An annealing process in reductive atmosphere of flowing H 2 /Ar improves the rate capability and cycling stability of electrodeposited MoO x film, which is favorable for its future application as micro-electrode for micro-supercapacitors. MoO 2 grains were found in the films annealed at temperatures above 350 • C, and the content of MoO 2 nanocrystallites was controlled by adjusting the annealing time. After annealing for 1.5 h at 350 • C, the 63 nm thick film exhibited the best electrochemical property, with a high volumetric capacitance of 594 F cm −3 at 20 mV s −1 , good rate capability with a relaxation time constant of 11 ms, and excellent cycling stability of 99% capacitance retention after 4000 cycles. This could be attributed to the combination of nanocrystalline MoO 2 , which is electronically conductive, and amorphous MoO x (x>2), which is pseudocapacitive in aqueous electrolyte.Miniaturized supercapacitors, or micro-supercapacitors (m-SCs), which possess the merits of conventional supercapacitors, i.e. fast power delivery and long cycle life, could play an important part in energy storage for micro-power systems such as self-powered sensors, microelectromechanical systems (MEMS), and portable electronics. 1-3 Much research has been recently devoted to exploring thin film electrode materials with superior. 4-8 According to the capacitive mechanism, there are two types of electrode materials, electrochemical double layer capacitor (EDLC) electrodes and pseudocapacitor electrodes which deliver charge through fast redox reactions. 9 As a representative of EDLC materials, carbon microelectrode, such as carbide-derived-carbon film, onion-like carbon microelectrode, and reduced grapheme oxide film, 1,6,7 could deliver charge at a fast rate; however, their specific capacitance is limited. Transition metal oxides are typical pseudocapacitive materials, which could potentially provide high specific capacitance thus high energy density. 2,8-10 However, the poor conductivity restrains their future application. The usual solution to overcome this disadvantage is to make composite microelectrode. For example, Si et al. prepared MnO x /Au multilayers by electron beam evaporation, which showed higher capacitance at a fast scan rate than the bare MnO x electrode does. 11 Shen et al. fabricated MnO 2 -based composite material following the synthesis methodology of conventional supercapacitors and injected it into the interdigital electrode channels. 10 However, compounding active materials and conductive additives requires either a more complicated fabrication process and higher cost, or produces unsatisfactory structural robustness and uniformity. To improve the conductivity by controlling the intrinsic composition of the pseudocapacitive materials could be another promising method. For example, nanocrystalline VN, with pseudocapacitive nano-layers of VO x on the electronically conducting VN grains, was found to be a superior electrode material. 12 MoO 3-x is pseudocapacitive in neutral or slightly acidic aqueous solut...