刘越仁,辛永磊,许立坤,段体岗,高显泽,郭明帅.Ti/Co3O4/RuO2-IrO2纳米结构阳极电催化析氧研究[J].表面技术,2022,51(11):436-444, 461.
LIU Yue-ren,XIN Yong-lei,XU Li-kun,DUAN Ti-gang,GAO Xian-ze,GUO Ming-shuai.Electrocatalytic Oxygen Evolution Performance of Nanostructured Ti/Co3O4/RuO2-IrO2 Anode[J].Surface Technology,2022,51(11):436-444, 461
Ti/Co3O4/RuO2-IrO2纳米结构阳极电催化析氧研究
Electrocatalytic Oxygen Evolution Performance of Nanostructured Ti/Co3O4/RuO2-IrO2 Anode
  
DOI:10.16490/j.cnki.issn.1001-3660.2022.11.041
中文关键词:  RuO2-IrO2  Co3O4纳米片  电催化  析氧  金属氧化物阳极  伏安电量
英文关键词:RuO2-IrO2  Co3O4 nanosheets  electrocatalysis  oxygen evolution  metallic oxide anode  voltammetric charge
基金项目:
作者单位
刘越仁 中国船舶重工集团公司第七二五研究所 海洋腐蚀与防护重点实验室,山东 青岛 266237 
辛永磊 中国船舶重工集团公司第七二五研究所 海洋腐蚀与防护重点实验室,山东 青岛 266237 
许立坤 中国船舶重工集团公司第七二五研究所 海洋腐蚀与防护重点实验室,山东 青岛 266237 
段体岗 中国船舶重工集团公司第七二五研究所 海洋腐蚀与防护重点实验室,山东 青岛 266237 
高显泽 中国船舶重工集团公司第七二五研究所 海洋腐蚀与防护重点实验室,山东 青岛 266237;哈尔滨工程大学 材料科学与化学工程学院,哈尔滨 150001 
郭明帅 中国船舶重工集团公司第七二五研究所 海洋腐蚀与防护重点实验室,山东 青岛 266237;哈尔滨工程大学 材料科学与化学工程学院,哈尔滨 150001 
AuthorInstitution
LIU Yue-ren State Key Laboratory for Marine Corrosion and Protection, Luoyang Ship Material Research Institute LSMRI, Shandong Qingdao 266101, China 
XIN Yong-lei State Key Laboratory for Marine Corrosion and Protection, Luoyang Ship Material Research Institute LSMRI, Shandong Qingdao 266101, China 
XU Li-kun State Key Laboratory for Marine Corrosion and Protection, Luoyang Ship Material Research Institute LSMRI, Shandong Qingdao 266101, China 
DUAN Ti-gang State Key Laboratory for Marine Corrosion and Protection, Luoyang Ship Material Research Institute LSMRI, Shandong Qingdao 266101, China 
GAO Xian-ze State Key Laboratory for Marine Corrosion and Protection, Luoyang Ship Material Research Institute LSMRI, Shandong Qingdao 266101, China;College of Material Science and Chemical Engineering, Harbin Engineering University, Harbin 15001, China 
GUO Ming-shuai State Key Laboratory for Marine Corrosion and Protection, Luoyang Ship Material Research Institute LSMRI, Shandong Qingdao 266101, China;College of Material Science and Chemical Engineering, Harbin Engineering University, Harbin 15001, China 
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中文摘要:
      目的 研发含纳米结构Co3O4中间层的Ti/Co3O4/RuO2-IrO2阳极,并对其电化学析氧性能进行研究,以提升Ti/RuO2-IrO2金属氧化物阳极的电化学析氧性能。方法 在Ti基底上电沉积制备Co(OH)2,烧结形成Co3O4纳米片结构,随后采用热分解工艺在Ti/Co3O4表面制备RuO2-IrO2电催化层,从而构建了Ti/Co3O4/ RuO2-IrO2复合阳极。使用透射电子显微镜(TEM)、扫描电子显微镜(SEM)、X-射线衍射仪(XRD)和电化学工作站对涂层的微观表面形貌、物相组成、电化学性能等进行观察与分析。结果 SEM显示出Ti/Co3O4纳米片上RuO2-IrO2的负载量随涂刷次数增加逐渐增多,最终完全遮盖Co3O4纳米片中间层。且随着RuO2- IrO2前驱体溶液涂覆次数的增加,XRD观察到RuO2-IrO2衍射峰强度在逐渐增大。TEM测试显示Co3O4中间层是由纳米颗粒堆叠组成且具有多孔结构。电化学极化曲线测试表明,涂覆三次RuO2-IrO2层的含Co3O4中间层阳极析氧电位最低,当电流密度达到10 mA/cm2时,析氧电位仅为1.326 V(vs. SCE),低于无中间层的Ti/RuO2-IrO2阳极(1.413 V)。循环伏安测试表明,Ti/Co3O4/RuO2-IrO2阳极的伏安电量达到62.83 mC/cm2,相较于Ti/RuO2-IrO2阳极的23.65 mC/cm2提高了166%。稳定性能试验表明,在经过1 000次循环稳定性试验后,加入Co3O4纳米片中间层的复合阳极的伏安电量降低了35.94%,低于无中间层阳极48.88%的伏安电量损耗率。循环极化试验后的Ti/Co3O4/RuO2-IrO2复合阳极的电化学活性仍明显优于循环极化试验前的Ti/RuO2-IrO2阳极。结论 Co3O4纳米片中间层的加入使得Ti/Co3O4/RuO2-IrO2阳极的电催化析氧性能和稳定性都得到了提升。
英文摘要:
      In order to improve the electrocatalytic oxygen evolution performance of Ti/RuO2-IrO2 anode, Ti/Co3O4/RuO2- IrO2 composite anode with nano-structured Co3O4 interlayer was developed. The electrochemical oxygen evolution performance of the composite anode was studied. The TA0 titanium plate sample (100 mm×20 mm×10 mm) was degreased and cleaned, then boiled in 10wt.