三价铬镀铬惰性复合阳极材料的电沉积制备及电化学性能研究
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摘要
传统六价铬镀铬工艺因其具有高污染、高能耗等致命弱点,已逐步被三价铬镀铬工艺所取代。目前,三价铬镀铬工艺中通常使用的阳极是铅合金(如铅银合金等)材料,该类阳极存在耐蚀性差、催化活性低、析氧电位高,无法有效抑制六价铬导致镀液稳定性差等固有缺陷。近年,研究和开发能够抑制六价铬的产生、提高镀液稳定性、降低阳极析氧电位和降低能耗等方面有明显改善的新型三价铬镀铬阳极材料成为热点。
论文针对铅合金阳极的固有缺点,采用直流和脉冲复合电沉积的方法阳极氧化制备了三价铬镀铬用惰性复合阳极材料——不锈钢基/SnO2-Sb2O3/β-PbO2-CeO2-ZrO2。通过系列电化学方法的测量,系统研究了电极制备影响因素与其电化学性能的规律和作用机理；分析了电极材料的腐蚀行为和沉积过程,探讨了电极材料耐蚀性机理、复合电沉积机理；应用于硫酸盐体系三价铬镀铬工艺,考察了该电极材料在镀铬过程的综合性能,探究了惰性复合阳极在降低槽电压、抑制六价铬产生等方面的本质原因。主要完成工作及获得结论如下：
(1)不锈钢基/SnO2-Sb2O3/β-PbO2-CeO2-ZrO2复合电极材料的制备及性能研究
采用热分解法制备不锈钢基/SnO2-Sb2O3中间层,热分解温度500℃,热分解次数4次制备的SnO2-Sb2O3中间层结合力优良,耐蚀性、电催化活性和节能性良好。对β-PbO2-CeO2-ZrO2电极活性层的电化学性能与改性物质研究表明,Ce02具有细化晶粒和减少电极材料晶格缺陷的作用,Zr02能够细化晶粒和提高电极材料导电性,同时Zr02微粒产生的氧空穴能形成保护性氧化膜,分散剂具有的空间位阻效应使Ce02和Zr02均匀分散在镀液中形成稳定的胶体溶液,促进固体微粒的共沉积。镀液中改性物质CeO216g·L-1, ZrO230g·L-1,分散剂30mL·L-1时可以有效改善β-PbO2-CeO2-ZrO2电极材料的电化学性能和细化晶粒尺寸。直流工艺对β-PbO2-CeO2-ZrO2电极材料电化学性能的影响主要体现在适宜的施镀温度和搅拌速度能够增大固体微粒的动能,促进微粒向阳极表面迁移和吸附,合适的电流密度使金属氧化物有效包覆纳米颗粒形成具有一定厚度的致密、平整镀层,由此得到电流密度20mA cm-2,温度80℃,搅拌速度350r·min-1可以有效促进β-PbO2-CeO2-Zr02电极材料的沉积过程,提高电极材料性能。对不同脉冲工艺制备的β-PbO2-CeO2-Zr02电极材料的电化学性能研究表明,适宜的脉冲平均电流密度、占空比和脉冲工作时间可以有效促进晶核的形成,抑制晶粒的快速长大,消除阳极附近的浓差极化,由此确定脉冲平均电流密度0.3A·cm-2,占空比30%,脉冲工作时间100ms。
结合表面形貌和电化学性能分析可知；制备的不锈钢基/SnO2-Sb2O3/β-PbO2-CeO2-ZrO2复合电极材料晶粒细致,结构致密均匀,具有良好的耐蚀性和节能性,催化活性高且微观活性分布均匀,可显著提升电极材料的性能。相比于直流技术,采用脉冲技术制备的电极材料表面颗粒排列更平整有序、孔隙率更低,在耐腐蚀性和节能性方面都有明显改善。通过交流阻抗图谱对复合电极材料腐蚀过程分析确定：复合电极材料的腐蚀过程都存在弥散效应；不同分散剂浓度、电流密度、温度、搅拌速度、脉冲平均电流密度、占空比和脉冲工作时间制备的电极材料的腐蚀过程主要由电荷转移步骤控制；不同Ce02和ZrO2浓度制备的电极材料的腐蚀过程前期由电荷转移步骤控制,后期由扩散步骤控制。通过扫描电化学显微镜测试结合扫描电镜和能谱分析可知：最佳工艺条件制备可以有效促进复合电极材料中的纳米颗粒含量,使电极表面形貌细化和平整均匀,电极的电催化活性和活性分布均一性显著提升。
(2)惰性复合电极材料沉积机理探讨
采用循环伏安曲线考察复合电极材料的沉积过程,确定沉积机理为：Pb2+与羟基自由基生成中间产物Pb(OHads)2+后逐渐转变为Pb02,中间产物向Pb02转变的过程为决速步骤；改性添加物能促进β-PbO2-CeO2-ZrO2的晶粒形核,延缓晶粒长大,使晶粒尺寸更加细小,镀液中CeO216g·L-1, ZrO230g·L-1,分散剂50mL·L-1时最有利于β-PbO2-CeO2-Zr02的沉积；β-PbO2-CeO2-ZrO2的生成反应是稳定、不可逆的过程。
(3)三价铬镀铬阳极性能研究
采用电化学方法研究表明,较之β-PbO2和Pb-Ag(0.75)合金电极,β-PbO2-CeO2-ZrO2复合电极表现出更为优异的耐腐蚀性和节能性；Ce02和Zr02的加入改变了Pb02结晶的生长取向,改善了镀层的组织结构和晶粒尺寸。对电极材料在三价铬镀铬过程的综合性能考察发现,β-PbO2-CeO2-ZrO2复合电极材料能够有效降低槽电压,提高耐腐蚀,抑制六价铬的生成。当ZrO2浓度为30g·L-1时,制备的电极材料中Zr含量高,氧气优先析出,可降低和稳定槽电压,有效抑制镀液中的六价铬浓度,保证镀铬过程的节能和镀液的稳定性。
For heavy pollution, high energy consumption and other important drawbacks, conventional hexavalent chromium plating has been replaced by trivalent chromium plating gradually. Currently, lead-based alloys (e.g. lead-silver alloy or the like) as anode materials are widely used in trivalent chromium plating. However, lead-based alloys have many inherent defects, such as poor corrosion resistance, low catalytic activity, high oxygen evolution potential and ineffective in restraining poor stability of plating bath caused by hexavalent chromium. In recent years, the research and development of new trivalent chromium plating anode materials that can improve the stability of plating bath, inhibit the formation of hexavalent chromium, decrease oxygen evolution overpotential of anode and energy consumption significantly have become one of the hottest issue.
