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Cryo-transmission electron microscopy of Ag nanoparticles grown on an ionic liquid substrate

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Abstract

We report a novel method of growing silver nanostructures by cathodic sputtering onto an ionic liquid (IL) and our visualization by transmission cryo-electron microscopy to avoid beam-induced motion of the nanoparticles. By freezing the IL suspension and controlling electron dose, we can assess properties of particle size, morphology, crystallinity, and aggregation in situ and at high detail. We observed round silver nanoparticles with a well-defined diameter of 7.0 ± 1.5 nm that are faceted with crystalline cubic structures and ˜80% of the particles have multiply twinned faults. We also applied cryo-electron tomography to investigate the structure of the nanoparticles and to directly visualize the IL wetting around them. In addition to particles, we observed nanorods that appear to have assembled from individual nanoparticles. Reexamination of the samples after 4-5 days from initial preparation showed significant changes in morphology, and potential mechanisms for this are discussed.

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References

  1. K.S. Nagabhushana, H. Bönnemann: Wet chemical synthesis of nanoparticles Nanotechnology in Catalysis edited by B. Zhou, S. Hermans, and G.A. Somorjai Vol. 1 (Kluwer Academic/Plenum Press, New York 2004)51–82

    Article  CAS  Google Scholar 

  2. M. Niederberger, G. Garnweitner, J. Ba, J. Polleux, N. Pinna: Nonaqueous synthesis, assembly and formation mechanisms of metal oxide nanocrystals. Int. J. Nanotechnol.4263 (2007)

    Article  CAS  Google Scholar 

  3. P. Singh, A. Katyal, R. Kalra, R. Chandra: Copper nanoparticles in ionic liquid: An easy and efficient catalyst for the coupling of thiazolidine-2,4-dione, aromatic aldehyde and ammonium acetate. Catal. Commun.91618 (2008)

    Article  CAS  Google Scholar 

  4. J. Dupont, G.S. Fonseca, A.P. Umpierre, P.F. Fichtner, S.R. Teixeira: Transition-metal nanoparticles in imidazolium ionic liquids: Recyclable catalysts for biphasic hydrogenation reactions. J. Am. Chem. Soc.1244228 (2002)

    Article  CAS  Google Scholar 

  5. P. Singh, S. Kumarb, A. Katyala, R. Kalrac, R. Chandraa: A novel route for the synthesis of indium nanoparticles in ionic liquid. Mater. Lett.624164 (2008)

    Article  CAS  Google Scholar 

  6. Z-Y. Yan, Q. Liu, W-J. Zheng: Synthesis and characterization of titania powders from mixture of ionic liquid-water. Chin. J. Inorg. Chem.222055 (2006)

    CAS  Google Scholar 

  7. Y. Zhai, Y. Gao, F. Liu, Q. Zhang, G. Gao: Synthesis of nanostructured TiO2 particles in room temperature ionic liquid and its photocatalytic performance. Mater. Lett.615056 (2007)

    Article  CAS  Google Scholar 

  8. S. Chen, Y. Liu, G. Wu: Stabilized and size-tunable gold nanoparticles formed in a quaternary ammonium-based room-temperature ionic liquid under γ-irradiation. Nanotechnology162360 (2005)

    Article  CAS  Google Scholar 

  9. N. Li, B. Dong, W. Yuan, Y. Gao, L. Zheng, Y. Huang, S. Wang: ZrO2 nanoparticles synthesized using ionic liquid microemulsion. J. Dispersion Sci. Technol.281030 (2007)

    Google Scholar 

  10. X.L. Zhao, C-X. Wang, X-P. Hao, J-X. Yang, Y-Z. Wu, Y-P. Tian, X-T. Tao, M-H. Jiang: Synthesis of PbS nanocubes using an ionic liquid as the solvent. Mater. Lett.614791 (2007)

    Article  CAS  Google Scholar 

  11. Y. Jiang, Y.J. Zhu: Microwave-assisted synthesis of nanocrystalline metal sulfides using an ionic liquid. Chem. Lett.331390 (2004)

