制备方法对二氧化铅电极结构及性能的影响
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摘要
本文以PbO_2电极为研究对象,探讨了制备方法对PbO_2电极结构、形貌、电化学性能以及电极稳定性和寿命的影响,并以不同方法制备的PbO_2电极为阳极,研究了Cr~(3+)电化学氧化过程的反应速率及瞬时电流效率。
(1)分别采用电解法制备了Pb/PbO_2电极、用电沉积法制备了Ti/SnO_2+Sb_2O_3/PbO_2电极、用热分解法制备了钛基铅氧化物膜层,对它们的结构及形貌进行了表征。研究了热分解法制备的钛基铅氧化物膜层及电沉积法制备的钛基PbO_2电极添加中间层前后的形貌和结构。结果表明:三种不同方法制备的PbO_2结构明显不同。电解法制备的Pb/PbO_2电极的表面结构由β-PbO_2和α-PbO_2组成;采用电沉积法制备的Ti/SnO_2+Sb_2O_3/PbO_2电极其表面结构主要为β-PbO_2;而热分解法制备的钛基铅氧化物膜层表面结构主要是Pb3O4,且需经阳极氧化方可转为β-PbO_2电极。此外,热分解法制备的钛基铅氧化物膜层及电沉积法制备的钛基PbO_2电极添加中间层前后的结构无明显差异。三种不同方法制备的PbO_2电极的表面形貌存在明显差异,Pb/PbO_2电极没有规则的结晶,表面有明显孔洞,堆积疏松。电沉积法制备的Ti/SnO_2+Sb_2O_3/PbO_2电极表面呈块状堆积,而热分解法制备的添加锡锑中间层的钛基铅氧化物膜层呈棒状,经电解转为β-PbO_2,形貌仍为棒状。
(2)电极活性表面积的大小可反映电极的电催化性能,而电极表面的电化学活性表面积又可用伏安电荷来表征。在硫酸介质中,对不同扫描速度下的循环伏安曲线积分可得到伏安电荷,根据伏安电荷与扫描速度的关系可以计算得到电极的电化学内活性表面积和外活性表面积。实验结果表明:电沉积法制备的Ti/SnO_2+Sb_2O_3/PbO_2电极的电化学活性表面积最小,热分解法制备的Ti/SnO_2+Sb_2O_3/PbO_2电极与Pb/PbO_2电极相比,总电化学活性表面积及内活性表面积均较高,外活性表面积则比较小。三种不同方法制备的PbO_2电极在硫酸溶液中的伏安特性研究表明:析氧电位由小到大依次为:热分解法制备的Ti/SnO_2+Sb_2O_3/PbO_2电极、电解法制备的Pb/PbO_2电极、电沉积法制备的Ti/SnO_2+Sb_2O_3/PbO_2电极。在相同电位下,阳极氧化过程的电流密度由高到低依次为:热分解法制备的Ti/SnO_2+Sb_2O_3/PbO_2电极、电解法制备的Pb/PbO_2电极、电沉积法制备的Ti/SnO_2+Sb_2O_3/PbO_2电极。在60℃、1.0mol/L H_2SO_4溶液、电流密度为4.0A/cm~2的实验条件下,强化电极寿命结果表明:电沉积法制备的Ti/SnO_2+Sb_2O_3/PbO_2电极的强化寿命最长为135h,电极电解120h槽电压变化不大,比较稳定;而热分解法制备Ti/SnO_2+Sb_2O_3/PbO_2电极的寿命仅为25h,电解22h电极比较稳定。
(3)分别以不同方法制备的PbO_2电极为工作电极,研究了Cr~(3+)的电化学氧化,测试结果表明:三种电极的阳极氧化峰电流均随着硫酸介质中Cr~(3+)浓度的增大而略有降低。分别以三种不同方法制备的PbO_2电极为阳极,研究了Cr~(3+)电化学氧化过程的反应速率及电流效率。实验结果表明:在相同实验的条件下,以热分解法制备的Ti/SnO_2+Sb_2O_3/PbO_2电极为阳极时,Cr~(3+)电化学氧化过程的反应速率及电流效率最大,Pb/PbO_2电极次之,而以电沉积法制备的Ti/SnO_2+Sb_2O_3/PbO_2电极为阳极时过程的反应速率及电流效率则最小。
The anodes of PbO_2 were studied in this paper. The surface microstructure and morphology, electrochemical performance and life time of the PbO_2 anodes prepared by different methods were studied. The reaction rates and current efficiencies of the oxidation of Cr~(3+) with the PbO_2 prepared by different methods as anodes under the same experimental condition were compared.
