Hollow Sn and Pb nanoparticles have been prepared by a rapid injection of an aqueous solution of SnCl2-poly(vinylpyrrolidone) (PVP, surfactant) and Pb(OAc)2·3H2O-PVP into an aqueous solution of sodium borohydride (reducing agent) in simple, one-pot reaction at room temperature under an argon atmosphere, respectively. The two hollow nanoparticles have been fully characterized by TEM, HRTEM, SAED, XRD, and EDX analyses. Upon exposure to air, the black Pb hollow nanoparticles are gradually transformed into a mixture of Pb, litharge (tetragonal PbO), massicot (orthorhombic PbO), and Pb5O8. The order and speed of mixing of the reactants between the metal precursor-PVP and the reductant solutions and stoichiometry of all the reactants are crucial factors for the formation of the two hollow nanocrystals. The Sn and Pb hollow nanoparticles were produced only when 1 :(1.5-2) and 1:3 ratios of the Sn and Pb precursors to NaBHt were employed with a rapid injection, respectively.
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