The effects of the zinc salt precursors, the reaction temperature and the alkaline ratio b (b = [OH-]/[Zn 2+ ]) on the aqueous synthesis of ZnO nanocrystals were investigated. Depending on the type of the zinc precursor, Zn 5 (OH) 8 Cl 2 ·H 2 O or Zn 5 (OH) 8 (NO 3 ) 2 .2H 2 O lamellar phases were obtained at room temperature (20°C) when the alkaline ratio is lower (0.5 £ b £ 1, 6 £ pH £ 6.4). When the reaction temperature increased to 95°C, zinc hydroxide chloride monohydrate was obtained in one case whereas zinc oxide was formed in the other, and no lamellar phase of Zn 5 (OH) 8 (NO 3 ) 2 .2H 2 O was obtained. Thermal decomposition of the two lamellar phases was carried out and mainly showed that Zn 5 (OH) 8 (NO 3 ) 2 .2H 2 O was completely decomposed to ZnO when the annealed temperature reached~250°C while Zn 5 (OH) 8 Cl 2 ·H 2 O was totally transformed to ZnO at about 400°C, a higher comparative temperature that confirms the better thermal stability of the zinc hydroxide chloride monohydrate. Figure 8 FTIR spectra of lamellar phases: (A) CLP: at room temperature, (a) CLP after annealing up to 400°C. (B) NLP: at room temperature, (a) NLP after annealing up to 250 °C.