    Article  CAS  Google Scholar 

  12. X. Hou, F. Zhou, Y. Sun, W. Liu: Ultrasound-assisted synthesis of dentritic ZnO nanostructure in ionic liquid. Mater. Lett.611789 (2007)

    Article  CAS  Google Scholar 

  13. S.Z. El Abedin, N. Borissenko, F. Endres: Electrodeposition of nanoscale silicon in a room temperature ionic liquid. Electrochem. Commun.6510 (2004)

    Article  Google Scholar 

  14. D.M. Mattox Handbook of Physical Vapor Deposition Processing (Noyes Publication, Park Ridge, NJ 1998)

    Google Scholar 

  15. J.J. Finley: Development of a multilayer thin-film solar control windshield. J. Vac. Sci. Technol., A14739 (1996)

    Article  CAS  Google Scholar 

  16. J.J. Finley: Method of producing particles by physical vapor deposition in an ionic liquid. Inter. Pat. Appl. WO2007/084558A3 (2007)

    Google Scholar 

  17. K. Taylor, R.M. Glaeser: Electron microscopy of frozen-hydrated biological specimens. J. Ultrastruct. Res.55448 (1976)

    Article  CAS  Google Scholar 

  18. J. Frank: Single-particle imaging of macromolecules by cryo-electron microscopy. Annu. Rev. Biophys. Biomol. Struct.31303 (2002)

    Article  CAS  Google Scholar 

  19. E.M. Pouget, P.H. Bomans, J.A. Goos, P.M. Frederik, G. de With, N.A. Sommerdijk: The initial stages of template-controlled CaCO3 formation revealed by cryo-TEM. Science3231455 (2009)

    Article  CAS  Google Scholar 

  20. B. Leng, Z. Shao, P.H. Bomans, L.J. Brylka, N.A. Sommerdijk, G. de With, W. Ming: Cryogenic electron tomography reveals the template effect of chitosan in biomimetic silicification. Chem. Commun. (Camb.)461703 (2010)

    CAS  Google Scholar 

  21. A. Dey, G. de With, N.A. Sommerdijk: In situ techniques in biomimetic mineralization studies of calcium carbonate. Chem. Soc. Rev.39397 (2010)

    CAS  Google Scholar 

  22. Y. Wang, A. Neyman, E. Arkhangelsky, V. Gitis, L. Meshi, I.A. Weinstock: Self-assembly and structure of directly imaged inorganic-anion monolayers on a gold nanoparticle. J. Am. Chem. Soc.13117412 (2009)

    CAS  Google Scholar 

  23. Y. He, Z. Li, P.M. Simone, T.P. Lodge: Self-assembly of block copolymer micelles in an ionic liquid. J. Am. Chem. Soc.1282745 (2006)

    CAS  Google Scholar 

  24. P.M. Simone, T.P. Lodge: Micellization of PS-PMMA diblock copolymers in an ionic liquid. Macromol. Chem. Phys.208339 (2007)

    CAS  Google Scholar 

  25. G. Effantin, P. Boulanger, E. Neumann, L. Letellier, J.F. Conway: Bacteriophage T5 structure reveals similarities with HK97 and T4 suggesting evolutionary relationships. J. Mol. Biol.361993 (2006)

    CAS  Google Scholar 

  26. M.D. Abramoff, P.J. Magelhaes, S.J. Ram: Image processing with ImageJ. Biophotonics Int.1136 (2004)

    Google Scholar 

  27. J.R. Kremer, D.N. Mastronarde, J.R. McIntosh: Computer visualization of three-dimensional image data using IMOD. J. Struct. Biol.11671 (1996)

    CAS  Google Scholar 

  28. D.N. Mastronarde: Dual-axis tomography: An approach with alignment methods that preserve resolution. J. Struct. Biol.120343 (1997)

    Article  CAS  Google Scholar 

  29. D.J. Smith, L.D. Marks: High resolution studies of small particles of gold and silver: II. Single crystals, lamellar twins and polyparticles. J. Cryst. Growth54433 (1981)

