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Novel MEMS-Based Gas-Cell/Heating Specimen Holder Provides Advanced Imaging Capabilities for In Situ Reaction Studies

  • Lawrence F. Allard (a1), Steven H. Overbury (a1), Wilbur C. Bigelow (a2), Michael B. Katz (a2), David P. Nackashi (a3) and John Damiano (a3)...
Abstract
Abstract

In prior research, specimen holders that employ a novel MEMS-based heating technology (AduroTM) provided by Protochips Inc. (Raleigh, NC, USA) have been shown to permit sub-Ångström imaging at elevated temperatures up to 1,000°C during in situ heating experiments in modern aberration-corrected electron microscopes. The Aduro heating devices permit precise control of temperature and have the unique feature of providing both heating and cooling rates of 106°C/s. In the present work, we describe the recent development of a new specimen holder that incorporates the Aduro heating device into a “closed-cell” configuration, designed to function within the narrow (2 mm) objective lens pole piece gap of an aberration-corrected JEOL 2200FS STEM/TEM, and capable of exposing specimens to gases at pressures up to 1 atm. We show the early results of tests of this specimen holder demonstrating imaging at elevated temperatures and at pressures up to a full atmosphere, while retaining the atomic resolution performance of the microscope in high-angle annular dark-field and bright-field imaging modes.

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Corresponding author
Corresponding author. E-mail: allardLFjr@ornl.gov
References
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Allard L.F., Bigelow W.C., Blom D.A. & Liu J. (2011). A stable double-tilt heating capability for precision atomic-level imaging of catalysts at elevated temperatures. Microsc Microanal 17(S2), 468469.
Allard L.F., Bigelow W.C., Jose-Yacaman M., Nackashi D.P., Damiano J. & Mick S.E. (2009a). A new MEMS-based system for ultra-high-resolution imaging at elevated temperatures. Microsc Res Techniq 72(3), 208215.
Allard L.F., Borisevich A., Deng W., Si R., Flytzani-Stephanopoulos M. & Overbury S.H. (2009b). Evolution of gold structure during thermal treatment of Au/FeO x catalysts revealed by aberration-corrected electron microscopy. J Elect Microsc 58(3), 199212.
Boyes E.D. & Gai P.L. (1997). Environmental high-resolution electron microscopy and applications to chemical science. Ultramicroscopy 67(1-4), 219232.
Creemer J.F., Helveg S., Hoveling G.H., Ullmann S., Molenbroek A.M., Sarro P.M. & Zandbergen H.W. (2008). Atomic-scale electron microscopy at ambient pressure. Ultramicroscopy 108(9), 993998.
Gai P.L. (1999a). Environmental high-resolution electron microscopy of gas-catalyst reactions. Top Catal 8(1-2), 97113.
Gai P.L. (1999b). Probing selective oxidation catalysis under reaction conditions by atomic-scale environmental high-resolution electron microscopy. Curr Opin Solid St Mater Sci 4(1), 6373.
Gai P.L. (2002). Developments in in situ environmental cell high-resolution electron microscopy and applications to catalysis. Top Catal 21(4), 161173.
Gai P.L. & Boyes E.D. (2009). Advances in atomic resolution in situ environmental transmission electron microscopy and 1 Å aberration-corrected in situ electron microscopy. Microsc Res Techniq 72, 153164.
Katz M.B., Zhang S.Y., Duan Y.W., Wang H.J., Fang M.H., Zhang K., Li B.H., Graham G.W. & Pan X.Q. (forthcoming). Reversible precipitation/dissolution of precious-metal clusters in perovskite-based catalyst materials: Bulk versus surface re-dispersion. J Catal (in press).
Sharma R. (2001). Design and applications of environmental cell transmission electron microscope for in situ observations of gas-solid reactions. Microsc Microanal 7(6), 494506.
Sharma R., Crozier P.A., Kang Z.C. & Eyring L. (2004). Observation of dynamic nanostructural and nanochemical changes in ceria-based catalysts during in situ reduction. Phil Mag 84(25-26), 27312747.
Sharma R. & Weiss K. (1998). Development of a TEM to study in situ structural and chemical changes at an atomic level during gas-solid interactions at elevated temperatures. Microsc Res Techniq 42(4), 270280.
van Huis M.A., Young N.P., Pandraud G., Creemer J.F., Vanmaekelbergh D., Kirkland A.I. & Zandbergen H.W. (2009). Atomic imaging of phase transitions and morphology transformations in nanocrystals. Adv Mater 21, 49924995.
Wittig J.E., Bentley J., Allard L.F. & Lukehart C.M. (2010). Evolution of FePt nanoparticle shape and L10 order during in situ annealing. Microsc Microanal 16(S2), 17541755.
Yaguchi T., Suzuki M., Watabe A., Nagakubo Y., Ueda K. & Kamino T. (2011). Development of a high temperature–atmospheric pressure environmental cell for high-resolution TEM. J Elect Microsc 60(3), 217225.
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Microscopy and Microanalysis
  • ISSN: 1431-9276
  • EISSN: 1435-8115
  • URL: /core/journals/microscopy-and-microanalysis
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