Key laboratory of Science and Technology of Eco-Textile, Ministry of Education, Jiangnan University, Wuxi, Jiangsu 214122, People's Republic of China.
Nanoscale Res Lett. 2014 Apr 9;9(1):172. doi: 10.1186/1556-276X-9-172.
A method for situ preparing a hybrid material consisting of silica nanoparticles (SiO2) attached onto the surface of functionalized graphene nanoplatelets (f-GNPs) is proposed. Firstly, polyacrylic acid (PAA) was grafted to the surface of f-GNPs to increase reacting sites, and then 3-aminopropyltriethoxysilane (APTES) KH550 reacted with abovementioned product PAA-GNPs to obtain siloxane-GNPs, thus providing reaction sites for the growth of SiO2 on the surface of GNPs. Finally, the SiO2/graphene nanoplatelets (SiO2/GNPs) hybrid material is obtained through introducing siloxane-GNPs into a solution of tetraethyl orthosilicate, ammonia and ethanol for hours' reaction. The results from Fourier transform infrared spectroscopy (FTIR) showed that SiO2 particles have situ grown on the surface of GNPs through chemical bonds as Si-O-Si. And the nanostructure of hybrid materials was characterized by scanning electron microscopy (SEM) and transmission electron microscopy (TEM). All the images indicated that SiO2 particles with similar sizes were grafted on the surface of graphene nanoplatelets successfully. And TEM images also showed the whole growth process of SiO2 particles on the surface of graphene as time grows. Moreover, TGA traces suggested the SiO2/GNPs hybrid material had stable thermal stability. And at 900°C, the residual weight fraction of polymer on siloxane-GNPs was about 94.2% and that of SiO2 particles on hybrid materials was about 75.0%. However, the result of Raman spectroscopy showed that carbon atoms of graphene nanoplatelets became much more disordered, due to the destroyed carbon domains during the process of chemical drafting. Through orthogonal experiments, hybrid materials with various sizes of SiO2 particles were prepared, thus achieving the particle sizes controllable. And the factors' level of significance is as follows: the quantity of ammonia > the quantity of tetraethyl orthosilicate (TEOS) > the reaction time.
提出了一种原位制备由附着在功能化石墨烯纳米片（f-GNPs）表面的二氧化硅纳米颗粒（SiO2）组成的杂化材料的方法。首先，将聚丙烯酸（PAA）接枝到 f-GNPs 的表面以增加反应位点，然后 3-氨丙基三乙氧基硅烷（APTES）KH550 与上述产物 PAA-GNPs 反应，得到硅氧烷-GNPs，从而为 SiO2 在 GNPs 表面的生长提供反应位点。最后，通过将硅氧烷-GNPs 引入正硅酸乙酯、氨和乙醇的溶液中反应数小时，得到 SiO2/石墨烯纳米片（SiO2/GNPs）杂化材料。傅里叶变换红外光谱（FTIR）的结果表明，SiO2 颗粒通过化学键 Si-O-Si 原位生长在 GNPs 的表面上。通过扫描电子显微镜（SEM）和透射电子显微镜（TEM）对杂化材料的纳米结构进行了表征。所有图像表明，SiO2 颗粒以相似的尺寸成功接枝在石墨烯纳米片的表面上。TEM 图像还显示了 SiO2 颗粒随时间在石墨烯表面上的整个生长过程。此外，TGA 痕迹表明 SiO2/GNPs 杂化材料具有稳定的热稳定性。在 900°C 下，硅氧烷-GNPs 上聚合物的残余重量分数约为 94.2%，杂化材料上 SiO2 颗粒的残余重量分数约为 75.0%。然而，拉曼光谱的结果表明，由于化学制图过程中碳域的破坏，石墨烯纳米片的碳原子变得更加无序。通过正交实验，制备了具有不同尺寸 SiO2 颗粒的杂化材料，从而实现了颗粒尺寸的可控性。各因素的显著水平如下：氨的量 > 正硅酸乙酯（TEOS）的量 > 反应时间。