(1) The Pb/PbO_2 anode was prepared by electrolysis, the Ti/SnO_2+Sb_2O_3/PbO_2 anode was prepared by electrodeposition, and the lead oxide coatings were prepared by thermal decomposition. The surface microstructure of the PbO_2 prepared by different methods was examined by means of XRD. The experimental results show that the microstructures of the PbO_2 anodes prepared by different methods are different. The microstructure of the Pb/PbO_2 anode prepared by electrolysis is consisted of mixture ofα- andβ-phases of PbO_2; The microstructure of the Ti/SnO_2+Sb_2O_3/PbO_2 anode prepared by electrodeposition is detected mainly theβ-phases of PbO_2, and an examination of the XRD show the microstructure of lead oxide coatings prepared by thermal decomposition are Pb3O4. In addition, the microstructure of lead oxide coatings prepared by thermal decomposition are changing during electrolysis in H_2SO_4, the films of Pb3O4 are completely converted to theβ-PbO_2 after electrolysis. In addition, The surface morphology of the PbO_2 anodes prepared by different methods was examined by means of SEM. An amorphous mass with high porosity is formed in the surface of the Pb/PbO_2 anode and the morphology of the Ti/SnO_2+Sb_2O_3/PbO_2 anode prepared by electrodeposition display a blocklike structure; The SEM micrographs of the lead oxide coatings prepared by thermal decomposition showed that its morphology is sticklike structure.
(2) The activity of electrocatalysts depends on the electrochemical active surface area partly. Electrochemical active surface area of PbO_2 anodes prepared by different methods was calculated. The results show that the electrochemical active surface area of PbO_2 anodes prepared by electrodeposition is the lowest. And the electrochemical active surface area of Ti/SnO_2+Sb_2O_3/PbO_2 anode prepared by thermal decomposition is higher than the anode of Pb/PbO_2. The electrochemical behavior of the PbO_2 anodes prepared by different methods was determined, the experimental results show that the peak current of the evolution of oxygen may be arranged by the following order: the anode of Ti/SnO_2+Sb_2O_3/PbO_2 prepared by thermal decomposition is higher than the anode of Pb/PbO_2 prepared by electrolysis, and the anode of Pb/PbO_2 prepared by electrolysis is higher than the anode of Ti/SnO_2+Sb_2O_3/PbO_2 prepared by electrodeposition. The lifetimes of the Ti/SnO_2+Sb_2O_3/PbO_2 anodes prepared by different methods were assessed by the accelerated lifetime test, and the experimental results show that the lifetime of Ti/SnO_2+Sb_2O_3/PbO_2 anode prepared by electrodeposition performed at 60℃and in 1.0mol/L H_2SO_4 with an anodic current density of 4.0A/cm~2 is 135h while the lead oxide coatings prepared by thermal decomposition is 25h.
(3) The electrochemical behavior of the PbO_2 anodes prepared by different methods were studied, the experimental results show that the peak current of the evolution of oxygen decrease with increasing the concentration of Cr~(3+). Under the same experimental condition, the reaction rates and current efficiencies of the oxidation of Cr~(3+) with the Ti/SnO_2+Sb_2O_3/PbO_2 prepared by thermal decomposition as anode are higher than the Pb/PbO_2, and the Ti/SnO_2+Sb_2O_3/PbO_2 anode prepared by electrodeposition is the lowest.