% oxalic acid aqueous solution for 2 hours to remove the surface oxide film. The coating was prepared by potentiostatic electrodeposition. Electrodeposition adopts standard three-electrode system, and the plating solution is 0.05 mol/L aqueous solution of Co(NO3)2. The electrodeposition parameters were:applied potential ‒1.0 V (vs. SCE), solution temperature was 25 ℃, and deposition time was 30 min. After the electrodeposition was completed, the coated samples were placed in a muffle furnace and sintered at 350 ℃ for 1 hour to obtain Co3O4 nanosheet structure (Ti/Co3O4). H2IrCl6.6H2O and RuCl3.xH2O were mixed and dissolved in n-butanol, and then stirred for 30 min to form a coating solution with a concentration of 0.3 mol/L (Ir∶Ru=1∶9). The solution was uniformly coated on the prepared Ti/Co3O4 sample, then the sample was placed in a constant temperature oven at 120 ℃ for 20 min, and finally calcined in a muffle furnace at 500 ℃ for 1 hour. The above process was repeated 1 to 5 times to obtain Ti/Co3O4/RuO2-IrO2 composite anodes with different RuO2-IrO2 loadings. Then,the micro morphology of the coating was observed by scanning electron microscope (JSM-6700F) and transmission electron microscope (TECNAI G2 F20 s-twin). The component is analyzed by the EDS spectrum of each selected point taken by an energy spectrometer. Analyze the phase composition of the coating by an X-ray diffractometer (D8 Advance). Finally, electrochemical analysis was performed using an electrochemical workstation (Parstat 2273), and the samples were subjected to potentiodynamic polarization tests, cyclic voltammetry tests and cyclic stability tests. The Ti/Co3O4/RuO2-IrO2 anode with nanostructured Co3O4 interlayer was successfully prepared on the surface of Ti substrate by electrodeposition and sintering. The results showed that the intensity of XRD diffraction peak of RuO2-IrO2 gradually increased with the increase of coating times on the surface of Co3O4 nanosheets. SEM showed that the RuO2-IrO2 mixed nanoparticles loaded on Co3O4 nanosheets increased gradually with the increment of coating times, and finally the Co3O4 interlayer was covered. TEM analysis showed that Co3O4 nanosheets were made up of nanoparticles and had a porous structure. The polarization curves showed that the oxygen evolution potential of the composite anode containing Co3O4 interlayer coated with three layers of RuO2-IrO2 was the lowest. When the current density was 10 mA/cm2, the oxygen evolution potential of the composite anode was 1.326 V (vs. SCE), lower than that of the Ti/RuO2-IrO2 anode without interlayer (1.413 V). Cyclic voltammetric measurement showed that Ti/Co3O4/RuO2-IrO2 anode had a high electrocatalytic active surface area with a voltammetric charge of 62.83 mC/cm2, which was 166% higher than that of Ti/ RuO2-IrO2 anode (23.65 mC/cm2). Stability test demonstrated that after 1 000 cycles of cyclic stability test, the loss rate of voltammetric charge of the composite anode was 35.94%, which was lower than that of the anode without interlayer (48.88%), and the electrochemical activity of the composite anode with interlayer after the stability test with cyclic polarization was still obviously better than that of Ti/RuO2-IrO2 anode before cyclic polarization test. The Co3O4 with nanosheet structure can improve the electronic conductivity and increase the specific surface area; after loading the uniformly dispersed RuO2-IrO2 nanoparticles, the electrochemically active surface area of the composite anode increases significantly. Therefore, the addition of the interlayer of Co3O4 nanosheets improves the electrocatalytic oxygen evolution performance and stability of the Ti/Co3O4/ RuO2-IrO2 anode.
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