Hydrothermal synthesis of nanocrystalline ZnSe: An in situ synchrotron radiation X-ray powder diffraction study
- iNANO and Department of Chemistry, University of Aarhus, DK-8000 Arhus C (Denmark)
- Chemistry Department, Brookhaven National Laboratory, Upton, NY 11973 (United States)
The hydrothermal synthesis of nanocrystalline ZnSe has been studied by in situ X-ray powder diffraction using synchrotron radiation. The formation of ZnSe was studied using the following starting mixtures: Zn+Se+H{sub 2}O (route A) and ZnCl{sub 2}+Se+H{sub 2}O+Na{sub 2}SO{sub 3} (route B). The route A experiment showed that Zn powder starts reacting with water at 134 deg. C giving ZnO and H{sub 2} followed by the formation of ZnSe which takes place in temperature range from 167 to 195 deg. C. The route B experiment shows a considerably more complex reaction path with several intermediate phases and in this case the formation of ZnSe starts at 141 deg. C and ZnSe and Se were the only crystalline phases observed at the end of the experiment where the temperature was 195 deg. C. The sizes of the nanocrystalline particles were determined to 18 and 9 nm in the route A and B experiments, respectively. Nanocrystalline ZnSe was also synthesized ex situ using the route A and B methods and characterized by conventional X-ray powder diffraction and transmission electron microscopy. An average crystalline domain size of ca. 8 nm was determined by X-ray powder diffraction in fair agreement with TEM images, which showed larger aggregates of nanoparticles having approximate diameters of 10 nm. Furthermore, a method for purification of the ZnSe nanoparticles was developed and the prepared particles showed signs of anisotropic size broadening of the diffraction peaks. - Graphical abstract: Stack of powder diagrams showing the formation of nanocrystalline ZnSe under hydrothermal conditions.
- OSTI ID:
- 21128393
- Journal Information:
- Journal of Solid State Chemistry, Vol. 181, Issue 8; Other Information: DOI: 10.1016/j.jssc.2008.04.026; PII: S0022-4596(08)00199-0; Copyright (c) 2008 Elsevier Science B.V., Amsterdam, The Netherlands, All rights reserved; Country of input: International Atomic Energy Agency (IAEA); ISSN 0022-4596
- Country of Publication:
- United States
- Language:
- English
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Related Subjects
ORGANIC
PHYSICAL AND ANALYTICAL CHEMISTRY
ANISOTROPY
CRYSTALS
HYDROTHERMAL SYNTHESIS
NANOSTRUCTURES
PARTICLES
PURIFICATION
SYNCHROTRON RADIATION
TEMPERATURE RANGE 0273-0400 K
TEMPERATURE RANGE 0400-1000 K
TRANSMISSION ELECTRON MICROSCOPY
X-RAY DIFFRACTION
ZINC CHLORIDES
ZINC OXIDES
ZINC SELENIDES