(1)分别采用电解法制备了Pb/PbO_2电极、用电沉积法制备了Ti/SnO_2+Sb_2O_3/PbO_2电极、用热分解法制备了钛基铅氧化物膜层,对它们的结构及形貌进行了表征。研究了热分解法制备的钛基铅氧化物膜层及电沉积法制备的钛基PbO_2电极添加中间层前后的形貌和结构。结果表明:三种不同方法制备的PbO_2结构明显不同。电解法制备的Pb/PbO_2电极的表面结构由β-PbO_2和α-PbO_2组成;采用电沉积法制备的Ti/SnO_2+Sb_2O_3/PbO_2电极其表面结构主要为β-PbO_2;而热分解法制备的钛基铅氧化物膜层表面结构主要是Pb3O4,且需经阳极氧化方可转为β-PbO_2电极。此外,热分解法制备的钛基铅氧化物膜层及电沉积法制备的钛基PbO_2电极添加中间层前后的结构无明显差异。三种不同方法制备的PbO_2电极的表面形貌存在明显差异,Pb/PbO_2电极没有规则的结晶,表面有明显孔洞,堆积疏松。电沉积法制备的Ti/SnO_2+Sb_2O_3/PbO_2电极表面呈块状堆积,而热分解法制备的添加锡锑中间层的钛基铅氧化物膜层呈棒状,经电解转为β-PbO_2,形貌仍为棒状。
(2)电极活性表面积的大小可反映电极的电催化性能,而电极表面的电化学活性表面积又可用伏安电荷来表征。在硫酸介质中,对不同扫描速度下的循环伏安曲线积分可得到伏安电荷,根据伏安电荷与扫描速度的关系可以计算得到电极的电化学内活性表面积和外活性表面积。实验结果表明:电沉积法制备的Ti/SnO_2+Sb_2O_3/PbO_2电极的电化学活性表面积最小,热分解法制备的Ti/SnO_2+Sb_2O_3/PbO_2电极与Pb/PbO_2电极相比,总电化学活性表面积及内活性表面积均较高,外活性表面积则比较小。三种不同方法制备的PbO_2电极在硫酸溶液中的伏安特性研究表明:析氧电位由小到大依次为:热分解法制备的Ti/SnO_2+Sb_2O_3/PbO_2电极、电解法制备的Pb/PbO_2电极、电沉积法制备的Ti/SnO_2+Sb_2O_3/PbO_2电极。在相同电位下,阳极氧化过程的电流密度由高到低依次为:热分解法制备的Ti/SnO_2+Sb_2O_3/PbO_2电极、电解法制备的Pb/PbO_2电极、电沉积法制备的Ti/SnO_2+Sb_2O_3/PbO_2电极。在60℃、1.0mol/L H_2SO_4溶液、电流密度为4.0A/cm~2的实验条件下,强化电极寿命结果表明:电沉积法制备的Ti/SnO_2+Sb_2O_3/PbO_2电极的强化寿命最长为135h,电极电解120h槽电压变化不大,比较稳定;而热分解法制备Ti/SnO_2+Sb_2O_3/PbO_2电极的寿命仅为25h,电解22h电极比较稳定。
(3)分别以不同方法制备的PbO_2电极为工作电极,研究了Cr~(3+)的电化学氧化,测试结果表明:三种电极的阳极氧化峰电流均随着硫酸介质中Cr~(3+)浓度的增大而略有降低。分别以三种不同方法制备的PbO_2电极为阳极,研究了Cr~(3+)电化学氧化过程的反应速率及电流效率。实验结果表明:在相同实验的条件下,以热分解法制备的Ti/SnO_2+Sb_2O_3/PbO_2电极为阳极时,Cr~(3+)电化学氧化过程的反应速率及电流效率最大,Pb/PbO_2电极次之,而以电沉积法制备的Ti/SnO_2+Sb_2O_3/PbO_2电极为阳极时过程的反应速率及电流效率则最小。
The anodes of PbO_2 were studied in this paper. The surface microstructure and morphology, electrochemical performance and life time of the PbO_2 anodes prepared by different methods were studied. The reaction rates and current efficiencies of the oxidation of Cr~(3+) with the PbO_2 prepared by different methods as anodes under the same experimental condition were compared.
