In this work, we report a hybrid architecture of layered MoS₂/graphene synthesized by an ultrasonic-assisted hydrothermal method at 230°C with a reaction time of 2 h. The microstructure, morphology, chemical composition and optical properties of MoS₂/graphene were analyzed by x-ray diffraction, field emission scanning electron microscope (FESEM), high resolution transmission electron microscope (HRTEM), Raman spectroscopy, hard x-ray photoelectron spectroscopy (HAXPES), energy dispersive x-ray (EDX) spectroscopy and photoluminescence measurements. The FESEM results show that the ultrathin MoS₂ nanosheets directly deposited on the surfaces of graphene sheets with high density and uniform shape. The TEM and HRTEM images indicate that MoS₂ nanosheets with average thickness of ∼ 3–6 nm (6–8 layers) grow vertically on the graphene surface, forming three-dimensional MoS₂/graphene hybrid structures. Both XRD and Raman analyses elucidate that the as-grown MoS₂ phase of MoS₂/graphene composite crystalized in a hexagonal phase (2H-MoS₂) with low impurity, which was later confirmed by the HAXPES and EDX. Interestingly, the D-band in the Raman spectrum of MoS₂/graphene hybrid samples almost disappears as the 2D-band arises, revealing that defects in the graphene oxide are well repaired under the hydrothermal process. Furthermore, the as-synthesized MoS₂/graphene exhibits strong photoluminescence with separately resolved emission peaks in the visible range (∼ 1.75–1.78 eV, ∼ 1.89–1.93 eV and ∼ 1.99–2.05 ,eV) which is a signature of mid-gap states in their optical bandgap compare to that of as-synthesized MoS₂. Our synthesis approach is favorable for easy and low-cost preparation of MoS₂/graphene composite, rendering the material attractive for various optoelectronic and catalysis applications.

在这项工作中，我们报告了通过超声辅助水热法在230°C的反应时间为2 h的条件下合成的MoS ₂ /石墨烯层状混合体系。通过X射线衍射，场发射扫描电子显微镜（FESEM），高分辨率透射电子显微镜（HRTEM），拉曼光谱，硬X射线光电子能谱分析了MoS ₂ /石墨烯的微观结构，形貌，化学组成和光学性质。（HAXPES），能量色散X射线（EDX）光谱和光致发光测量。FESEM结果表明，超薄MoS ₂纳米片直接沉积在石墨烯片表面，具有高密度和均匀形状。TEM和HRTEM图像表明MoS ₂纳米片的平均厚度约为3–6 nm（6-8层），在石墨烯表面垂直生长，形成三维MoS ₂ /石墨烯杂化结构。XRD和拉曼分析均阐明了MoS ₂ /石墨烯复合物的MoS ₂相生长态是在具有低杂质的六方相（2H-MoS ₂）中结晶的，后来被HAXPES和EDX证实。有趣的是，随着2 D带的出现，MoS ₂ /石墨烯杂化样品的拉曼光谱中的D带几乎消失，这表明氧化石墨烯的缺陷在水热过程中得到了很好的修复。此外，合成后的MoS ₂石墨烯/石墨烯具有很强的光致发光特性，在可见光范围内分别分辨出发射峰（〜1.75–1.78 eV，〜1.89–1.93 eV和〜1.99–2.05 eV），这是其光学带隙中带隙状态的标志合成的MoS _2的数量。我们的合成方法有利于轻松，低成本地制备MoS ₂ /石墨烯复合材料，使该材料对各种光电和催化应用具有吸引力。