Aiming at eliminating inherent defects of lead-based alloys, stainless steel-based/SnO2-Sb2O3/β-PbO2-CeO2-ZrO2inert composite electrode materials used for trivalent chromium plating were prepared by direct-current and pulse-current composite electrodeposition methods with anodic oxidation. Through a series of electrochemical measurement, the laws and action mechanism between influence factors of electrode preparation and its electrochemical properties were studied systematically; analyzing corrosion behavior and deposition process; exploring the mechanism of corrosion resistance and composite electrodeposition of the electrode. The comprehensive performance of the new anode materials were investigated while they were applied to trivalent chromium plating in sulfate bath. The essential reason of inert composite anode in reducing cell voltage and restraining the formation of hexavalent chromium were explored. The mainly work and conclusions are as follows:
(1) Preparation and performance study of stainless steel-based/SnO2-Sb2O3/β-PbO2-CeO2-ZrO2composite materials
The process conditions for preparing SnO2-Sb2O3intermediate with thermal decomposition method:thermal decomposition temperature is500℃, thermal decomposition number is4times. The bonding force, corrosion resistance, electrocatalytic activity and energy conservation of SnO2-Sb2O3intermediate are improved significantly. The studies on electrochemical properties of β-PbO2-CeO2-ZrO2coating under different concentration of modified substances showed that:CeO2particles can refine grains and reduce lattice defects of electrode materials; ZrO2particles can refine grains and increase electrical conductivity of electrode material; meanwhile, oxygen vacancies produced by ZrO2particles can form protective oxidation film; the dispersant agent with steric-hinerance effect accelerate dispersion of CeO2and ZrO2uniformly forming a stable colloidal solution and promoting co-deposition of solid particles. When the modified substances of CeO2,ZrO2and dispersant agent concentration is16g·L-1,30g·L-1,30mL·L-1respectively, the electrochemical properties of β-PbO2-CeO2-ZrO2electrode is improved effectively and its grain size is refined. The influence of direct-current(DC) process on electrochemical properties of β-PbO2-CeO2-ZrO2electrode are mainly reflected in three aspects: appropriate plating temperature and stirring rate can increase kinetic energy of solid particles that promoting the particles to migrate and adsorb on anode surface; appropriate current density can accelerate metal oxide to coat nano-particles effectively forming a compact and smooth coating with a certain thickness. It follows that the optimum conditions for preparing β-PbO2-CeO2-ZrO2electrode materials by DC electrodeposition:current density is20mA·cm-2, temperature is80℃, stirring rate is350r·min-1. The researches on electrochemical properties of P-PbO2-CeO2-ZrO2electrode materials prepared under different pulse conditions showed that appropriate pulse average current density, duty cycle and pulse work time can promote the formation of crystal nucleus effectively, prevent the grains growing excessively and eliminate concentration polarization around the anode. Thereby the optimum conditions for preparing β-PbO2-CeO2-ZrO2electrode materials by pulse electrodeposition:pulse average current density is0.3A-cm-2, duty cycle is30%, pulse work time is100ms.
