王兰喜,何延春,卯江江,左华平,王虎,王艺,胡汉军,刘兴光,张凯锋,周晖.真空退火对氧化石墨烯纸的还原特性研究[J].表面技术,2021,50(10):186-193.
WANG Lan-xi,HE Yan-chun,MAO Jiang-jiang,ZUO Hua-ping,WANG Hu,WANG Yi,HU Han-jun,LIU Xing-guang,ZHANG Kai-feng,ZHOU Hui.Study on the Reduction Characteristic of Vacuum-annealed Graphene Oxide Paper[J].Surface Technology,2021,50(10):186-193 |
| 真空退火对氧化石墨烯纸的还原特性研究 |
| Study on the Reduction Characteristic of Vacuum-annealed Graphene Oxide Paper |
| 投稿时间：2021-01-06 修订日期：2021-03-24 |
| DOI：10.16490/j.cnki.issn.1001-3660.2021.10.017 |
| 中文关键词: 氧化石墨烯纸 真空退火 还原 含氧基团 晶体质量 电阻率 |
| 英文关键词:graphene oxide paper vacuum annealing reduction oxygenous group crystalline quality specific resistance |
| 基金项目:真空技术与物理重点实验室基金项目(6142207190405);甘肃省自然科学基金项目(20JR5RA080) |
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| Author | Institution |
| WANG Lan-xi | Key Laboratory of Vacuum Technology and Physics, Lanzhou Institute of Physics, Lanzhou 730000, China |
| HE Yan-chun | Key Laboratory of Vacuum Technology and Physics, Lanzhou Institute of Physics, Lanzhou 730000, China |
| MAO Jiang-jiang | School of Nuclear Science and Technology, Lanzhou University, Lanzhou 730000, China |
| ZUO Hua-ping | Key Laboratory of Vacuum Technology and Physics, Lanzhou Institute of Physics, Lanzhou 730000, China |
| WANG Hu | Key Laboratory of Vacuum Technology and Physics, Lanzhou Institute of Physics, Lanzhou 730000, China |
| WANG Yi | Key Laboratory of Vacuum Technology and Physics, Lanzhou Institute of Physics, Lanzhou 730000, China |
| HU Han-jun | Key Laboratory of Vacuum Technology and Physics, Lanzhou Institute of Physics, Lanzhou 730000, China |
| LIU Xing-guang | Key Laboratory of Vacuum Technology and Physics, Lanzhou Institute of Physics, Lanzhou 730000, China |
| ZHANG Kai-feng | Key Laboratory of Vacuum Technology and Physics, Lanzhou Institute of Physics, Lanzhou 730000, China |
| ZHOU Hui | Key Laboratory of Vacuum Technology and Physics, Lanzhou Institute of Physics, Lanzhou 730000, China |
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| 中文摘要: |
| 目的 获得真空退火对氧化石墨烯纸的还原特性，为制备石墨烯纸柔性功能材料提供有效的还原方法。方法 通过不同温度真空退火对氧化石墨烯纸进行还原。利用X射线光电子能谱仪分析还原氧化石墨烯纸中的含氧基团及其含量，利用X射线衍射仪、拉曼光谱仪和扫描电子显微镜表征还原氧化石墨烯纸的晶体质量，利用高阻计和四探针测试还原氧化石墨烯纸的电阻率。研究了真空退火还原氧化石墨烯纸中含氧基团、晶体质量和电阻率随退火温度的演化规律。结果 200 ℃真空退火可有效去除氧化石墨烯纸中的主要含氧基团——环氧基，使氧化石墨烯纸的电阻率大幅下降;600 ℃以下真空退火主要以含氧基团相互作用形成羰基，并形成原子空位缺陷;600~1000 ℃真空退火主要去除缺陷边缘的羰基和羧基，侵蚀原子空位形成较大的孔洞，使晶体质量变差;1200 ℃真空退火能够使石墨烯重结晶，同时修复缺陷，促进sp2结构的恢复，但仍残留少量含氧基团不易去除，晶体质量和电阻率与石墨比较也存在一定的差距。结论 真空退火是一种还原氧化石墨烯纸的有效方法，退火温度在1000 ℃以上具有良好的还原特性。为了获得深度还原的氧化石墨烯纸，需要进一步提高真空退火温度或发展较低温度下氧化石墨烯纸的增强还原方法。 |
| 英文摘要: |
| The aim of the study was to achieve the reduction characteristic of vacuum annealed graphene oxide paper, and to provide an effective reduction method for preparing flexible graphene paper functional materials. The graphene oxide papers were reduced by vacuum annealing with different temperatures. Oxygenous groups and their percentages in reduced graphene oxide papers were analyzed by X-ray photoelectron spectroscopy. Crystalline quality of the reduced graphene oxide papers was characterized by X-ray diffraction and Raman spectrum. High resistance meter and four probe meter were used to measure the specific resistance of the reduced graphene oxide papers. From all above, evolutions of oxygenous groups, crystalline quality and specific resistance with annealing temperature were studied. The major oxygenous group in graphene oxide paper, epoxy group, can be removed by vacuum annealing at 200 ℃, which resulted in significant decrease of the specific resistance. When the Graphene oxide paper was vacuum-annealed below 600 ℃, the oxygenous groups would be interacted remarkably to form carbonyl groups and atomic vacancy defects. Carbonyl and carboxyl groups at defect edges would be removed primarily at temperatures between 600~1000 ℃. Meanwhile, the crystalline quality would get worse as a consequence of large lattice holes generated by etching atomic vacancies. The graphene can be recrystallized to mend defects and restore sp2 phase by vacuum annealing at 1200 ℃. However, there were still a small number of oxygenous groups existing in the reduced graphene oxide paper annealed at 1200 ℃, and the crystalline quality and specific resistance were not as good as the corresponding values of graphite. The results show that vacuum annealing is an effective method to reduce graphene oxide paper. Good reduction characteristic can be achieved by vacuum annealing above 1000 ℃. In order to obtain reduced graphene oxide paper to an extreme, it is necessary to further increase the vacuum annealing temperature or develop enhanced reduction methods at lower temperatures. |
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