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喷雾成型单壁碳纳米管薄膜的O等离子体蚀刻方法及其作为电化学传感器电极的应用研究

A Study on the O Plasma Etching Method of Spray-Formed SWCNT Films and Their Utilization as Electrodes for Electrochemical Sensors.

作者信息

Kim Jinkyeong, Han Ji-Hoon, Kim Joon Hyub

机构信息

Department of Nanomechatronics Engineering, Pusan University, 2 Busandaehak-ro 63 Beon-gil, Geumjeong-gu, Busan 46241, Republic of Korea.

KIURI Center for Hydrogen Based Next Generation Mechanical System, Inha University, Incheon 22212, Republic of Korea.

出版信息

Sensors (Basel). 2023 Sep 11;23(18):7812. doi: 10.3390/s23187812.

Abstract

In this study, we analyzed the morphological changes and molecular structure changes on the surface of single-walled carbon nanotube (SWCNT) films during oxygen plasma (O) etching of SWCNT surfaces formed by the spray method and analyzed their potential use as electrochemical electrodes. For this purpose, a SWCNT film was formed on the surface of a glass substrate using a self-made spray device using SWCNT powder prepared with DCB as a solvent, and SEM, AFM, and XPS analyses were performed as the SWCNT film was O plasma etched. SEM images and AFM measurements showed that the SWCNT film started etching after about 30 s under 50 W of O plasma irradiation and was completely etched after about 300 s. XPS analysis showed that as the O plasma etching of the SWCNT film progressed, the sp bonds representing the basic components of graphite decreased, the 3 bonds representing defects increased, and the C-O, C=O, and COO peaks increased simultaneously. This result indicates that the SWCNT film was etched by the O plasma along with the oxygen species. In addition, electrochemical methods were used to verify the damage potential of the remaining SWCNTs after O plasma etching, including cyclic voltammetry, Randles plots, and EIS measurements. This resulted in a reversible response based on perfect diffusion control in the cyclic voltammetry, and an ideal linear curve in the Randles plot of the peak current versus square root scan rate curve. EIS measurements also confirmed that the charge transfer resistance of the remaining SWCNTs after O plasma etching is almost the same as before etching. These results indicate that the remaining SWCNTs after O plasma etching do not lose their unique electrochemical properties and can be utilized as electrodes for biosensors and electrochemical sensors. Our experimental results also indicate that the ionic conductivity enhancement by O plasma can be achieved additionally.

摘要

在本研究中,我们分析了通过喷雾法形成的单壁碳纳米管(SWCNT)薄膜表面在氧等离子体(O)蚀刻过程中的形态变化和分子结构变化,并分析了它们作为电化学电极的潜在用途。为此,使用以二氯苯为溶剂制备的SWCNT粉末,通过自制喷雾装置在玻璃基板表面形成SWCNT薄膜,并在对SWCNT薄膜进行O等离子体蚀刻时进行扫描电子显微镜(SEM)、原子力显微镜(AFM)和X射线光电子能谱(XPS)分析。SEM图像和AFM测量结果表明,在50 W的O等离子体辐照下,SWCNT薄膜在约30 s后开始蚀刻,并在约300 s后完全蚀刻。XPS分析表明,随着SWCNT薄膜的O等离子体蚀刻的进行,代表石墨基本成分的sp键减少,代表缺陷的3键增加,同时C-O、C=O和COO峰增加。该结果表明,SWCNT薄膜与氧物种一起被O等离子体蚀刻。此外,采用电化学方法验证了O等离子体蚀刻后剩余SWCNT的损伤潜力,包括循环伏安法、兰德尔图和电化学阻抗谱(EIS)测量。这导致在循环伏安法中基于完美扩散控制的可逆响应,以及在峰值电流与平方根扫描速率曲线的兰德尔图中呈现理想的线性曲线。EIS测量还证实,O等离子体蚀刻后剩余SWCNT的电荷转移电阻与蚀刻前几乎相同。这些结果表明,O等离子体蚀刻后剩余的SWCNT不会失去其独特的电化学性质,可作为生物传感器和电化学传感器的电极。我们的实验结果还表明,通过O等离子体还可以额外实现离子电导率的增强。

https://cdn.ncbi.nlm.nih.gov/pmc/blobs/4a10/10537897/33bb29cb1507/sensors-23-07812-g001.jpg

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