Preparation of metallic bismuth by reduction of bismuth formates in ethylene glycol medium

Institute of Solid State Chemistry and Mechanochemistry, SBRAS, 630128, Novosibirsk, Russia

^一 Correspondingauthor: mishenko.k@solid.nsc.ru

Abstract

Nano -and microcrystalline bismuth metal powders consisting of spherical particles with a size of 150-250 nm were obtained by reducing bismuth formates in an ethylene glycol medium. The phase composition and morphology of the obtained reaction products were studied by X-ray phase and thermal analysis, differential scanning calorimetry, scanning and transmission electron microscopy. Using Uv-vis, it was shown that a bismuth-ethylene glycol complex is formed with an absorption maximum at 249 nm and an extinction coefficient of 5.7×10³ (L mol^-1 cm^-1) in a solution of chloric acid at 23°C. The concentration of bismuth enhances to 0.018 g L^-1 in the ethylene glycol medium with a gradual increase in the temperature to 60°C of the reaction mixture. Thermolysis of bismuth glycolate with a composition of Bi₂(OCH₂CH₂O)₃ is accompanied by the formation of metallic bismuth at 190°C, which is oxidized to a monoclinic modification of bismuth oxide when the temperature increases in the air.