退火时间对Ni催化非晶碳转变石墨烯的影响  

Effects of Annealing Duration on Transformation from Amorphous Carbon to Graphene via Nickel Catalyst

作　　者：李汉超 魏菁 郭鹏[1,2,3] 孙丽丽[1,2,3] 崔平[1,2,3,4] 汪爱英[1,2,3,5] LI Han-chao;WEI Jing;GUO Peng;SUN Li-li;CUI Ping;WANG Ai-ying(Key Laboratory of Marine Materials and Related Technologies, Chinese Academy of Sciences, Ningbo 315201, China;Zhejiang Key Laboratory of Marine Materials and Protective Technologies, Chinese Academy of Sciences, Ningbo 315201, China;Ningbo Institute of Materials Technology and Engineering, Chinese Academy of Sciences, Ningbo 315201, China;School of Physical Science and Technology, Shanghai Tech University, Shanghai 201210, China;Center of Materials Science and Optoelectronics Technology, University of Chinese Academy of Sciences, Beijing 100049, China)

机构地区：[1]中国科学院海洋新材料与应用技术重点实验室,浙江宁波315201 [2]中国科学院浙江省海洋材料与防护技术重点实验室,浙江宁波315201 [3]中国科学院宁波材料技术与工程研究所,浙江宁波315201 [4]上海科技大学物质科学与技术学院,上海201210 [5]中国科学院大学材料与光电研究中心,北京100049

出　　处：《表面技术》2019年第6期66-72,共7页Surface Technology

基　　金：中国科学院A类战略性先导科技专项(XDA22010303);宁波市科技创新2025重大专项(2018B10014);宁波市自然科学基金(2018A610171);宁波市江北区重大科技专项(201801A03)~~

摘　　要：目的研究不同退火时间对Ni催化非晶碳转化生成石墨烯的影响。方法采用磁过滤电弧沉积技术,在SiO2/Si基片上制备非晶碳薄膜,之后利用磁控溅射技术,在非晶碳薄膜上镀上一层金属Ni。再将样品放置在管式炉中进行真空退火热处理。通过X射线光电子能谱(XPS)表征非晶碳的化学价态,利用扫描电子显微镜(SEM)观察退火前后样品的表面形貌变化,利用拉曼光谱(Raman spectra)对生成的石墨烯进行质量表征,采用透射电子显微镜(TEM)对微观石墨烯结构进行表征。结果 700~800℃范围内,合理延长退火时间至60 min,可以提高生成的石墨烯质量,使得ID/IG值分别从0.63、0.61降至0.53、0.46。TEM显示,700℃退火60min时,得到的石墨烯约为32层。900℃时,在1~10min短时间内退火,即可得到高质量石墨烯。结论退火时间显著影响非晶碳转化生成的石墨烯。900℃时,短时间退火可以生成高质量石墨烯,而在700~800℃时,则需要延长退火时间才可得到高质量石墨烯。退火时间并不能无限延长,否则会导致生成的石墨烯结构被破坏。This work aims to investigate effects of annealing duration on transformation from amorphous carbon to graphene via nickel catalyst. The magnetic filtered arc deposition technology was used to prepare amorphous carbon (a-C) film on the SiO2/Si substrate. Then, a layer of nickel was deposited on the amorphous carbon film by magnetron sputtering. Then the sample was put in a pipe furnace for vacuum thermal annealing processing. The chemical valence state of a-C was characterized by X-ray photoelectron spectroscopy. The structure and surface morphology change before and after annealing were investigated with a SEM and the quality of the graphene generated was characterized with Raman spectroscopy. The micro structure of the graphene was characterized with a TEM. The annealing duration greatly affected the graphene generated for transformation of a-C. At 900 ℃, high-quality graphene was obtained in a short time of annealing. Similar high-quality graphene was obtained at 700 ℃ and 800 ℃ after the annealing duration was extended. However, the annealing duration cannot be extended infinitely;otherwise the structure of the graphene might be damaged. Proper extension of annealing duration to 60 min at 700 ℃ to 800 ℃ can improve the quality of the graphene generated and reduce ID/IG from 0.63 to 0.53. TEM shows that 32 layers of graphene can be obtained by annealing at 700 ℃ for 60 min. Graphene of high quality can be obtained by short time (1 min-10 min) of annealing at 900 ℃.

关 键 词：非晶碳 石墨烯 相转变 Ni催化 退火时间 固体碳源 

分 类 号：TG156[金属学及工艺—热处理]