(1) The Pb/PbO_2 anode was prepared by electrolysis, the Ti/SnO_2+Sb_2O_3/PbO_2 anode was prepared by electrodeposition, and the lead oxide coatings were prepared by thermal decomposition. The surface microstructure of the PbO_2 prepared by different methods was examined by means of XRD. The experimental results show that the microstructures of the PbO_2 anodes prepared by different methods are different. The microstructure of the Pb/PbO_2 anode prepared by electrolysis is consisted of mixture ofα- andβ-phases of PbO_2; The microstructure of the Ti/SnO_2+Sb_2O_3/PbO_2 anode prepared by electrodeposition is detected mainly theβ-phases of PbO_2, and an examination of the XRD show the microstructure of lead oxide coatings prepared by thermal decomposition are Pb3O4. In addition, the microstructure of lead oxide coatings prepared by thermal decomposition are changing during electrolysis in H_2SO_4, the films of Pb3O4 are completely converted to theβ-PbO_2 after electrolysis. In addition, The surface morphology of the PbO_2 anodes prepared by different methods was examined by means of SEM. An amorphous mass with high porosity is formed in the surface of the Pb/PbO_2 anode and the morphology of the Ti/SnO_2+Sb_2O_3/PbO_2 anode prepared by electrodeposition display a blocklike structure; The SEM micrographs of the lead oxide coatings prepared by thermal decomposition showed that its morphology is sticklike structure.
(2) The activity of electrocatalysts depends on the electrochemical active surface area partly. Electrochemical active surface area of PbO_2 anodes prepared by different methods was calculated. The results show that the electrochemical active surface area of PbO_2 anodes prepared by electrodeposition is the lowest. And the electrochemical active surface area of Ti/SnO_2+Sb_2O_3/PbO_2 anode prepared by thermal decomposition is higher than the anode of Pb/PbO_2. The electrochemical behavior of the PbO_2 anodes prepared by different methods was determined, the experimental results show that the peak current of the evolution of oxygen may be arranged by the following order: the anode of Ti/SnO_2+Sb_2O_3/PbO_2 prepared by thermal decomposition is higher than the anode of Pb/PbO_2 prepared by electrolysis, and the anode of Pb/PbO_2 prepared by electrolysis is higher than the anode of Ti/SnO_2+Sb_2O_3/PbO_2 prepared by electrodeposition. The lifetimes of the Ti/SnO_2+Sb_2O_3/PbO_2 anodes prepared by different methods were assessed by the accelerated lifetime test, and the experimental results show that the lifetime of Ti/SnO_2+Sb_2O_3/PbO_2 anode prepared by electrodeposition performed at 60℃and in 1.0mol/L H_2SO_4 with an anodic current density of 4.0A/cm~2 is 135h while the lead oxide coatings prepared by thermal decomposition is 25h.
(3) The electrochemical behavior of the PbO_2 anodes prepared by different methods were studied, the experimental results show that the peak current of the evolution of oxygen decrease with increasing the concentration of Cr~(3+). Under the same experimental condition, the reaction rates and current efficiencies of the oxidation of Cr~(3+) with the Ti/SnO_2+Sb_2O_3/PbO_2 prepared by thermal decomposition as anode are higher than the Pb/PbO_2, and the Ti/SnO_2+Sb_2O_3/PbO_2 anode prepared by electrodeposition is the lowest.
引文
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