-P合金的沉积反应中,计算出热力学函数吸附自由能AGdepθ、熵变ΔSdepθ和焓变ΔHdepθ。ΔGdepθ<0,表明该反应是自发进行的；ΔHdepθ>0,说明反应是吸热的,这与化学镀要在一定温度条件下才能进行是吻合的。通过试验测定不同温度下的化学镀沉积速率,采用阿累尼乌斯方程作图,计算出Ni-P合金沉积反应的表观活化能Ea=35.36KJ/mol。通过实验和推算,得到了含复合络合剂在酸性条件下化学镀Ni-P合金的沉积速度的经验方程式：v=8.91·107·[Ni2+]0.81·[H2PO2-]0.20·[L1]0.70·[H+]-0.10·exp(-35360/RT)
(2).研究了纳米Si02颗粒的加入对化学镀层生长机理的影响,结果发现复合镀层的生长机制与化学镀有所不同,复合镀层是以纳米颗粒为中心的外延式生长,但没有影响Ni-P晶核的择优形核和胞状物沿横向生长扩展以及纵向生长增厚的形核长大方式,纳米颗粒的加入为基体表面提供了更多的活性形核点,使得复合镀层变得更加致密,没有出现化学镀Ni-P的胞状结构。
(3).根据非晶态合金晶化的动力学分析模型对Ni-P-SiO2复合镀层的晶化行为进行研究,推导出Ni-P镀层的晶化激活能是254.28kJ/mol, Ni-P-SiO2复合镀层的晶化激活能为222.30kJ/mol,这表明化学镀镍磷层中加入纳米Si02粒子会显著地降低镀层的晶化激活能。随着热处理温度升高,Ni-P镀层和Ni-P-SiO2复合镀层都会由非晶态转化为晶态,最终均转化为晶体Ni和Ni3P相。镀态的Ni-P-SiO2复合镀层的显微硬度值高于Ni-P镀层,晶化后镀层的显微硬度均会进一步提高,镀层在400℃热处理时显微硬度值达到最大值,Ni-P镀层的显微硬度最大值为Hv1001027,Ni-P-SiO2复合镀层的最大值为Hv1001118。
(4).研究了Ni-P-SiO2复合镀层分别在5%稀硫酸和3.5%NaCl溶液中的腐蚀行为,实验结果表明,纳米Si02颗粒的加入提高了化学镀Ni-P在硫酸和含C1-腐蚀环境中的腐蚀电位,促进了阳极的钝化行为,增加了腐蚀电化学反应的阻抗,从而强化了Ni-P镀层耐蚀性能。首次开展了纳米Si02颗粒复合化学镀技术抗硫酸露点腐蚀的实验研究,发现碳钢表面复合镀后的抗露点腐蚀性能提高了25倍,将复合镀技术应用到加热炉对流段炉管进行工业化应用考核,取得了良好的效果,证明了本文开发的复合镀技术有很重要的工程应用价值。
(5).首次研究了Ni-P-SiO2化学复合镀层的表面能,测得复合镀层的表面接触角达到110°,远高于化学镀层的74°和碳钢的40°,说明化学镀层降低了碳钢的表面能,而SiO2的引入则进一步降低了镀层的表面能。采用垂直平板冷凝实验装置研究了纳米Si02强化复合镀层表面水蒸汽冷凝传热特性。结果表明复合镀层由于表面能较低,实现了水蒸汽的滴状冷凝型态。与膜状冷凝传热相比,滴状冷凝传热系数比Nusselt计算值有大幅度提高,在相同过冷度下,复合镀层表面冷凝传热系数提高了3-5倍。
Electroless nickel-phosphorus(Ni-P) alloys reinforforced with nanoparticles are prepared by adding nanoparticles into plating bath. The incorporation of nanoparticles into Ni-P matrix can provide excellent functional properties. In this paper, Ni-P-SiO2 composite plating was developed by co-depositing nano-sized power SiO2 during electroless plating, and their growth mechanism, micro-structure, crystallization dynamics, enhanced corrosion resistance and condensation heat transfer characteristics were investigated systematically. The following are the main conclusions and innovation achievements:
(1). The values of△GdepΘ、△SdepΘand△HdepΘwere calculated by application of Bockris equation into the deposition reaction of Ni-P. The results showed that the process was spontaneous and endothermic, which was consistent with the reaction condition of electroless plating. After the effects of different plating parameters on the electroless Ni-P deposition were given through experiments, the plot of coating temperatures versus deposition rates was made according to Arrhennius equation. The surface activation energy calculated using the slope of the plot was 35.36 KJ/mol. In addition, the kinetic equation was presented as: v=9.91·107·[Ni2+]0.81·[H2PO2-]0.20·[L]10.70·[H+]-0.10·exp(-35360/RT).
