title: Synthesis and size characterization of silica nanospheres using sedimentation field-flow fractionation (SdFFF).
abstract: Silica nanoparticles were synthesized by a conventional emulsion polymerization by mixing ethanol, ammonium hydroxide, water and tetra ethyl orthosilicate (TEOS). A new reaction apparatus was assembled for a large scale synthesis of silica nanospheres in the laboratory, which was designed for uniform mixing of the reactants. The apparatus was equipped with a disc type agitator with six rectangular propellers. The new apparatus allowed high reproducibility in terms of the mean size and the size distribution of the silica nanoparticles with the relative standard deviation of less than about 6%. Sedimentation field-flow fractionation (SdFFF) was employed for determination of the size distribution of the silica nanoparticles. SdFFF provided size-based separation of the silica nanoparticles, with the retention time increasing with the size. When SdFFF analysis was repeated three times for the same sample, the standard deviation was less than 4%, showing reliability of SdFFF in size measurement. SdFFF seems to provide more accurate size distribution than DLS, particularly for those having broad and multimodal size distributions. Change in the agitation speed resulted in significant change in the mean diameter of the silica nanoparticles. Agitation speed of 400 rpm in 3 L reaction vessel yielded silica particles of about 100 nm in diameter, while at 200 rpm in 1 L vessel yielded those of about 500 nm.
authors.affiliation: Department of Chemistry, Hannam University, Daejeon 305-811, Korea.
authors.forename: Woon Jung
authors.initials: WJ
authors.lastname: Kim
authors.forename: Se Young
authors.initials: SY
authors.lastname: Ahn
authors.forename: Jai Hoon
authors.initials: JH
authors.lastname: Kim
authors.forename: Jong Han
authors.initials: JH
authors.lastname: Chun
authors.forename: Jong Shin
authors.initials: JS
authors.lastname: Yu
authors.forename: Euo Chang
authors.initials: EC
authors.lastname: Jung
authors.forename: Seungho
authors.initials: S
authors.lastname: Lee
mesh_terms: D003460:Crystallization / Q000379:methods*; D031521:Fractionation, Field Flow / Q000379:methods*; D046911:Macromolecular Substances / Q000737:chemistry; D008422:Materials Testing; D008968:Molecular Conformation; D054118:Nanospheres / Q000737:chemistry* / Q000648:ultrastructure*; D010316:Particle Size; D012822:Silicon Dioxide / Q000737:chemistry*; D013499:Surface Properties
chemical_list: D046911:Macromolecular Substances; D012822:Silicon Dioxide