本研究以氧化還原法製備石墨烯,探討三種氧化方法(Hummers法、Modified Hummers法及Tour''s Improved法)所製得氧化石墨的氧化程度及結構分析,再經由本研究所設計的三步還原法還原氧化石墨,試圖製備出低含氧基團的石墨烯,並以石墨烯作為補強材,以溶液法製備石墨烯/聚乳酸奈米複合材料,同時探討石墨烯在聚乳酸奈米複合材料中對熱性質、機械性質及電性質的補強效應。由XRD分析中發現, Hummers法製備之氧化石墨仍有原始石墨之訊號。進一步的還原石墨烯,由XPS中C1s的分峰可發現還原石墨烯中含氧基團的含量明顯降低。在石墨烯/聚乳酸奈米複合材料的熱裂解分析中可得知石墨烯/聚乳酸奈米複合材料仍屬於一級裂解,且石墨烯在聚乳酸的裂解過程中能擔任催化劑的角色。由非等溫結晶動力中可得知填加石墨烯能增加聚乳酸結晶長成的速率,但並不會影響其結晶的晶型。
In this study, the graphene was prepared by chemical oxidation and reduction reaction. The graphite oxide was prepared by Hummers, modified Hummers and Tour''s Improved methods. The degree of oxidation and structure of graphite oxide were investigated by XRD, XPS, Raman spectrum, and TGA. In reduction reaction stage, we design a synthetic strategy (triple step reaction) to prepare the graphene with low oxide content. The graphene/polylactide composites were fabricated through solvent method. The thermal and mechanical properties, nonisothermal crystallization kinetics, and the conductivity of the composites were investigated. The XRD analysis revealed that the Hummers method cannot oxidize graphite to graphite oxide completely. The C1s peak in the XPS analysis indicated that the oxide content was decreased for the graphene obtained after the triple step reaction. The thermal degradation analysis revealed that the degradation behavior of graphene/polylactide composites was first order reaction, and graphene could be the catalyst of the degradation reaction. The results of nonisothermal crystallization kinetics indicated that graphene can accelerate the crystallization rate of polylactide, but would not affect the type of crystallization.