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High-Resolution Imaging and Spectroscopy at High Pressure: A Novel Liquid Cell for the Transmission Electron Microscope

Published online by Cambridge University Press:  09 December 2015

Mihaela Tanase
Affiliation:
Center for Nanoscale Science and Technology, National Institute of Standards and Technology, Gaithersburg, MD 20899, USA Institute for Research in Electronics and Applied Physics, University of Maryland, College Park, MD 20742, USA
Jonathan Winterstein
Affiliation:
Center for Nanoscale Science and Technology, National Institute of Standards and Technology, Gaithersburg, MD 20899, USA
Renu Sharma
Affiliation:
Center for Nanoscale Science and Technology, National Institute of Standards and Technology, Gaithersburg, MD 20899, USA
Vladimir Aksyuk
Affiliation:
Center for Nanoscale Science and Technology, National Institute of Standards and Technology, Gaithersburg, MD 20899, USA
Glenn Holland
Affiliation:
Center for Nanoscale Science and Technology, National Institute of Standards and Technology, Gaithersburg, MD 20899, USA
James A. Liddle*
Affiliation:
Center for Nanoscale Science and Technology, National Institute of Standards and Technology, Gaithersburg, MD 20899, USA
*Corresponding
* Corresponding author. liddle@nist.gov

Abstract

We demonstrate quantitative core-loss electron energy-loss spectroscopy of iron oxide nanoparticles and imaging resolution of Ag nanoparticles in liquid down to 0.24 nm, in both transmission and scanning transmission modes, in a novel, monolithic liquid cell developed for the transmission electron microscope (TEM). At typical SiN membrane thicknesses of 50 nm the liquid-layer thickness has a maximum change of only 30 nm for the entire TEM viewing area of 200×200 µm.

Type
Equipment and Techniques Development
Copyright
© Microscopy Society of America 2015 