(2). Nanoparticles codeposition played a major role in the growth of Ni-P matrix. Composite plating's growth model was epitaxial island with nanoparticles adsorbing on the substrate acted as nucleating centers, which didn't affect crystal's optimal nucleation and nodules's growth during electroless plating Ni-P alloys. During electroless composite plating, the deposition of nickel phosphor alloy would wrap the nano-particle. Numerous nucleating centers were helpful to decrease the dimension of nodules. This resulted in refinement in microstructure and disappearance of nodules in the deposit.
(3). Crystallization behavior of nano-sized SiO2 particles reinforced composite coatings were investigated according to the dynamical model of amorphous alloys. The activation energy of composite coating was calculated as 222.3 kJ/mol, while it was 254.28 kJ/mol for the Ni-P coating. It indicated that the SiO2 particles had an influence on the crystallization behaviors of composite coatings. The crystallization temperature was lowered due to the existence of SiO2 particles. After heat treatment, Ni-P and Ni-P-SiO2 coatings transformed to be the mixture of crystal nickel and Ni3P. Because of the existence of second phase particles, microhardness of the electroless Ni-P alloy enhanced with SiO2 particles greatly increased. After annealing at 400℃, microhardness value of Ni-P-SiO2 composite coatings approached as high as HV1001118, while it approached HV1001027 for electroless plating.
(4). The corrosion behavior of the composite coatings in 5%H2SO4 and 3.5%NaCl solutions had been investigated. The results showed that the incorporation of SiO2 nanoparticles into Ni-P matrixes increased the corrosion potential, surface resistance, greatly improved the corrosion resistance properties of the coatings. Dewpoint corrosion resistance property of the Ni-P-SiO2 composite plating was evaluated by the experiments. The results showed that the corrosion resistance of carbon steel is increased by 25 times after coated with composite platings. And composite plating was applied on the furnace tubes for industrial practice and the tubes succeeds in sustain dewpoint corrosion during two years'operation.
(5). In this paper, surface free energy of carbon steel, electroless Ni-P and Ni-P-SiO2 were investigated by measuring contact angles of water on the three surfaces. The contact angle of water on the composite plating is 110°, greatly higher than that of carbon steel (40°) and electroless plating (74°). The incorporation of nanoparticles into Ni-P matrixes reduces the total surface energy of the coating. Condensation heat transfer characteristics of steam on vertical plates with Ni-P and Ni-P-SiO2 platings were investigated experimentally and theoretically. Stable dropwise condensation was achived on composite platings for its low surface energy. Compared with film condensation, the heat transfer coefficient for the composite platings was improved 3-5 times at the same subcooling temperature.
(1).把Bockris方程用于化学镀Ni-P合金的沉积反应中,计算出热力学函数吸附自由能AGdepθ、熵变ΔSdepθ和焓变ΔHdepθ。ΔGdepθ<0,表明该反应是自发进行的；ΔHdepθ>0,说明反应是吸热的,这与化学镀要在一定温度条件下才能进行是吻合的。通过试验测定不同温度下的化学镀沉积速率,采用阿累尼乌斯方程作图,计算出Ni-P合金沉积反应的表观活化能Ea=35.36KJ/mol。通过实验和推算,得到了含复合络合剂在酸性条件下化学镀Ni-P合金的沉积速度的经验方程式：v=8.91·107·[Ni2+]0.81·[H2PO2-]0.20·[L1]0.70·[H+]-0.10·exp(-35360/RT)
(2).研究了纳米Si02颗粒的加入对化学镀层生长机理的影响,结果发现复合镀层的生长机制与化学镀有所不同,复合镀层是以纳米颗粒为中心的外延式生长,但没有影响Ni-P晶核的择优形核和胞状物沿横向生长扩展以及纵向生长增厚的形核长大方式,纳米颗粒的加入为基体表面提供了更多的活性形核点,使得复合镀层变得更加致密,没有出现化学镀Ni-P的胞状结构。
(3).根据非晶态合金晶化的动力学分析模型对Ni-P-SiO2复合镀层的晶化行为进行研究,推导出Ni-P镀层的晶化激活能是254.28kJ/mol, Ni-P-SiO2复合镀层的晶化激活能为222.30kJ/mol,这表明化学镀镍磷层中加入纳米Si02粒子会显著地降低镀层的晶化激活能。随着热处理温度升高,Ni-P镀层和Ni-P-SiO2复合镀层都会由非晶态转化为晶态,最终均转化为晶体Ni和Ni3P相。镀态的Ni-P-SiO2复合镀层的显微硬度值高于Ni-P镀层,晶化后镀层的显微硬度均会进一步提高,镀层在400℃热处理时显微硬度值达到最大值,Ni-P镀层的显微硬度最大值为Hv1001027,Ni-P-SiO2复合镀层的最大值为Hv1001118。
(4).研究了Ni-P-SiO2复合镀层分别在5%稀硫酸和3.5%NaCl溶液中的腐蚀行为,实验结果表明,纳米Si02颗粒的加入提高了化学镀Ni-P在硫酸和含C1-腐蚀环境中的腐蚀电位,促进了阳极的钝化行为,增加了腐蚀电化学反应的阻抗,从而强化了Ni-P镀层耐蚀性能。首次开展了纳米Si02颗粒复合化学镀技术抗硫酸露点腐蚀的实验研究,发现碳钢表面复合镀后的抗露点腐蚀性能提高了25倍,将复合镀技术应用到加热炉对流段炉管进行工业化应用考核,取得了良好的效果,证明了本文开发的复合镀技术有很重要的工程应用价值。
(5).首次研究了Ni-P-SiO2化学复合镀层的表面能,测得复合镀层的表面接触角达到110°,远高于化学镀层的74°和碳钢的40°,说明化学镀层降低了碳钢的表面能,而SiO2的引入则进一步降低了镀层的表面能。采用垂直平板冷凝实验装置研究了纳米Si02强化复合镀层表面水蒸汽冷凝传热特性。结果表明复合镀层由于表面能较低,实现了水蒸汽的滴状冷凝型态。与膜状冷凝传热相比,滴状冷凝传热系数比Nusselt计算值有大幅度提高,在相同过冷度下,复合镀层表面冷凝传热系数提高了3-5倍。
