World Journal of Engineering THERMOSTIMULATED SYNTHESIS OF MoO3 AND WXMo1-XO3 NANO- AND MICROSCALE PARTICLES AND THEIR APPLICATION FOR DEPOSITION OF Ni-OXIDE COMPOSITES T.V. Sviridova1, L.I. Stepanova2, D.V. Sviridov 1 1 Chemistry Department of Belarusian State University, e-mail: sviridov@bsu.by 2 Institute for Physico- Chemical Problems of Belarusian State University, e-mail: stepanovali@bsu.by Leningradskaya str., 14, Minsk, 2200030, Belarus One of the challenges of modern synthetic chemistry is elaboration of effective approaches to preparation of nano- and microparticles, in particular, oxide and oxide-hydroxide nano- and micro-phases. The considerable progress in this direction was attained in recent years through using thermostimulated polymerization of oxo-acids, which opens the possibility of obtaining wide range of metastable compounds and permits one to exert an effective control over the characteristics of resultant crystals. Here we demonstrate the possibility of synthesis of nanometer- and micron-sized particles of molybdenum trioxide and molybdenum-tungsten mixed oxides in aqueous medium and discuss their applicability for electrochemical deposition of metal-matrix composites with different tribological properties. These studies evidenced that the change of synthetic conditions is a powerful tool for controlling the polycondensation process that in its turn allows regulation of structural characteristics and relative stability of precursors of growing oxide phase. In the case of molybdic acid, which exhibit low rate of oxolation and rather long induction period of solid phase growth, it is possible to “freeze” MoO3 nuclei at different stages of growing and ripening by changing the concentration of mature solution and to perform there growing and recrystallization at further synthetic steps. As a result, a wide range of molybdenum trioxide particles of different structure and dispersity can be produced including spherical nanoparticles, needles or perfect prisms of hexagonal MoO3(fig. 1). 1429 Fig. 1 SEM images of MoO3 particles of different shapes: (a) nanosized spherolites, (b) micron-sized prisms, (c) micron-sized needles Particles of mixed oxide WxMo1-xO3 can similarly be obtained using the process of two-step thermostimulated polycondensation. The solid product of the reaction is not a mechanical mixture of tungsten and molybdenum oxides, with Mo:W ratio in the mixed oxide and in the precursor being the same. The XRD analysis has revealed that solid solutions are formed, the lattice parameters being close to those of the prevailing oxide. When percentages of World Journal of Engineering molybdenum and tungsten in the precursor are Being added to a nickel plating bath, approximately the same, the product of the reaction both MoO3 and WxMo1-xO3 particles cois a mixed oxide with the composition W0.4Mo0.6O3. deposit with nickel yielding composite Thus synthesized particles of mixed oxide are coatings. Pronounced redox activity inherent spindle-shaped (fig. 2) and their size is determined in MoO3 and WxMo1-xO3 creates favorable by composition of precursor and exhibits increase condition for electrochemical codeposition as the molybdenum content in the reaction product with nickel and provides rapid and effective increases overgrowing of incorporated particles by matrix metal. The oxide loading varies within 1-12 wt. % being dependent on the oxide concentration in the electrolyte, particle size and plating conditions. At high concentrations of oxide in the plating bath the deposition rate exhibits decrease, whereas at modest concentrations (0.1-3.0 g/l) the rate of composite growth is not affected by the presence of the oxide particles in the plating solution. Wear resistance of the composite coatings obtained through embedment of MoO3 and WxMo1-xO3 particles in the nickel matrix even in rather low incorporation degree (1-4 wt. %) exceeds wear resistance of bare nickel coatings by 7-10 times. Metal-oxide composite coatings of antifrictional or frictional types (with friction coefficient 0.15 and 0.4, respectively) can be deposited depending on the size of the particles, their morphology and concentration in the plating bath. The distinctive feature of Ni-MoO3 (WxMo1-xO3) composites is the fact that they preserve the antifriction properties and stability at the enhanced temperatures (up to 500 oC) and remains stable under conditions of oxidation wearing. Acknowledgements: This work was supported by Basic Research Foundation of Belarus. References 1. Stepanova L.I., Mozolevskaya T.V., Bodrykh T.I., Sviridov V.V. Composite Films Nickel-Ultradispersed Oxide of Molybdenum or Tungsten Electrochemical Forming in Water Solutions // Reports of Belorussian National Academy of Sciences. 2002. № 2. P. 5-11 (in Russ). 2. Sviridova T.V., Stepanova L.I., Fig. 2 TEM images of WxMo1-xO3 Sviridov D.V. Nano- and Microcrystals of particles of different shapes: (a) aggregates of Molybdenum Trioxide and Metal-Matrix nanoneedles, (b) submicron-sized and (c) micronComposites on Their Basis In: “Molybdenum: sized spindle-like crystalites, synthesized by Characteristics, Production and Applications”. thermoinduced polycondensation of tungsticNY: Nova Science Publisher Inc., 2011. molybdic acid used as the precursor. 1430