Department of Energy, Environmental and Chemical Engineering, Washington University in St. Louis, MO 63130, USA.
Department of Energy, Environmental and Chemical Engineering, Washington University in St. Louis, MO 63130, USA; Department of Chemical and Environmental Engineering, Yale University, CT 06520, USA.
J Colloid Interface Sci. 2021 Apr 15;588:725-736. doi: 10.1016/j.jcis.2020.11.102. Epub 2020 Nov 30.
Herein, we describe the synthesis of graphene oxide (GO) over a large range of conditions, exploring the effects of reaction temperature, reaction time, oxidant ratio, and sonication time on the chemical and colloidal properties of the product. As a function of reaction parameters, modified from Hummers' method, GO products were characterized and described via a suite of spectroscopic, structural, and morphological techniques, including TEM, UV-vis spectroscopy, XPS, Raman spectroscopy, FTIR, and DLS. Average carbon oxidation state and the yield (upon sonication) were chosen as the two criteria to evaluate synthesized GO materials. It was observed that as reaction temperature increased, GO oxidation state and yield of the sonication step both increased. Further, increasing reaction time and oxidant ratio not only increased the oxidation state, but also had a pronounced effect on the final yield. As synthesized, GO with higher degrees of oxidization exhibited higher negative ζ-potential, slightly smaller hydrodynamic diameter, and higher critical coagulation concentration(s). Data sets collectively demonstrate that carbon oxidation state, functional group ratios, and the aggregation kinetics of GO products can be readily controlled by varying processing time and conditions with expected changes in aqueous behavior(s), including stability/aggregation.
在此,我们描述了在大范围条件下合成氧化石墨烯(GO)的过程,探索了反应温度、反应时间、氧化剂比和超声时间对产物化学和胶体性质的影响。通过对 Hummers 法的修改,作为反应参数的函数,GO 产物通过一系列光谱、结构和形态学技术进行了表征和描述,包括 TEM、UV-vis 光谱、XPS、拉曼光谱、FTIR 和 DLS。平均碳氧化态和产率(超声后)被选为评估合成 GO 材料的两个标准。结果表明,随着反应温度的升高,GO 的氧化态和超声步骤的产率都增加了。此外,增加反应时间和氧化剂比不仅增加了氧化态,而且对最终产率也有显著影响。合成的 GO 具有较高的氧化度,表现出较高的负 ζ 电位、稍小的水动力直径和更高的临界聚集浓度(s)。数据集共同表明,通过改变处理时间和条件,可以很容易地控制碳氧化态、官能团比以及 GO 产物的聚集动力学,预期会改变其在水溶液中的行为,包括稳定性/聚集。