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References

Abrams, I.M. & Mcbain, J.W. (1944). A closed cell for electron microscopy. J Appl Phys 15(8), 607609.CrossRefGoogle Scholar
Baker, R.T.K. & Harris, P.S. (1972). Controlled atmosphere electron microscopy. J Phys E Sci Instrum 5(8), 793.CrossRefGoogle Scholar
Bartholomew, C.H. & Farrauto, R.J. (2011). Fundamentals of Industrial Catalytic Processes . Hoboken, NJ: Wiley.Google Scholar
Bell, A.T. (2003). The impact of nanoscience on heterogeneous catalysis. Science 299(5613), 16881691.CrossRefGoogle ScholarPubMed
Burge, R.E. & Misell, D.L. (1968). Electron energy loss spectra for evaporated carbon films. Philos Mag 18(152), 251259.CrossRefGoogle Scholar
Cavé, L., Al, T., Loomer, D., Cogswell, S. & Weaver, L. (2006). A STEM/EELS method for mapping iron valence ratios in oxide minerals. Micron 37(4), 301309.CrossRefGoogle ScholarPubMed
Chen, Q., Smith, J.M., Park, J., Kim, K., Ho, D., Rasool, H.I., Zettl, A. & Alivisatos, A.P. (2013). 3D motion of DNA-Au nanoconjugates in graphene liquid cell electron microscopy. Nano Lett 13(9), 45564561.CrossRefGoogle ScholarPubMed
Cosslett, V.E. (1969). Energy loss and chromatic aberration in electron microscopy. Z Angew Physik 27, 138141.Google Scholar
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.CrossRefGoogle ScholarPubMed
de Jonge, N., Peckys, D.B., Kremers, G.J. & Piston, D.W. (2009). Electron microscopy of whole cells in liquid with nanometer resolution. Proc Natl Acad Sci U S A 106, 21592164.CrossRefGoogle Scholar
de Jonge, N., Poirier-Demers, N., Demers, H., Peckys, D.B. & Drouin, D. (2010). Nanometer-resolution electron microscopy through micrometers-thick water layers. Ultramicroscopy 110(9), 11141119.CrossRefGoogle ScholarPubMed
de Jonge, N. & Ross, F.M. (2011). Electron microscopy of specimens in liquid. Nat Nanotechnol 6(11), 695704.CrossRefGoogle ScholarPubMed
Dukes, M.J., Jacobs, B.W., Morgan, D.G., Hegde, H. & Kelly, D.F. (2013). Visualizing nanoparticle mobility in liquid at atomic resolution. Chem Commun 49(29), 30073009.CrossRefGoogle ScholarPubMed
Egerton, R.F. (2011). Electron Energy-Loss Spectroscopy in the Electron Microscope. Berlin and New York: Springer.CrossRefGoogle Scholar
Egerton, R.F., Wang, F., Malac, M., Moreno, M.S. & Hofer, F. (2008). Fourier-ratio deconvolution and its Bayesian equivalent. Micron 39(6), 642647.CrossRefGoogle ScholarPubMed
Gai, P. (2002). Developments in in situ environmental cell high-resolution electron microscopy and applications to catalysis. Top Catal 21(4), 161173.CrossRefGoogle Scholar
Grogan, J.M. & Bau, H.H. (2010). The nanoaquarium: A platform for in situ transmission electron microscopy in liquid media. J Microelectromech Syst 19(4), 885894.CrossRefGoogle Scholar
Gu, M., Parent, L.R., Mehdi, B.L., Unocic, R.R., McDowell, M.T., Sacci, R.L., Xu, W., Connell, J.G., Xu, P., Abellan, P., Chen, X., Zhang, Y., Perea, D.E., Evans, J.E., Lauhon, L.J., Zhang, J.-G., Liu, J., Browning, N.D., Cui, Y., Arslan, I. & Wang, C.-M. (2013). Demonstration of an electrochemical liquid cell for operando transmission electron microscopy observation of the lithiation/delithiation behavior of Si nanowire battery anodes. Nano Lett 13(12), 61066112.CrossRefGoogle ScholarPubMed
Holtz, M.E., Yu, Y., Gao, J., Abruña, H.D. & Muller, D.A. (2013). In situ electron energy-loss spectroscopy in liquids. Microsc Microanal 19(4), 10271035.CrossRefGoogle ScholarPubMed
Iakoubovskii, K., Mitsuishi, K., Nakayama, Y. & Furuya, K. (2008). Thickness measurements with electron energy loss spectroscopy. Microsc Res Tech 71(8), 626631.CrossRefGoogle ScholarPubMed
Jeangros, Q., Faes, A., Wagner, J.B., Hansen, T.W., Aschauer, U., Van herle, J., Hessler-Wyser, A. & Dunin-Borkowski, R.E. (2010). In situ redox cycle of a nickel–YSZ fuel cell anode in an environmental transmission electron microscope. Acta Mater 58(14), 45784589.CrossRefGoogle Scholar
Jensen, E., Burrows, A. & Mølhave, K. (2014). Monolithic chip system with a microfluidic channel for in situ electron microscopy of liquids. Microsc Microanal 20(2), 445451.CrossRefGoogle ScholarPubMed
Jungjohann, K.L., Evans, J.E., Aguiar, J.A., Arslan, I. & Browning, N.D. (2012). Atomic-scale imaging and spectroscopy for in situ liquid scanning transmission electron microscopy. Microsc Microanal 18(3), 621627.CrossRefGoogle ScholarPubMed
Klein, K., Anderson, I. & de Jonge, N. (2011 a). Transmission electron microscopy with a liquid flow cell. J Microsc 242(2), 117123.CrossRefGoogle ScholarPubMed
Klein, K., de Jonge, N. & Anderson, I. (2011 b). Energy-loss characteristics for EFTEM imaging with a liquid flow cell. Microsc Microanal 17(Suppl 2), 780781.CrossRefGoogle Scholar
Li, D., Nielsen, M.H., Lee, J.R.I., Frandsen, C., Banfield, J.F. & De Yoreo, J.J. (2012). Direction-specific interactions control crystal growth by oriented attachment. Science 336(6084), 10141018.CrossRefGoogle ScholarPubMed
Liao, H.-G., Zherebetskyy, D., Xin, H., Czarnik, C., Ercius, P., Elmlund, H., Pan, M., Wang, L.-W. & Zheng, H. (2014). Facet development during platinum nanocube growth. Science 345(6199), 916919.CrossRefGoogle ScholarPubMed
Liddle, J.A., Huggins, H.A., Mulgrew, P., Harriott, L.R., Wade, H.H. & Bolan, K. (1994). Fracture strength of thin ceramic membranes. MRS Online Proceedings Library 338.Google Scholar
