改进Hummers法制备氧化石墨烯的机理研究 |
作者:徐博,李春丽,张浩月,弓哲,于颖,邱广明 |
单位: 内蒙古工业大学 能源与动力工程,呼和浩特 010000 |
关键词: 改进Hummers法;氧化石墨烯;氧化程度;热稳定性 |
出版年,卷(期):页码: 2021,41(6):18-26 |
摘要: |
本文基于改进Hummers法,在不使用硝酸纳的情况下制备氧化石墨烯(Graphene Oxide, GO),实验研究了制备过程中氧化剂用量及中温阶段氧化反应时间对GO氧化程度的影响。采用扫描电镜(SEM)对GO样品的形态结构进行表征;傅里叶红外光谱(FT-IR)、X射线能谱分析(EDS)、激光显微拉曼光谱(Raman)对样品的官能团及氧化程度进行分析;热重分析(TG-DTG)对样品进行热稳定性测试。SEM图片显示,氧化剂用量和氧化反应时间在一定程度上影响所制备GO的表面形貌;Raman光谱表明制备的GO具有不同的缺陷密度;FT-IR和EDS分析发现GO表面含丰富含氧官能团,不同GO样品的含氧量在33%-43%之间,C/O在1.9-1.1之间;TGA分析与元素分析结果相关,表明热失重与元素组成有明显的依赖关系,由于氧含量提高,GOc-3具有最大的失重,而GOa-1具有较高的热稳定性。本研究所得的基于改进的Hummers法制备GO的氧化剂用量和氧化时间的结果分析为后续GO功能化改性提供了理论和数据支撑。 |
Based on the improved Hummers method, graphene oxide (GO) was prepared without sodium nitrate.The effects of oxidant dosage and oxidation reaction time at medium temperature on the GO oxidation degree were studied in this experiment.The morphological structure of GO samples was characterized by SEM; The functional groups and oxidation degree of the samples were analyzed by Fourier infrared spectroscopy (FT-IR), X-ray energy spectrum analysis (EDS), laser microscopic Raman spectroscopy (Raman) ;The thermal stability of the samples was tested by Thermogravimetric analysis (TG-DTG).The SEM image showed that the amount of oxidant and the oxidation reaction time affected the surface morphology of the prepared GO to some extent; Raman spectra showed that the prepared GO had different defect densities; FT-IR and EDS analysis showed that the surface of GO was rich in oxygen-containing functional groups, The oxygen content of different GO samples was between 33%-43%, and the C/O was between 1.9-1.1;The correlation between TGA analysis and elemental analysis results indicated that the thermal weight loss is obviously dependent on element composition, due to the increase of oxygen content, GOc-3 had the largest weight loss, while GOa-1 had better thermal stability.The analysis of the oxidant dosage and oxidation time of GO prepared by the improved Hummers method provides theoretical and data support for the subsequent functional modification of GO. |
徐博(1996-),男,吉林省公主岭市人,硕士生,研究方向为膜分离水处理技术,E-mail:914739874@qq.com |
参考文献: |
[1]LIU Y, LU J, CUI Y. Improved thermal conductivity of epoxy resin by graphene-nickel three-dimensional filler[J]. Carbon Resources Conversion, 2020, 3(12):29-35. [2]HUANG Kun, ZENG Xianguang, PEI Songfeng, et al. Research on low voltage high electric heating performance of graphere composite coatings[J]. Paint and Coatings Industry, 2016, 46(4):13-17. [3]王朋辉, 李怡恩, 张亚涛.氧化石墨烯尺寸调控及其复合膜分离性能研究[J].膜科学与技术, 2019, 39(03):62-69. [4]金文杰, 胡朝武, 李丽华, 等.氧化石墨烯含量对聚砜超滤膜结构和性能的影响[J].