Electroless nickel-phosphorus(Ni-P) alloys reinforforced with nanoparticles are prepared by adding nanoparticles into plating bath. The incorporation of nanoparticles into Ni-P matrix can provide excellent functional properties. In this paper, Ni-P-SiO2 composite plating was developed by co-depositing nano-sized power SiO2 during electroless plating, and their growth mechanism, micro-structure, crystallization dynamics, enhanced corrosion resistance and condensation heat transfer characteristics were investigated systematically. The following are the main conclusions and innovation achievements:
(1). The values of△GdepΘ、△SdepΘand△HdepΘwere calculated by application of Bockris equation into the deposition reaction of Ni-P. The results showed that the process was spontaneous and endothermic, which was consistent with the reaction condition of electroless plating. After the effects of different plating parameters on the electroless Ni-P deposition were given through experiments, the plot of coating temperatures versus deposition rates was made according to Arrhennius equation. The surface activation energy calculated using the slope of the plot was 35.36 KJ/mol. In addition, the kinetic equation was presented as: v=9.91·107·[Ni2+]0.81·[H2PO2-]0.20·[L]10.70·[H+]-0.10·exp(-35360/RT).
(2). Nanoparticles codeposition played a major role in the growth of Ni-P matrix. Composite plating's growth model was epitaxial island with nanoparticles adsorbing on the substrate acted as nucleating centers, which didn't affect crystal's optimal nucleation and nodules's growth during electroless plating Ni-P alloys. During electroless composite plating, the deposition of nickel phosphor alloy would wrap the nano-particle. Numerous nucleating centers were helpful to decrease the dimension of nodules. This resulted in refinement in microstructure and disappearance of nodules in the deposit.
(3). Crystallization behavior of nano-sized SiO2 particles reinforced composite coatings were investigated according to the dynamical model of amorphous alloys. The activation energy of composite coating was calculated as 222.3 kJ/mol, while it was 254.28 kJ/mol for the Ni-P coating. It indicated that the SiO2 particles had an influence on the crystallization behaviors of composite coatings. The crystallization temperature was lowered due to the existence of SiO2 particles. After heat treatment, Ni-P and Ni-P-SiO2 coatings transformed to be the mixture of crystal nickel and Ni3P. Because of the existence of second phase particles, microhardness of the electroless Ni-P alloy enhanced with SiO2 particles greatly increased. After annealing at 400℃, microhardness value of Ni-P-SiO2 composite coatings approached as high as HV1001118, while it approached HV1001027 for electroless plating.
(4). The corrosion behavior of the composite coatings in 5%H2SO4 and 3.5%NaCl solutions had been investigated. The results showed that the incorporation of SiO2 nanoparticles into Ni-P matrixes increased the corrosion potential, surface resistance, greatly improved the corrosion resistance properties of the coatings. Dewpoint corrosion resistance property of the Ni-P-SiO2 composite plating was evaluated by the experiments. The results showed that the corrosion resistance of carbon steel is increased by 25 times after coated with composite platings. And composite plating was applied on the furnace tubes for industrial practice and the tubes succeeds in sustain dewpoint corrosion during two years'operation.
(5). In this paper, surface free energy of carbon steel, electroless Ni-P and Ni-P-SiO2 were investigated by measuring contact angles of water on the three surfaces. The contact angle of water on the composite plating is 110°, greatly higher than that of carbon steel (40°) and electroless plating (74°). The incorporation of nanoparticles into Ni-P matrixes reduces the total surface energy of the coating. Condensation heat transfer characteristics of steam on vertical plates with Ni-P and Ni-P-SiO2 platings were investigated experimentally and theoretically. Stable dropwise condensation was achived on composite platings for its low surface energy. Compared with film condensation, the heat transfer coefficient for the composite platings was improved 3-5 times at the same subcooling temperature.
引文
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