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Kinetic Precipitation of Solution-Phase Polyoxomolybdate Followed by Transmission Electron Microscopy: A Window to Solution-Phase Nanostructure

  1. Yan Zhu Dr.1,
  2. Arthur Cammers-Goodwin Prof. Dr.1,
  3. Bin Zhao2,
  4. Alan Dozier Dr.3,
  5. Elizabeth C. Dickey Prof. Dr.4

Article first published online: 22 MAR 2004

DOI: 10.1002/chem.200305468

Issue

Chemistry - A European Journal

Chemistry - A European Journal

Volume 10, Issue 10, pages 2421–2427, May 17, 2004

Additional Information

How to Cite

Zhu, Y., Cammers-Goodwin, A., Zhao, B., Dozier, A. and Dickey, E. C. (2004), Kinetic Precipitation of Solution-Phase Polyoxomolybdate Followed by Transmission Electron Microscopy: A Window to Solution-Phase Nanostructure. Chemistry - A European Journal, 10: 2421–2427. doi: 10.1002/chem.200305468

Author Information

  1. 1

    University of Kentucky, Chemistry Department, Lexington, KY 40506-0055, USA, Fax: (+1) 859 323-1069

  2. 2

    University of California Riverside, Department of Chemistry, Riverside, CA 92521-0403, USA

  3. 3

    University of Kentucky, Chemical and Materials Engineering, A004 ASTeCC Bldg, Lexington, KY 40506-0286, USA

  4. 4

    Pennsylvania State University, Department of Materials Science and Engineering, 195 MRI Bldg. University Park, PA 16802, USA

Publication History

  1. Issue published online: 7 MAY 2004
  2. Article first published online: 22 MAR 2004
  3. Manuscript Received: 20 AUG 2003

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Keywords:

  • electron microscopy;
  • molecular recognition;
  • nanostructures;
  • phase transitions;
  • polyanions

Graphical Abstract

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The structural nature of the polydisperse, nanoscopic components is elucidated both in the solution and the solid states of partially reduced polyoxomolybdate (see picture) derived from the {Mo132} keplerate, {(Mo)Mo5}12-{Mo2 acetate}30.

Abstract

This study aimed to elucidate the structural nature of the polydisperse, nanoscopic components in the solution and the solid states of partially reduced polyoxomolybdate derived from the {Mo132} keplerate, {(Mo)Mo5}12-{Mo2 acetate}30. Designer tripodal hexamine-tris-crown ethers and nanoscopic molybdate coprecipitated from aqueous solution. These microcrystalline solids distributed particle radii between 2–30 nm as assayed by transmission electron microscopy (TEM). The solid materials and their particle size distributions were snap shots of the solution phase. The mother liquor of the preparation of the {Mo132} keplerate after three days revealed large species (r=20–30 nm) in the coprecipitate, whereas {Mo132} keplerate redissolved in water revealed small species (3–7 nm) in the coprecipitate. Nanoparticles of coprecipitate were more stable than solids derived solely from partially reduced molybdate. The TEM features of all material analyzed lacked facets on the nanometer length scale; however, the structures diffracted electrons and appeared to be defect-free as evidenced by Moiré patterns in the TEM images. Moiré patterns and size-invariant optical densities of the features in the micrographs suggested that the molybdate nanoparticles were vesicular.

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