Combined with the surface morphology and electrochemical performance analysis, it is obvious that the stainless steel-based/SnO2-Sb2O3/β-PbO2-CeO2-ZrO2materials have many advantages, such as grain refinement, compact and uniform structure, excellent corrosion resistance and energy conservation, high catalytic activity and even distribution of the micro activity, which can improve comprehensive properties of electrode materials significantly. Compared to direct-current technology, the electrode prepared by pulse technology with lower porosity, better corrosion resistance and energy saving is more smooth and orderly arrangement of surface particles. Through AC impedance spectroscopy analysis of corrosion process of composite electrode, it showed that:dispersion effect was existed in corrosion process of composite electrode; the corrosion process of composite electrode prepared under different concentration of dispersant agent, current density, temperature, stirring rate, pulse average current density, duty cycle and pulse work time was mainly controlled by charge transfer; However, that of electrode prepared under different concentration of CeO2and ZrO2was controlled by charge transfer in early stage, the late stage was controlled by diffusion step. Combining scanning electrochemistry microscope (SECM) with SEM and energy spectrum testing showed that:the composite electrode materials prepared under optimum conditions contained more nanometer particles, the surface morphology of them were level and electrocatalatic activity and its uniformity distribution were improved.
(2) Investigating of deposition mechanism of inert composite electrode
By analyzing CV curves, the deposition process of composite electrode was investigated. The deposition mechanism is proposed:Pb2+and hydroxyl radicals formed intermediate product Pb(OHads)2+and then it transformed into PbO2. The process of intermediate product Pb(OHads)2+transformed into PbO2was rate-determining step. The modified substances can accelerate grain nucleation, delay grain growth and refine grain size. It is favorable toward promoting co-deposition of β-PbO2-CeO2-ZrO2when plating bath component:CeO2concentration is16g·L-1, ZrO2concentration is30g·L-1and dispersant agent concentration is50mL·L-1. The formation reaction of β-PbO2-CeO2-ZrO2was steady and irreversible process.
(3) The study of anode properties for trivalent chromium plating
Through electrochemical studies, it is easy to conclude that the p-PbO2-CeO2-ZrO2composite electrode showed excellent corrosion resistance and energy conservation compared to P-PbO2and Pb-Ag alloy. The addition of CeO2and ZrO2changed growth orientation of PbO2grains and improved texture structure and grain size of coating. Through the comprehensive performance investigation of electrode in trivalent chromium plating, it was found that β-PbO2-CeO2-ZrO2composite electrode can effectively reduce cell voltage, improve corrosion resistance and inhibit formation of hexavalent chromium. When the concentration of ZrO2is30g·L-1in bath, the Zr concentration in prepared electrode materials is high, which can reduce and stabilize cell voltage, reduce hexavalent chromium concentration effectively and ensure energy conservation and the stability of plating bath.