Liu, K.-L., Wu, C.-C., Huang, Y.-J., Peng, H.-L., Chang, H.-Y., Chang, P., Hsu, L. & Yew, T.-R. (2008). Novel microchip for in situ TEM imaging of living organisms and bio-reactions in aqueous conditions. Lab Chip 8(11), 19151921.CrossRefGoogle ScholarPubMed
Maier-Schneider, D., Maibach, J. & Obermeier, E. (1995). A new analytical solution for the load-deflection of square membranes. J Microelectromech Syst 4(4), 238241.CrossRefGoogle Scholar
Marton, L. (1935). La microscopie electronique des objets biologiques. Bull Acad Roy Belgique 21, 553560.Google Scholar
Mele, L., Santagata, F., Pandraud, G., Morana, B., Tichelaar, F.D., Creemer, J.F. & Sarro, P.M. (2010). Wafer-level assembly and sealing of a MEMS nanoreactor for in situ microscopy. J Micromech Microeng 20(8), 085040.CrossRefGoogle Scholar
Menon, N.K. & Krivanek, O.L. (2002). Synthesis of electron energy loss spectra for the quantification of detection limits. Microsc Microanal 8(3), 203215.CrossRefGoogle ScholarPubMed
O’Keefe, M., Allard, L. & Blom, D. (2008). Young’s fringes are not evidence of HRTEM resolution. Microsc Microanal 14(Suppl 2), 834835.CrossRefGoogle Scholar
O’Keefe, M., Allard, L. & Blom, D. (2010). Defining HRTEM resolution: Image resolutions and microscope limits. Microsc Microanal 16(Suppl 2), 766767.CrossRefGoogle Scholar
Peña, F.d.l., Burdet, P., Sarahan, M., Nord, M., Ostasevicius, T., Taillon, J., Eljarrat, A., Mazzucco, S., Fauske, V.T., Donval, G., Zagonel, L.F., Walls, M. & Iyengar, I. (2015). Hyperspy 0.8.Google Scholar
Radisic, A., Ross, F.M. & Searson, P.C. (2006 a). In situ study of the growth kinetics of individual island electrodeposition of copper. J Phys Chem B 110(15), 78627868.CrossRefGoogle ScholarPubMed
Radisic, A., Vereecken, P.M., Hannon, J.B., Searson, P.C. & Ross, F.M. (2006 b). Quantifying electrochemical nucleation and growth of nanoscale clusters using real-time kinetic data. Nano Lett 6(2), 238242.CrossRefGoogle ScholarPubMed
Ramachandra, R., Demers, H. & de Jonge, N. (2013). The influence of the sample thickness on the lateral and axial resolution of aberration-corrected scanning transmission electron microscopy. Microsc Microanal 19(1), 93101.CrossRefGoogle ScholarPubMed
Reimer, L. (1997). Transmission Electron Microscopy: Physics of Image Formation and Microanalysis. New York: Springer-Verlag.CrossRefGoogle Scholar
Riegler, K. & Kothleitner, G. (2010). EELS detection limits revisited: Ruby—a case study. Ultramicroscopy 110(8), 10041013.CrossRefGoogle Scholar
Ross, F.M. (2010). Controlling nanowire structures through real time growth studies. Rep Prog Phys 73(11), 114501.CrossRefGoogle Scholar
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.Google ScholarPubMed
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. Philos Mag 84(25–26), 27312747.CrossRefGoogle Scholar
Sharma, R., Rez, P., Brown, M., Du, G. & Treacy, M.M.J. (2007). Dynamic observations of the effect of pressure and temperature conditions on the selective synthesis of carbon nanotubes. Nanotechnology 18(12), 125602.CrossRefGoogle Scholar
Smeets, P.J.M., Cho, K.R., Kempen, R.G.E., Sommerdijk, N.A.J.M. & De Yoreo, J.J. (2015). Calcium carbonate nucleation driven by ion binding in a biomimetic matrix revealed by in situ electron microscopy. Nat Mater 14(4), 394399.CrossRefGoogle Scholar
Swift, J.A. & Brown, A.C. (1970). An environmental cell for the examination of wet biological specimens at atmospheric pressure by transmission scanning electron microscopy. J Phys E Sci Instrum 3(11), 924.CrossRefGoogle ScholarPubMed
Vendelbo, S.B., Elkjær, C.F., Falsig, H., Puspitasari, I., Dona, P., Mele, L., Morana, B., Nelissen, B.J., van Rijn, R., Creemer, J.F., Kooyman, P.J. & Helveg, S. (2014). Visualization of oscillatory behaviour of Pt nanoparticles catalysing CO oxidation. Nat Mater (advance online publication). Nat Mater 13(9), 884890.Google Scholar
Wang, C.-M., Liao, H.-G. & Ross, F.M. (2015). Observation of materials processes in liquids by electron microscopy. MRS Bull 40(1), 4652.CrossRefGoogle Scholar
Wang, C., Qiao, Q., Shokuhfar, T. & Klie, R.F. (2014). High-resolution electron microscopy and spectroscopy of ferritin in biocompatible graphene liquid cells and graphene sandwiches. Adv Mater 26(21), 34103414.CrossRefGoogle ScholarPubMed
Wang, F., Egerton, R. & Malac, M. (2009 a). Fourier-ratio deconvolution techniques for electron energy-loss spectroscopy (EELS). Ultramicroscopy 109(10), 12451249.CrossRefGoogle Scholar
Wang, R., Crozier, P.A. & Sharma, R. (2009 b). Structural transformation in ceria nanoparticles during redox processes. J Phys Chem C 113(14), 57005704.CrossRefGoogle Scholar
Welch, D.A., Faller, R., Evans, J.E. & Browning, N.D. (2013). Simulating realistic imaging conditions for in situ liquid microscopy. Ultramicroscopy 135, 3642.CrossRefGoogle ScholarPubMed
Williamson, M.J., Tromp, R.M., Vereecken, P.M., Hull, R. & Ross, F.M. (2003). Dynamic microscopy of nanoscale cluster growth at the solid-liquid interface. Nat Mater 2(8), 532536.CrossRefGoogle ScholarPubMed
Yuk, J.M., Park, J., Ercius, P., Kim, K., Hellebusch, D.J., Crommie, M.F., Lee, J.Y., Zettl, A. & Alivisatos, A.P. (2012). High-resolution EM of colloidal nanocrystal growth using graphene liquid cells. Science 336(6077), 6164.CrossRefGoogle ScholarPubMed
Zheng, H., Smith, R.K., Jun, Y.-w., Kisielowski, C., Dahmen, U. & Alivisatos, A.P. (2009). Observation of single colloidal platinum nanocrystal growth trajectories. Science 324(5932), 13091312.CrossRefGoogle ScholarPubMed

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