Taguchi robust design to optimize synthesis of lead oxalate nano-disks

Disk-shaped lead oxalate nanoparticles were synthesized via sol-precipitation in aqueous media without any surfactant, template or catalyst. Significance of reaction conditions such as: lead and oxalate concentrations, flow rate of reagent addition and temperature of reactor on diameter of synthesized lead oxalate disk-shaped particles were investigated and optimized. The participation of the studied variables in the particle size control of lead oxalate was quantitatively evaluated by analysis of variance. The results showed that lead oxalate nano-disks can be synthesized via controlling effective procedure parameters. Under optimum conditions, disk shaped nano-sized lead oxalate particles with two dimensions (95 nm diameter and 35 nm thickness) were synthesized. The structure and morphology of the lead oxalate nano-disks obtained under optimum conditions of synthesis process were characterized by scanning electron microscopy, X-ray diffraction, infrared spectroscopy and thermal analysis techniques. The Thermal analysis of the nanoparticles obtained under optimum conditions indicates that the main thermal degradation of the nano-disks occurs in the temperature range of 310–380 °C; while, submicron particles decomposed exothermally in more wider temperature range of 320–430 °C.