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运用电化学扫描隧道显微镜(EC-STM)和循环伏安(CV)技术对高氯酸根阴离子ClO_4~-在高序热解石墨(HOPG)中的电化学嵌入行为进行了研究.通过观察嵌入前后石墨台阶处高度的变化,比较了不同高度的台阶对嵌入的影响,讨论了ClO_4~-离子嵌入石墨的可行性、可逆性和嵌入速率.研究表明,3层以上的台阶位才有可能观察到由四阶和三阶嵌入引起的台阶高度变化,4~8个原子层高度的石墨台阶可以实现ClO_4~-在台阶处较为可逆的四阶嵌入,但1~2层台阶处无法观察到嵌入引起的台阶高度变化,嵌入反应通常会伴随台阶的剥离和脱落现象.四阶的嵌入反应较三阶可逆,二阶和一阶时,嵌入所需反应电势较高,此时氧化反应较为剧烈,嵌入反应被掩盖,很难观察到台阶高度的变化,更多的形貌变化是台面和台阶处不可逆的损坏如剥落、断层、黑坑等.
The electrochemical intercalation behavior of perchlorate anion ClO_4 ~ - in high order pyrolytic graphite (HOPG) was studied by electrochemical scanning tunneling microscope (EC-STM) and cyclic voltammetry (CV) The influence of steps with different heights on the embedding was compared and the feasibility, reversibility and embedment rate of ClO_4 ~ - ions intercalated with graphite were discussed. It was found that it was only possible to observe the steps above 3 layers The step height changes caused by the fourth-order and third-order embedding, and the graphite step with 4 ~ 8 atomic layer height can achieve more reversible fourth-order intercalation of ClO_4 ~ - but no embedding can be observed in the 1st ~ 2nd step The embedding reaction usually accompanied by the peel-off and detachment of the step.The embedding reaction of the fourth order is more reversible than the third order, and the reaction potential required for embedding is higher when the second order and the first order are embedded. In this case, the oxidation reaction is more intense and the embedding The reaction is masked and it is difficult to observe changes in the height of the step. More morphological changes are irreversible damage to the surface and steps such as exfoliation, faults and black pits.