Zarska Sandra, Kulawik Damian, Pavlyuk Volodymyr, Tomasik Piotr, Bachmatiuk Alicja, Szukiewicz Rafał, Ciesielski Wojciech
Faculty of Science and Technology, Institute of Chemistry, Jan Dlugosz University in Czestochowa, 42-200 Czestochowa, Poland.
Nantes Nanotechnological Systems, 59-700 Boleslawiec, Poland.
Materials (Basel). 2021 Jun 8;14(12):3161. doi: 10.3390/ma14123161.
The bromination of multi-walled carbon nanotubes (MWCNT) was performed with vapor bromine in a closed vessel, and they were subjected to intensive stirring with a magnetic stirrer for up to 14 days. The efficiency of bromination was compared depending upon duration. The structure and surface of the crude and purified products were characterized by detailed physicochemical analyses, such as SEM/EDS, TEM, XRD, TGA, Raman, and XPS spectroscopies. The studies confirmed the presence of bromine covalently bound with nanotubes as well as the formation of inclusion MWCNT-Br complexes. It was confirmed that Br molecules are absorbed on the surface of nanotubes (forming the CNT-Br complex), while they can dissociate close to dangling bonds at CNT defect sites with the formation of covalent C-Br bonds. Thus, any covalent attachment of bromine to the graphitic surface achieved around room temperature is likely related to the defects in the MWCNTs. The best results, i.e., the highest amount of attached Br, were obtained for brominated nanotubes brominated for 10 days, with the content of covalently bound bromine being 0.68 at% (by XPS).
在密闭容器中用气态溴对多壁碳纳米管（MWCNT）进行溴化处理，并使用磁力搅拌器进行长达14天的剧烈搅拌。根据持续时间比较溴化效率。通过详细的物理化学分析，如扫描电子显微镜/能谱仪（SEM/EDS）、透射电子显微镜（TEM）、X射线衍射仪（XRD）、热重分析仪（TGA）、拉曼光谱仪和X射线光电子能谱仪（XPS）对粗产物和纯化产物的结构及表面进行表征。研究证实了溴与纳米管共价结合的存在以及包合物MWCNT-Br配合物的形成。已证实Br分子吸附在纳米管表面（形成CNT-Br配合物），同时它们可在CNT缺陷位点靠近悬空键处解离，形成共价C-Br键。因此，在室温左右实现的溴与石墨表面的任何共价连接可能与MWCNT中的缺陷有关。对于溴化10天的溴化纳米管，获得了最佳结果，即附着的Br量最高，共价结合溴的含量为0.68原子百分比（通过XPS）。