膜科学与技术, 2015, 35(04):20-34. [5]DAS R S, WARKHADE S K, KUMAR A, et al. Graphene oxide-based zirconium oxide nanocomposite for enhanced visible light-driven photocatalytic activity[J]. Research on Chemical Intermediates, 2019, 45(4):1689-1705. [6]SHAIKH M, SINGH S K, KHILARI S, et al. Graphene oxidee as a sustainable metal and solvent free catalyst for dehydration of fructose to 5-HMF:a new and green protocol[J]. Catalysis Communications, 2018, 106(018):64-67. [7]Brodie B C. On the atomic weight of graphite. Philos Trans R Soc London, 1859, 14(9):249-259. [8]Staudenmaier, L. Process for the preparation of graphite acid. Ber. Dtsch. Chem. Ges, 1898, 31(2):1481–1487. [9]Hummers, W. S. Offeman, R. E. Preparation of Graphitic Oxide. J. Am. Chem. Soc, 1958, 25(80):1334-1339. [10]Dreyer DR, Park S, Bielawski CW ,et al. The chemistry of graphene oxide. Chem Soc Rev,2010;39(1):228-40. [11]Sorokina NE, Khaskov MA, Avdeev VV ,et al.Reaction of graphite with sulfuric acid in the presence of KMnO4. Russ J Gen Chem 2005;75(2):162-8. [12]Marcano D C, Kosynkin D V , Berlin J M , et al. Improved synthesis of graphene oxide.[J]. Acs Nano, 2010, 4(8):4806-4810. [13]Ji Chen, Bowen Yao, Chun Li, et al. An improved Hummers method for eco-friendly synthesis of graphene oxide[J]. Carbon, 2013, 65(055):225-229. [14]Jesus Guerrero-Contreras, F. Caballero-Briones.Graphene oxide powders with different oxidation degree, prepared by synthesis variations of the Hummers method[J].Materials Chemistry and Physics, 2015, 153(5):209-220. [15]Alkhouzaam A, Qiblawey H , Khraisheh M, et al. Synthesis of graphene oxides particle of high oxidation degree using a modified Hummers method[J]. Ceramics International, 2020, 46(15):23997-24007. [16]Dikin D A, Stankovich S, Zimney E J, et al. Preparation and characterization of graphene oxide paper[J]. Nature, 2015, 7152(448):457-460. [17]Jannik C. Meyer, A. K. Geim, M. I. Katsnelson, et al. The structure of suspended graphene sheets[J]. Nature: International weekly journal of science, 2007, 446(7131):60-63. [18]R. Al-Gaashani, A. Najjar, Y. Zakaria, et al. XPS and structural studies of high quality graphene oxide and reduced graphene oxide prepared by different chemical oxidation methods[J]. Ceramics International, 2019, 45 (11):14439-14448. [19]Al-Gaashani R, Zakaria Y, Lee O S, et al. Effects of preparation temperature on production of graphene oxide by novel chemical processing[J]. Ceramics International, 2020, 47(12):10113-10112. [20]Alkhouzaam A, Qiblawey H , Khraisheh M, et al. Synthesis of graphene oxides particle of high oxidation degree using a modified Hummers method[J]. Ceramics International, 2020, 46(15):23997-24007. [21]赖奇, 罗学萍.氧化石墨烯的制备和定性定量分析[J].材料研究学报, 2015, 29(02):155-160. [22]Vasu KS, Chakraborty B, Sampath S, et al. Probing top-gated field effect transistor of reduced graphene oxide monolayer made by dielectrophoresis[J]. Solid State Communications,2010, 150(29):1295-1298. [23]T.Nakajima, A. Mabuchi, R. Hagiwara.A New Structure Model of Graphite Oxide[J].Carbon, 1988, 26(3):357-361. |
服务与反馈: |
【文章下载】【加入收藏】 |
《膜科学与技术》编辑部 地址:北京市朝阳区北三环东路19号蓝星大厦 邮政编码:100029 电话:010-64426130/64433466 传真:010-80485372邮箱:mkxyjs@163.com
京公网安备11011302000819号