Dependence of morphology of nanostructured nickel and cobalt powders on synthesis conditions

P. Lapsina1, E. Kagakin2, A. Popova3, V. Dodonov4
1Kemerovo Scientific Center SB RAS, , Kemerovo, Soviet pr., 18, 650000
2Kuzbass State Technical University, Russia, Kemerovo, Vesennyaya str., 28, 650000
3Kemerovo Scientific Center SB RAS, Russia, Kemerovo, Soviet pr., 18, 650000; Institute of Coal Chemistry and Material Science SB RAS, Russia, Kemerovo, Soviet pr., 18, 650000
4Kemerovo State University, Russia, Kemerovo, Krasnаya str., 6, 650043
Abstract
The paper is devoted to study of the effect of synthesis conditions on size-characteristics of nanostructured nickel and cobalt powders obtained by chemical reduction of hardly soluble metal carbonates by hydrazine hydrate in aqua solutions. It is found that morphology of nanostructured metals is dependent on the synthesis conditions (concentration of the reducing agent, temperature, magnetic field). Nanocrystalline Co and Ni powders of were prepared by chemical process involving the reduction of sparingly soluble nickel and cobalt carbonates at 80 ºС with hydrazine hydrate as the reducing agent. Obtained gray solid particles were filtered, washed first with distilled water several times and finally with isopropyl alcohol to remove hydrazine and allowed to dry at room temperature. The sample was kept in glass-stoppered bottle. Microstructural evaluation was studied with Scanning Electron Microscopy (SEM) of JEOL model JSM-6390, elemental composition – by x-ray fluorescence analysis with an energy dispersive X-ray (EDX) analyzer (in conjunction with SEM). The samples’ structure was characterized by X-ray powder diffraction (XRD) using a BRUKER D8-Advance X-ray diffractometer (Fe-Kα radiation, λ=0.193604 nm) to identify the nanocrystalline state of the alloys and the phase of the crystalline grains. To calculate the crystallite size the Scherrer Formula was used. The functions of particles distribution on size were calculated from curves obtained by the method of small-angle X-ray scattering (SAXS) at characteristic Fe-emission. The reported study was supported by RFBR, research project No. 14-03-31648 mol_a.
Received: 27 March 2015   Revised: 16 October 2015   Accepted: 06 November 2015
Views: 72   Downloads: 23
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