论文针对铅合金阳极的固有缺点,采用直流和脉冲复合电沉积的方法阳极氧化制备了三价铬镀铬用惰性复合阳极材料——不锈钢基/SnO2-Sb2O3/β-PbO2-CeO2-ZrO2。通过系列电化学方法的测量,系统研究了电极制备影响因素与其电化学性能的规律和作用机理；分析了电极材料的腐蚀行为和沉积过程,探讨了电极材料耐蚀性机理、复合电沉积机理；应用于硫酸盐体系三价铬镀铬工艺,考察了该电极材料在镀铬过程的综合性能,探究了惰性复合阳极在降低槽电压、抑制六价铬产生等方面的本质原因。主要完成工作及获得结论如下：
(1)不锈钢基/SnO2-Sb2O3/β-PbO2-CeO2-ZrO2复合电极材料的制备及性能研究
采用热分解法制备不锈钢基/SnO2-Sb2O3中间层,热分解温度500℃,热分解次数4次制备的SnO2-Sb2O3中间层结合力优良,耐蚀性、电催化活性和节能性良好。对β-PbO2-CeO2-ZrO2电极活性层的电化学性能与改性物质研究表明,Ce02具有细化晶粒和减少电极材料晶格缺陷的作用,Zr02能够细化晶粒和提高电极材料导电性,同时Zr02微粒产生的氧空穴能形成保护性氧化膜,分散剂具有的空间位阻效应使Ce02和Zr02均匀分散在镀液中形成稳定的胶体溶液,促进固体微粒的共沉积。镀液中改性物质CeO216g·L-1, ZrO230g·L-1,分散剂30mL·L-1时可以有效改善β-PbO2-CeO2-ZrO2电极材料的电化学性能和细化晶粒尺寸。直流工艺对β-PbO2-CeO2-ZrO2电极材料电化学性能的影响主要体现在适宜的施镀温度和搅拌速度能够增大固体微粒的动能,促进微粒向阳极表面迁移和吸附,合适的电流密度使金属氧化物有效包覆纳米颗粒形成具有一定厚度的致密、平整镀层,由此得到电流密度20mA cm-2,温度80℃,搅拌速度350r·min-1可以有效促进β-PbO2-CeO2-Zr02电极材料的沉积过程,提高电极材料性能。对不同脉冲工艺制备的β-PbO2-CeO2-Zr02电极材料的电化学性能研究表明,适宜的脉冲平均电流密度、占空比和脉冲工作时间可以有效促进晶核的形成,抑制晶粒的快速长大,消除阳极附近的浓差极化,由此确定脉冲平均电流密度0.3A·cm-2,占空比30%,脉冲工作时间100ms。
结合表面形貌和电化学性能分析可知；制备的不锈钢基/SnO2-Sb2O3/β-PbO2-CeO2-ZrO2复合电极材料晶粒细致,结构致密均匀,具有良好的耐蚀性和节能性,催化活性高且微观活性分布均匀,可显著提升电极材料的性能。相比于直流技术,采用脉冲技术制备的电极材料表面颗粒排列更平整有序、孔隙率更低,在耐腐蚀性和节能性方面都有明显改善。通过交流阻抗图谱对复合电极材料腐蚀过程分析确定：复合电极材料的腐蚀过程都存在弥散效应；不同分散剂浓度、电流密度、温度、搅拌速度、脉冲平均电流密度、占空比和脉冲工作时间制备的电极材料的腐蚀过程主要由电荷转移步骤控制；不同Ce02和ZrO2浓度制备的电极材料的腐蚀过程前期由电荷转移步骤控制,后期由扩散步骤控制。通过扫描电化学显微镜测试结合扫描电镜和能谱分析可知：最佳工艺条件制备可以有效促进复合电极材料中的纳米颗粒含量,使电极表面形貌细化和平整均匀,电极的电催化活性和活性分布均一性显著提升。
(2)惰性复合电极材料沉积机理探讨
采用循环伏安曲线考察复合电极材料的沉积过程,确定沉积机理为：Pb2+与羟基自由基生成中间产物Pb(OHads)2+后逐渐转变为Pb02,中间产物向Pb02转变的过程为决速步骤；改性添加物能促进β-PbO2-CeO2-ZrO2的晶粒形核,延缓晶粒长大,使晶粒尺寸更加细小,镀液中CeO216g·L-1, ZrO230g·L-1,分散剂50mL·L-1时最有利于β-PbO2-CeO2-Zr02的沉积；β-PbO2-CeO2-ZrO2的生成反应是稳定、不可逆的过程。
(3)三价铬镀铬阳极性能研究
采用电化学方法研究表明,较之β-PbO2和Pb-Ag(0.75)合金电极,β-PbO2-CeO2-ZrO2复合电极表现出更为优异的耐腐蚀性和节能性；Ce02和Zr02的加入改变了Pb02结晶的生长取向,改善了镀层的组织结构和晶粒尺寸。对电极材料在三价铬镀铬过程的综合性能考察发现,β-PbO2-CeO2-ZrO2复合电极材料能够有效降低槽电压,提高耐腐蚀,抑制六价铬的生成。当ZrO2浓度为30g·L-1时,制备的电极材料中Zr含量高,氧气优先析出,可降低和稳定槽电压,有效抑制镀液中的六价铬浓度,保证镀铬过程的节能和镀液的稳定性。
For heavy pollution, high energy consumption and other important drawbacks, conventional hexavalent chromium plating has been replaced by trivalent chromium plating gradually. Currently, lead-based alloys (e.g. lead-silver alloy or the like) as anode materials are widely used in trivalent chromium plating. However, lead-based alloys have many inherent defects, such as poor corrosion resistance, low catalytic activity, high oxygen evolution potential and ineffective in restraining poor stability of plating bath caused by hexavalent chromium. In recent years, the research and development of new trivalent chromium plating anode materials that can improve the stability of plating bath, inhibit the formation of hexavalent chromium, decrease oxygen evolution overpotential of anode and energy consumption significantly have become one of the hottest issue.
