Journal of Sol-Gel Science and Technology

, Volume 39, Issue 1, pp 25-36

In situ and simultaneous nanostructural and spectroscopic studies of ZnO nanoparticle and Zn-HDS formations from hydrolysis of ethanolic zinc acetate solutions induced by water

  • Valerie BrioisAffiliated withLURE, Centre Universitaire Paris-SudSynchrotron SOLEIL, L’Orme des Merisiers Email author 
  • , Christine GiorgettiAffiliated withLURE, Centre Universitaire Paris-Sud
  • , Elisabeth DartygeAffiliated withLURE, Centre Universitaire Paris-Sud
  • , Francois BaudeletAffiliated withSynchrotron SOLEIL, L’Orme des Merisiers
  • , Miriam S. TokumotoAffiliated withInstituto de Quimica, UNESPDepartamento de Engenharia Química, UFSCar
  • , Sandra H. PulcinelliAffiliated withInstituto de Quimica, UNESP
  • , Celso V. SantilliAffiliated withInstituto de Quimica, UNESP

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The simultaneous formation of nanometer sized zinc oxide (ZnO), and acetate zinc hydroxide double salt (Zn-HDS) is described. These phases, obtained using the sol-gel synthesis route based on zinc acetate salt in alcoholic media, were identified by direct characterization of the reaction products in solution using complementary techniques: nephelometry, in situ Small-Angle X-ray Scattering (SAXS), UV-Vis spectroscopy and Extended X-ray Absorption Fine Structures (EXAFS). In particular, the hydrolytic pathway of ethanolic zinc acetate precursor solutions promoted by addition of water with the molar ratio N=[H2O]/[Zn2+] = 0.05 was investigated in this paper. The aim was to understand the formation mechanism of ZnO colloidal suspension and to reveal the factors responsible for the formation of Zn-HDS in the final precipitates. The growth mechanism of ZnO nanoparticles is based on primary particle (radius ≈ 1.5 nm) rotation inside the primary aggregate (radius <3.5 nm) giving rise to an epitaxial attachment of particles and then subsequent coalescence. The growth of second ZnO aggregates is not associated with the Otswald ripening, and could be associated with changes in equilibrium between solute species induced by the superficial etching of Zn-HDS particles at the advanced stage of kinetic.


Quantum dots ZnO Particle formation and growth SAXS UV-Vis EXAFS Turbidity