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Preparation and Loading Process of Single Crystalline Samples into a Gas Environmental Cell Holder for In Situ Atomic Resolution Scanning Transmission Electron Microscopic Observation

  • Rainer Straubinger (a1), Andreas Beyer (a1) and Kerstin Volz (a1)
Abstract
Abstract

A reproducible way to transfer a single crystalline sample into a gas environmental cell holder for in situ transmission electron microscopic (TEM) analysis is shown in this study. As in situ holders have only single-tilt capability, it is necessary to prepare the sample precisely along a specific zone axis. This can be achieved by a very accurate focused ion beam lift-out preparation. We show a step-by-step procedure to prepare the sample and transfer it into the gas environmental cell. The sample material is a GaP/Ga(NAsP)/GaP multi-quantum well structure on Si. Scanning TEM observations prove that it is possible to achieve atomic resolution at very high temperatures in a nitrogen environment of 100,000 Pa.

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* Corresponding author. rainer.straubinger@physik.uni-marburg.de
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G.B. Adams Jr., H.L. Johnston & E.C. Kerr (1952). The heat capacity of gallium up from 15 to 320 K. The heat of fusion at the melting point. J Am Chem Soc 74, 4784.

L.F. Allard , S.H. Overbury , W.C. Bigelow , M.B. Katz , D.P. Nackashi & J. Damiano (2012). Novel MEMS-based gas-cell/heating specimen holder provides advanced imaging capabilities for in situ reaction studies. Microsc Microanal 18, 656666.

B.I. Birajdar , T. Antesberger , B. Butz , M. Stutzmann & E. Spiecker (2012). Direct in situ transmission electron microscopy observation of Al push up during early stages of the Al-induced layer exchange. Scr Mater 66, 550553.

E.D. Boyes & P.L. Gai (1997). Environmental high resolution electron microscopy and applications to chemical science. Ultramicroscopy 67, 219232.

J.F. Creemer , S. Helveg , G.H. Hoveling , S. Ullmann , A.M. Molenbroek , P.M. Sarro & H.W. Zandbergen (2008). Atomic-scale electron microscopy at ambient pressure. Ultramicroscopy 108, 993998.

L.A. Giannuzzi & F.A. Stevie (1999). A review of focused ion beam milling techniques for TEM specimen preparation. Micron 30, 197204.

S. Gies , M. Zimprich , T. Wegele , C. Kruska , A. Beyer , W. Stolz , K. Volz & W. Heimbrodt (2014). Annealing effects on the composition and disorder of Ga(N,As,P) quantum wells on silicon substrates for laser application. J Cryst Growth 402, 169174.

K. Hillerich , K.A. Dick , C.Y. Wen , M.C. Reuter , S. Kodambaka & F.M. Ross (2013). Strategies to control morphology in hybrid group III-V/group IV heterostructure nanowires. Nano Lett 13, 903908.

F. Hofer , W. Grogger , G. Kothleitner & P. Warbichler (1997). Quantitative analysis of EFTEM elemental distribution images. Ultramicroscopy 67, 83103.

R.C. Hugo , H. Kung , J.R. Weertman , R. Mitra , J.A. Knapp & D.M. Follstaedt (2003). In-situ TEM tensile testing of DC magnetron sputtered and pulsed laser deposited Ni thin films. Acta Mater 51, 19371943.

P.J. Imrich , C. Kirchlechner , D. Kiener & G. Dehm (2015). Internal and external stresses: In situ TEM compression of Cu bicrystals containing a twin boundary. Scr Mater 100, 9497.

C. Kallesøe , C.Y. Wen , T.J. Booth , O. Hansen , P. Bøggild , F.M. Ross & K. Mølhave (2012). In situ TEM creation and electrical characterization of nanowire devices. Nano Lett 12, 29652970.

M.B. Katz , Y. Duan , G.W. Graham , X. Pan & L.F. Allard (2012). In situ observation of the evolution of Pt particles in a perovskite-based catalyst during redox cycling at high temperature and atmospheric pressure with atomic resolution. Microsc Microanal 18, 11201121.

K. Kishita , H. Sakai , H. Tanaka , H. Saka , K. Kuroda , M. Sakamoto , A. Watabe & T. Kamino (2009). Development of an analytical environmental TEM system and its application. J Electron Microsc 58, 331339.

M. Legros , D.S. Gianola & K.J. Hemker (2008). In situ TEM observations of fast grain-boundary motion in stressed nanocrystalline aluminum films. Acta Mater 56, 33803393.

S. Liebich , M. Zimprich , A. Beyer , C. Lange , D.J. Franzbach , S. Chatterjee , N. Hossain , S.J. Sweeney , K. Volz , B. Kunert & W. Stolz (2011). Laser operation of Ga(NAsP) lattice-matched to (001) silicon substrate. Appl Phys Lett 99, 071109.

B.M. Morrow , R.J. McCabe , E.K. Cerreta & C.N. Tomé (2014). In-situ TEM observation of twinning and detwinning during cyclic loading in Mg. Metall Mater Trans A Phys Metall Mater Sci 45, 3640.

B. Schaffer , W. Grogger & G. Kothleitner (2004). Automated spatial drift correction for EFTEM image series. Ultramicroscopy 102, 2736.

M. Schaffer , B. Schaffer & Q. Ramasse (2012). Sample preparation for atomic-resolution STEM at low voltages by FIB. Ultramicroscopy 114, 6271.

S. Suzuki , C. Bower & O. Zhou (1998). In-situ TEM and EELS studies of alkali–metal intercalation with single-walled carbon nanotubes. Chem Phys Lett 285, 230234.

K. Volz , A. Beyer , W. Witte , J. Ohlmann , I. Nmeth , B. Kunert & W. Stolz (2011). GaP-nucleation on exact Si (0 0 1) substrates for III/V device integration. J Cryst Growth 315, 3747.

K. Werner , A. Beyer , J.O. Oelerich , S.D. Baranovskii , W. Stolz & K. Volz (2014). Structural characteristics of gallium metal deposited on Si (001) by MOCVD. J Cryst Growth 405, 102109.

T. Yaguchi , M. Suzuki , A. Watabe , Y. Nagakubo , K. Ueda & T. Kamino (2011). Development of a high temperature-atmospheric pressure environmental cell for high-resolution TEM. J Electron Microsc 60, 217225.

S. Zhang , C. Chen , M. Cargnello , P. Fornasiero , R.J. Gorte , G.W. Graham & X. Pan (2015). Dynamic structural evolution of supported palladium–ceria core–shell catalysts revealed by in situ electron microscopy. Nat Commun 6, 7778.

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Microscopy and Microanalysis
  • ISSN: 1431-9276
  • EISSN: 1435-8115
  • URL: /core/journals/microscopy-and-microanalysis
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