Chain-like MoS 2 assemblies consisting of hexagonal MoS 2 nanoparticles (20-60 nm) have been successfully synthesized in a Triton X-100/cyclohexane/hexanol/water W/O reverse microemulsion in the presence of (NH 4 ) 2 MoS 4 as the molybdenum source and NH 2 OH·HCl as the reducing agent. The products were characterized by X-ray powder diffraction (XRD), transmission electron microscopy (TEM) and UV-vis diffuse reflectance absorption spectra. The influence of synthetic parameters such as acidity, water/oil ratio (ï· 0 ), aging time and annealing temperature on the formation of MoS 2 assemblies was investigated. TEM analysis showed that these synthetic factors played important roles in controlling the size of MoS 2 nanoparticles and the length of the chain-like MoS 2 assemblies. XRD analysis indicated that the well-crystallized MoS 2 nanoparticles could be obtained by annealing the precursors at 700ï°C for 2 h under a flow of N 2 atmosphere. In addition, the as-prepared chain-like MoS 2 nanoparticles exhibited excellent photocatalytic H 2 activity in Ru ( The family of layered transition metal chalcogenides, such as MoS 2 , WS 2 , has aroused considerable interest during the past decade because of their unique properties and potential applications in hydrodesulfurization, Mg 2+ and Li + batteries, and solar photocells [1][2][3][4]. Increasing attention is now being focused on their potential applications as promising candidates for Pt, a co-catalyst and as well as a catalyst in photocatalytic H 2 production [5,6]. As it is well known, MoS 2 is an indirect, narrow band gap semiconductor (E g =1.0-1.2 eV, covering the range of solar spectrum energy) with high stability against photocorrosion in solution [7]. The band gap of MoS 2 depends on its crystallinity, size and shape due to the quantum confinement effect. Therefore, considerable effort has been made to the synthesis of MoS 2 nanomaterials with desired size and morphology. This material can be prepared under hydrothermal, solvothermal, sonolysis, inverse micelle, and ï§-irradiation conditions [8][9][10][11][12]. Among the methods, the inverse micelle synthesis has been proven to be a convenient, effective and promising method to regulate the size and morphology of MoS 2 . In this approach, particles are grown inside inverse micelle cages dispersed in non-aqueous solvents. The particle size and morphology of MoS 2 crystals can be tailored through controlling the micelle size, which can be easily achieved by changing the emulsifier/water ratio. For example, Wilcoxon et al. [13,14] synthesized the nanosized MoS 2 crystals as small as 2.5 and 4 nm in EHAB/hexanol/octane and TDAB/hexanol/octane micelle solutions. Chikan et al. [15] obtained MoS 2 nanocrystals with the size of 3.5, 4.5 and 8 nm in DDAB/hexanol/ octane and TDAI/hexanol/octane ternary micelles, respectively. Osseo-Asare and co-workers [11] got MoS 2 nanoparticles ranging 10-80 nm in NP-5/cyclohexane/water microemulsion system. Xie and co-workers [16] fabricated necklace-shaped assembly of fullerene-like Mo...