低温氧化石墨制备技术研究
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摘要
采用Hummers法、硫酸/磷酸法和反应釜法3种化学氧化法制备氧化石墨,在超声情况下,将氧化石墨分散于水中制备氧化石墨烯。采用X衍射(XRD)、扫描电镜(SEM)对所得氧化石墨、氧化石墨烯分别进行表征。并对制备氧化石墨的3种化学氧化过程进行对比分析,结果表明,Hummers法在高温阶段有红色刺激性气体放出,且发生喷溅现象。硫酸/磷酸法和反应釜法是在低温条件下进行,制备过程比Hummers法安全、环保。氧化石墨XRD结果表明,3种化学氧化法中氧化程度最好的是硫酸/磷酸法,其次是反应釜法,最后是Hummers法。氧化石墨烯SEM结果表明,氧化石墨经超声处理后剥离成为氧化石墨烯纳米片。
The graphite oxide(GO) was prepared by three methods of Hummers,H_2SO_4/H_3PO_4 and Reactor,then the graphene oxide was synthesized by ultrasonic treatment,GO and graphene oxide were characterized by XRD and SEM.After prepared on three kinds of chemical oxidation process of graphite were analyzed.The result was showed that there are red excitant gas and splashing occur in high temperature stage of Hummers method,and sulfuric acid/phosphoric acid method and the reactor method was conducted in low temperature,so the preparation process was safer,more environmental protection than Hummers method.The XRD results of GO showed that the oxidation degree of the sulfuric acid/phosphoric acid method is the best of three methods of chemical oxidation,the second is the reactor method,the last is the Hummers method.The SEM results of graphene oxide showed that GO by stripped with ultrasonic treatment become graphene oxide of nano-films.
The graphite oxide(GO) was prepared by three methods of Hummers,H_2SO_4/H_3PO_4 and Reactor,then the graphene oxide was synthesized by ultrasonic treatment,GO and graphene oxide were characterized by XRD and SEM.After prepared on three kinds of chemical oxidation process of graphite were analyzed.The result was showed that there are red excitant gas and splashing occur in high temperature stage of Hummers method,and sulfuric acid/phosphoric acid method and the reactor method was conducted in low temperature,so the preparation process was safer,more environmental protection than Hummers method.The XRD results of GO showed that the oxidation degree of the sulfuric acid/phosphoric acid method is the best of three methods of chemical oxidation,the second is the reactor method,the last is the Hummers method.The SEM results of graphene oxide showed that GO by stripped with ultrasonic treatment become graphene oxide of nano-films.
引文
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[11] 傅玲,刘洪波,邹艳红,等.Hummers法制备氧化石墨时影响氧化程度的工艺因素研究[J].炭素,2005,124(4):10-14.
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[2] 张超,陈学康,郭磊,等.石墨烯太阳能电池透明电极的可行性分析[J].真空与低温,2012,18(3):160-166.
[3] 许婧,杨德志,廖小珍,等.还原氧化石墨烯/TiO2复合材料在钠离子电池中的电化学性能[J].物理化学学报,2015,31(5):913-919.
[4] 周雄,张枝风,陈丽君,等.石墨烯包覆SnO2空心球的制备及其锂离子电池负极性能[J].湖南理工学院学报:自然科学版,2014,27(2):35-39.
[5] 龚佑宁,黎德龙,张豫鹏,等.石墨烯及其复合材料在锂离子电池负极材料中的应用[J].材料导报,2015,29(7):33-38.
[6] 方建军,李素芳,查文珂,等.镀镍石墨烯的微波吸收性能[J].无机材料学报,2011,26(5):467-471.
[7] 李国显,王涛,薛海荣,等.石墨烯/Fe3O4复合材料的制备及电磁波吸收性能[J].航空学报,2011,32(9):1732-1739.
[8] 王立娜,陈成猛,杨永岗,等.氧化石墨烯-酚醛树脂薄膜的制备及性能研究[J].材料导报,2010,24(9):54-56.
[9] 杜彦,季铁正,张教强,等.石墨烯/高密度聚乙烯导电复合材料的制备与表征[J].航空材料学报,2013,33(1):68-71.
[10] Hummers W,Offeman R.Preparation of graphitic oxide[J].Journal of American Chemical Society,1958,80:1339.
[11] 傅玲,刘洪波,邹艳红,等.Hummers法制备氧化石墨时影响氧化程度的工艺因素研究[J].炭素,2005,124(4):10-14.
[12] Marcano D C,Kosynkin D V,Berlin J M,et al.Improved synthesis of graphene oxide[J].ACS Nano,2010,4(8):4806-4814.