    Article  CAS  Google Scholar 

  30. L.D. Marks, D.J. Smith: High resolution studies of small particles of gold and silver: I. Multiply-twinned particles. J. Cryst. Growth54425 (1981)

    Article  CAS  Google Scholar 

  31. Y. Gao, L. Song, P. Jiang, P. Liu, L.F. Yan, X.Q. Zhou, Z.P. Liu, D.F. Wang, J.X. Yuan, H.J. Zhang, Z.X. Zhao, X.W. Dou, X.Y. Zhou, W.Y. Wang, G. Xie, S. Chen, H.Y. Huan, J.Q. Li: Silver nanowires with five-fold symmetric cross-section. J. Cryst. Growth276606 (2004)

    Article  Google Scholar 

  32. P.A. Buffat: Electron diffraction and HRTEM studies of multiply-twinned structures and dynamical events in metal nanoparticles: Facts and artefacts. Mater. Chem. Phys.81368 (2003)

    Article  CAS  Google Scholar 

  33. C. Ni, P.A. Hassan, E.W. Kaler: Structural characteristics and growth of pentagonal silver nanorods prepared by a surfactant method. Langmuir213334 (2005)

    Article  CAS  Google Scholar 

  34. F.P. Booy, J.B. Pawley: Cryo-crinkling: What happens to carbon films on copper grids at low temperature. Ultramicroscopy48273 (1993)

    Article  CAS  Google Scholar 

  35. D.D. Williams, C.B. Carter Transmission Electron Microscopy: A Textbook for Materials Science (Plenum Press, New York 1996)

    Book  Google Scholar 

  36. M. Grouchko, I. Popov, V. Uvarov, S. Magdassi, A. Kamyshny: Coalescence of silver nanoparticles at room temperature: Unusual crystal structure transformation and dendrite formation induced by self-assembly. Langmuir252501 (2009)

    Article  CAS  Google Scholar 

  37. Z. Li, J. Zhang, J. Du, H. Gao, Y. Gao, T. Mu, B. Han: Synthesis of LaCO3OH nanowires via a solvothermal process in the mixture of water and room-temperature ionic liquid. Mater. Lett.59963 (2005)

    Article  CAS  Google Scholar 

  38. I. Kazeminezhad, A.C. Barnes, J.D. Holbrey, K.R. Seddon, W. Schwarzacher: Templated electrodeposition of silver nanowires in a nanoporous polycarbonate membrane from a nonaqueous ionic liquid electrolyte. Appl. Phys. A: Mater. Sci. Process.86373 (2007)

    Article  CAS  Google Scholar 

  39. D.S. Jacob, I. Genish, L. Klein, A. Gedanken: Carbon coated shell structured copper and nickel-nanoparticles synthesized in ionic liquid. J. Phys. Chem. B11017711 (2006)

    Article  CAS  Google Scholar 

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Author notes

  1. James F. Conway

    Present address: Imaging & Characterization Facility, King Abdullah University of Science and Technology (KAUST), Thuwal, Saudi Arabia

Authors and Affiliations

  1. Department of Structural Biology, University of Pittsburgh-School of Medicine, Pittsburgh, Pennsylvania, 15260, USA

    Dalaver H. Anjum & James F. Conway

  2. Imaging & Characterization Facility, King Abdullah University of Science and Technology (KAUST), Thuwal, Saudi Arabia

    Dalaver H. Anjum

  3. PPG Glass Business and Discovery Center, Cheswick, Pennsylvania, 15024, USA

    Rebecca M. Stiger & James J. Finley

Authors
  1. Dalaver H. Anjum
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  2. Rebecca M. Stiger
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  3. James J. Finley
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  4. James F. Conway
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Correspondence to James F. Conway.

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Anjum, D.H., Stiger, R.M., Finley, J.J. et al. Cryo-transmission electron microscopy of Ag nanoparticles grown on an ionic liquid substrate. Journal of Materials Research 25, 1264–1271 (2010). https://doi.org/10.1557/JMR.2010.0166

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  • DOI: https://doi.org/10.1557/JMR.2010.0166

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