Vasi Sebastiano, Giofrè Salvatore Vincenzo, Perathoner Siglinda, Mallamace Domenico, Abate Salvatore, Wanderlingh Ulderico
Department of Mathematical and Computational Science, Physical Science and Earth Science, University of Messina, Viale F. Stagno D'Alcontres 31, I-98166 Messina, Italy.
Department of Chemical, Biological, Pharmaceutical and Environmental Sciences, University of Messina, Viale Ferdinando Stagno D'Alcontres 31, I-98166 Messina, Italy.
Materials (Basel). 2024 Aug 6;17(16):3887. doi: 10.3390/ma17163887.
An X-ray analysis of exfoliated MoS, produced by means of microwave-assisted liquid-phase exfoliation (LPE) from bulk powder in 1-methyl-2-pyrrolidone (NMP) or acetonitrile (ACN) + 1-methyl-2-pyrrolidone (NMP) solvents, has revealed distinct structural differences between the bulk powder and the microwave-exfoliated samples. Specifically, we performed X-ray diffraction (XRD) and X-ray photoelectron spectroscopy (XPS) measurements to identify the elements of our exfoliated sample deposited on a Si substrate by drop-casting, as well as their chemical state and its structural crystalline phase. In the exfoliated sample, the peaks pattern only partially resemble the theoretical Miller indices for MoS. In contrast, the bulk powder's spectrum shows the characteristic peaks of the 2H polytype of MoS, but with some broadening. Notable is the retention of partial crystallinity in the post-exfoliation phases, specifically in the normal-to-plane orientation, thus demonstrating the effectiveness of microwave-assisted techniques in producing 2D MoS and attaining desirable properties for the material. XPS measurements confirm the success of the exfoliation procedure and that the exfoliated sample retains its original structure. The exfoliation process has been optimized to maintain the structural integrity of MoS while enhancing its surface area and electrochemical performance, thereby making it a promising material for advanced electronic and optoelectronic applications ranging from energy storage to sensing devices under ambient conditions.
通过微波辅助液相剥离（LPE）从块状粉末在1-甲基-2-吡咯烷酮（NMP）或乙腈（ACN）+1-甲基-2-吡咯烷酮（NMP）溶剂中制备的剥离MoS₂的X射线分析揭示了块状粉末与微波剥离样品之间明显的结构差异。具体而言，我们进行了X射线衍射（XRD）和X射线光电子能谱（XPS）测量，以识别通过滴铸沉积在硅衬底上的剥离样品的元素，以及它们的化学状态及其结构结晶相。在剥离样品中，峰型仅部分类似于MoS₂的理论密勒指数。相比之下，块状粉末的光谱显示出MoS₂的2H多型的特征峰，但有一些展宽。值得注意的是，在剥离后阶段保留了部分结晶度，特别是在垂直于平面的方向上，从而证明了微波辅助技术在制备二维MoS₂和获得该材料所需性能方面的有效性。XPS测量证实了剥离过程的成功，并且剥离样品保留了其原始结构。剥离过程已经过优化，以保持MoS₂的结构完整性，同时提高其表面积和电化学性能，从而使其成为从能量存储到环境条件下传感设备等先进电子和光电子应用的有前途的材料。
