Freeze-drying, as a cryochemical powder processing method is applied in the synthesis of ZnO submicrometer to narrosized powders. The process involves rapid freezing of the sprayed precursor solution, drying under vacuum by sublimation of the Solvent and salt decomposition to oxide by thermal treatment. Calcination of dehydrated Zn(NO3)(2) was performed through destruction of the primary crystal structure, i.e. through accumulation of different defect complexes and based on this, the formation of a new state of the ZnO crystal lattice. An analysis of the microstructure evolution of zinc oxide particles in the temperature range from 548 to 898 K is described. The research was performed using differential scanning calorimetry (DSC), scanning electron microscopy (SEM), X-ray powder diffraction (XRPD), electronic paramagnetic resonance (EPR) and infrared spectroscopy (IR). It was shown that the least ("primary") coherent scattering region (580 Angstrom) and the most defective state were Zn...O obtained at the lowest calcination temperature (T-c = 548 K). Increase of the calcination temperature (T-c > 548 K) favors uniting of eight closest "primary" domains into "secondary" ones. Unification is accompanied by a pronounced increase in microstrainin "secondary" domains, whose size practically does not depend on the calcination temperature in the region 573-898 K.
TY - JOUR
AU - Marinković-Stanojević, Zorica
AU - Milošević, Olivera
AU - Nikolić, Maria Vesna
AU - Kakazey, MG
AU - Karpec, MV
AU - Tomila, TV
AU - Ristic, MM
PY - 2004
UR - http://rimsi.imsi.bg.ac.rs/handle/123456789/96
AB - Freeze-drying, as a cryochemical powder processing method is applied in the synthesis of ZnO submicrometer to narrosized powders. The process involves rapid freezing of the sprayed precursor solution, drying under vacuum by sublimation of the Solvent and salt decomposition to oxide by thermal treatment. Calcination of dehydrated Zn(NO3)(2) was performed through destruction of the primary crystal structure, i.e. through accumulation of different defect complexes and based on this, the formation of a new state of the ZnO crystal lattice. An analysis of the microstructure evolution of zinc oxide particles in the temperature range from 548 to 898 K is described. The research was performed using differential scanning calorimetry (DSC), scanning electron microscopy (SEM), X-ray powder diffraction (XRPD), electronic paramagnetic resonance (EPR) and infrared spectroscopy (IR). It was shown that the least ("primary") coherent scattering region (580 Angstrom) and the most defective state were ZnO obtained at the lowest calcination temperature (T-c = 548 K). Increase of the calcination temperature (T-c > 548 K) favors uniting of eight closest "primary" domains into "secondary" ones. Unification is accompanied by a pronounced increase in microstrainin "secondary" domains, whose size practically does not depend on the calcination temperature in the region 573-898 K.
PB - Elsevier Science Sa, Lausanne
T2 - Materials Science and Engineering A-Structural Materials Properties Microstructure and Processing
T1 - Evolution of the microstructure of disperse ZnO powders obtained by the freeze-drying method
EP - 624
SP - 620
VL - 375
DO - 10.1016/j.msea.2003.10.113
ER -
@article{
author = "Marinković-Stanojević, Zorica and Milošević, Olivera and Nikolić, Maria Vesna and Kakazey, MG and Karpec, MV and Tomila, TV and Ristic, MM",
year = "2004",
abstract = "Freeze-drying, as a cryochemical powder processing method is applied in the synthesis of ZnO submicrometer to narrosized powders. The process involves rapid freezing of the sprayed precursor solution, drying under vacuum by sublimation of the Solvent and salt decomposition to oxide by thermal treatment. Calcination of dehydrated Zn(NO3)(2) was performed through destruction of the primary crystal structure, i.e. through accumulation of different defect complexes and based on this, the formation of a new state of the ZnO crystal lattice. An analysis of the microstructure evolution of zinc oxide particles in the temperature range from 548 to 898 K is described. The research was performed using differential scanning calorimetry (DSC), scanning electron microscopy (SEM), X-ray powder diffraction (XRPD), electronic paramagnetic resonance (EPR) and infrared spectroscopy (IR). It was shown that the least ("primary") coherent scattering region (580 Angstrom) and the most defective state were ZnO obtained at the lowest calcination temperature (T-c = 548 K). Increase of the calcination temperature (T-c > 548 K) favors uniting of eight closest "primary" domains into "secondary" ones. Unification is accompanied by a pronounced increase in microstrainin "secondary" domains, whose size practically does not depend on the calcination temperature in the region 573-898 K.",
publisher = "Elsevier Science Sa, Lausanne",
journal = "Materials Science and Engineering A-Structural Materials Properties Microstructure and Processing",
title = "Evolution of the microstructure of disperse ZnO powders obtained by the freeze-drying method",
pages = "624-620",
volume = "375",
doi = "10.1016/j.msea.2003.10.113"
}
Marinković-Stanojević, Z., Milošević, O., Nikolić, M. V., Kakazey, M., Karpec, M., Tomila, T.,& Ristic, M.. (2004). Evolution of the microstructure of disperse ZnO powders obtained by the freeze-drying method. in Materials Science and Engineering A-Structural Materials Properties Microstructure and Processing
Elsevier Science Sa, Lausanne., 375, 620-624.
https://doi.org/10.1016/j.msea.2003.10.113
Marinković-Stanojević Z, Milošević O, Nikolić MV, Kakazey M, Karpec M, Tomila T, Ristic M. Evolution of the microstructure of disperse ZnO powders obtained by the freeze-drying method. in Materials Science and Engineering A-Structural Materials Properties Microstructure and Processing. 2004;375:620-624.
doi:10.1016/j.msea.2003.10.113 .
Marinković-Stanojević, Zorica, Milošević, Olivera, Nikolić, Maria Vesna, Kakazey, MG, Karpec, MV, Tomila, TV, Ristic, MM, "Evolution of the microstructure of disperse ZnO powders obtained by the freeze-drying method" in Materials Science and Engineering A-Structural Materials Properties Microstructure and Processing, 375 (2004):620-624,
https://doi.org/10.1016/j.msea.2003.10.113 . .