Aiming at eliminating inherent defects of lead-based alloys, stainless steel-based/SnO2-Sb2O3/β-PbO2-CeO2-ZrO2inert composite electrode materials used for trivalent chromium plating were prepared by direct-current and pulse-current composite electrodeposition methods with anodic oxidation. Through a series of electrochemical measurement, the laws and action mechanism between influence factors of electrode preparation and its electrochemical properties were studied systematically; analyzing corrosion behavior and deposition process; exploring the mechanism of corrosion resistance and composite electrodeposition of the electrode. The comprehensive performance of the new anode materials were investigated while they were applied to trivalent chromium plating in sulfate bath. The essential reason of inert composite anode in reducing cell voltage and restraining the formation of hexavalent chromium were explored. The mainly work and conclusions are as follows:
(1) Preparation and performance study of stainless steel-based/SnO2-Sb2O3/β-PbO2-CeO2-ZrO2composite materials
The process conditions for preparing SnO2-Sb2O3intermediate with thermal decomposition method:thermal decomposition temperature is500℃, thermal decomposition number is4times. The bonding force, corrosion resistance, electrocatalytic activity and energy conservation of SnO2-Sb2O3intermediate are improved significantly. The studies on electrochemical properties of β-PbO2-CeO2-ZrO2coating under different concentration of modified substances showed that:CeO2particles can refine grains and reduce lattice defects of electrode materials; ZrO2particles can refine grains and increase electrical conductivity of electrode material; meanwhile, oxygen vacancies produced by ZrO2particles can form protective oxidation film; the dispersant agent with steric-hinerance effect accelerate dispersion of CeO2and ZrO2uniformly forming a stable colloidal solution and promoting co-deposition of solid particles. When the modified substances of CeO2,ZrO2and dispersant agent concentration is16g·L-1,30g·L-1,30mL·L-1respectively, the electrochemical properties of β-PbO2-CeO2-ZrO2electrode is improved effectively and its grain size is refined. The influence of direct-current(DC) process on electrochemical properties of β-PbO2-CeO2-ZrO2electrode are mainly reflected in three aspects: appropriate plating temperature and stirring rate can increase kinetic energy of solid particles that promoting the particles to migrate and adsorb on anode surface; appropriate current density can accelerate metal oxide to coat nano-particles effectively forming a compact and smooth coating with a certain thickness. It follows that the optimum conditions for preparing β-PbO2-CeO2-ZrO2electrode materials by DC electrodeposition:current density is20mA·cm-2, temperature is80℃, stirring rate is350r·min-1. The researches on electrochemical properties of P-PbO2-CeO2-ZrO2electrode materials prepared under different pulse conditions showed that appropriate pulse average current density, duty cycle and pulse work time can promote the formation of crystal nucleus effectively, prevent the grains growing excessively and eliminate concentration polarization around the anode. Thereby the optimum conditions for preparing β-PbO2-CeO2-ZrO2electrode materials by pulse electrodeposition:pulse average current density is0.3A-cm-2, duty cycle is30%, pulse work time is100ms.
