Hydrothermal synthesis of nanocrystalline ZnSe: An in situ synchrotron radiation X-ray powder diffraction study

Jensen, T R; Hanson, J C

doi:10.1016/j.jssc.2008.04.026

Title: Hydrothermal synthesis of nanocrystalline ZnSe: An in situ synchrotron radiation X-ray powder diffraction study

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Abstract

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 showedmore »« less

Authors:

Jensen, T R ^[1]; Hanson, J C ^[2]

iNANO and Department of Chemistry, University of Aarhus, DK-8000 Arhus C (Denmark)
Chemistry Department, Brookhaven National Laboratory, Upton, NY 11973 (United States)

Publication Date:: Fri Aug 15 00:00:00 EDT 2008

OSTI Identifier:: 21128393

Resource Type:: Journal Article

Journal Name:: Journal of Solid State Chemistry

Additional Journal Information:: Journal Volume: 181; Journal 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); Journal ID: ISSN 0022-4596

Country of Publication:: United States

Language:: English

Subject:: 37 INORGANIC, 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

Citation Formats


                    Jorgensen, J.-E., Jensen, T R, and Hanson, J C. Hydrothermal synthesis of nanocrystalline ZnSe: An in situ synchrotron radiation X-ray powder diffraction study.  United States: N. p., 2008. 
        Web.  doi:10.1016/j.jssc.2008.04.026.

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                    Jorgensen, J.-E., Jensen, T R, & Hanson, J C. Hydrothermal synthesis of nanocrystalline ZnSe: An in situ synchrotron radiation X-ray powder diffraction study.  United States.  https://doi.org/10.1016/j.jssc.2008.04.026

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                    Jorgensen, J.-E., Jensen, T R, and Hanson, J C. 2008.  
        "Hydrothermal synthesis of nanocrystalline ZnSe: An in situ synchrotron radiation X-ray powder diffraction study".  United States.  https://doi.org/10.1016/j.jssc.2008.04.026.

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@article{osti_21128393,

  title        = {Hydrothermal synthesis of nanocrystalline ZnSe: An in situ synchrotron radiation X-ray powder diffraction study},

  author       = {Jorgensen, J.-E. and Jensen, T R and Hanson, J C},

  abstractNote = {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.},

  doi          = {10.1016/j.jssc.2008.04.026},

  url          = {https://www.osti.gov/biblio/21128393},
  journal      = {Journal of Solid State Chemistry},

  issn         = {0022-4596},

  number       = 8,

  volume       = 181,

  place        = {United States},

  year         = {Fri Aug 15 00:00:00 EDT 2008},

  month        = {Fri Aug 15 00:00:00 EDT 2008}

}

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