Combined with the surface morphology and electrochemical performance analysis, it is obvious that the stainless steel-based/SnO2-Sb2O3/β-PbO2-CeO2-ZrO2materials have many advantages, such as grain refinement, compact and uniform structure, excellent corrosion resistance and energy conservation, high catalytic activity and even distribution of the micro activity, which can improve comprehensive properties of electrode materials significantly. Compared to direct-current technology, the electrode prepared by pulse technology with lower porosity, better corrosion resistance and energy saving is more smooth and orderly arrangement of surface particles. Through AC impedance spectroscopy analysis of corrosion process of composite electrode, it showed that:dispersion effect was existed in corrosion process of composite electrode; the corrosion process of composite electrode prepared under different concentration of dispersant agent, current density, temperature, stirring rate, pulse average current density, duty cycle and pulse work time was mainly controlled by charge transfer; However, that of electrode prepared under different concentration of CeO2and ZrO2was controlled by charge transfer in early stage, the late stage was controlled by diffusion step. Combining scanning electrochemistry microscope (SECM) with SEM and energy spectrum testing showed that:the composite electrode materials prepared under optimum conditions contained more nanometer particles, the surface morphology of them were level and electrocatalatic activity and its uniformity distribution were improved.
(2) Investigating of deposition mechanism of inert composite electrode
By analyzing CV curves, the deposition process of composite electrode was investigated. The deposition mechanism is proposed:Pb2+and hydroxyl radicals formed intermediate product Pb(OHads)2+and then it transformed into PbO2. The process of intermediate product Pb(OHads)2+transformed into PbO2was rate-determining step. The modified substances can accelerate grain nucleation, delay grain growth and refine grain size. It is favorable toward promoting co-deposition of β-PbO2-CeO2-ZrO2when plating bath component:CeO2concentration is16g·L-1, ZrO2concentration is30g·L-1and dispersant agent concentration is50mL·L-1. The formation reaction of β-PbO2-CeO2-ZrO2was steady and irreversible process.
(3) The study of anode properties for trivalent chromium plating
Through electrochemical studies, it is easy to conclude that the p-PbO2-CeO2-ZrO2composite electrode showed excellent corrosion resistance and energy conservation compared to P-PbO2and Pb-Ag alloy. The addition of CeO2and ZrO2changed growth orientation of PbO2grains and improved texture structure and grain size of coating. Through the comprehensive performance investigation of electrode in trivalent chromium plating, it was found that β-PbO2-CeO2-ZrO2composite electrode can effectively reduce cell voltage, improve corrosion resistance and inhibit formation of hexavalent chromium. When the concentration of ZrO2is30g·L-1in bath, the Zr concentration in prepared electrode materials is high, which can reduce and stabilize cell voltage, reduce hexavalent chromium concentration effectively and ensure energy conservation and the stability of plating bath.
引文
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