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Design and Application of Variable Temperature Setup for Scanning Electron Microscopy in Gases and Liquids at Ambient Conditions

Published online by Cambridge University Press:  03 June 2015

Ahmed S. Al-Asadi ,
Jie Zhang ,
Jianbo Li ,
Radislav A. Potyrailo  and
Andrei Kolmakov
Ahmed S. Al-Asadi
Affiliation:
The Department of Physics, Southern Illinois University, Carbondale, IL 62901, USA Department of Physics, College of Education for Pure Science, University of Basrah, Basra, Iraq
Jie Zhang
Affiliation:
The Department of Physics, Southern Illinois University, Carbondale, IL 62901, USA
Jianbo Li
Affiliation:
The Department of Physics, Southern Illinois University, Carbondale, IL 62901, USA
Radislav A. Potyrailo
Affiliation:
Manufacturing, Chemical & Materials Technologies, GE Global Research Center, Niskayuna, NY 12309, USA
Andrei Kolmakov*
Affiliation:
The Department of Physics, Southern Illinois University, Carbondale, IL 62901, USA
*
*Corresponding author.andrei.kolmakov@nist.gov
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Abstract

Scanning electron microscopy (SEM) of nanoscale objects in dry and fully hydrated conditions at different temperatures is of critical importance in revealing details of their interactions with an ambient environment. Currently available WETSEM capsules are equipped with thin electron-transparent membranes and allow imaging of samples at atmospheric pressure, but do not provide temperature control over the sample. Here, we developed and tested a thermoelectric cooling/heating setup for WETSEM capsules to allow ambient pressure in situ SEM studies with a temperature range between −15 and 100°C in gaseous, liquid, and frozen conditions. The design of the setup also allows for correlation of the SEM with optical microscopy and spectroscopy. As a demonstration of the possibilities of the developed approach, we performed real-time in situ microscopy studies of water condensation on a surface of Morpho sulkowskyi butterfly wing scales. We observed that initial water nucleation takes place on top of the scale ridges. These results confirmed earlier discovery of a preexisting polarity gradient of the ridges of Morpho butterflies. Our developed thermoelectric cooling/heating setup for environmental capsules meets the diverse needs for in situ nanocharacterization in material science, catalysis, microelectronics, chemistry, and biology.

Keywords

liquid SEMin situ SEMbutterfly scaleshydrophobicWETSEM
Type
Techniques and Equipment Development
Information
Microscopy and Microanalysis , Volume 21 , Issue 3 , June 2015 , pp. 765 - 770
Copyright
© Microscopy Society of America 2015 

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References

Bixler, G.D. & Bhushan, B. (2012). Bioinspired rice leaf and butterfly wing surface structures combining shark skin and lotus effects. Soft Matter 8(44), 11271–11284.Google Scholar
Danilatos, G. (1988). Foundations of environmental scanning electron microscopy. Adv Electron Electron Phys 71, 109–250.Google Scholar
Donev, E.U. & Hastings, J.T. (2009). Electron-beam-induced deposition of platinum from a liquid precursor. Nano Lett 9(7), 2715–2718.Google Scholar
Drouin, D., Couture, A.R., Joly, D., Tastet, X., Aimez, V. & Gauvin, R. (2007). CASINO V2.42: A fast and easy‐to‐use modeling tool for scanning electron microscopy and microanalysis users. Scanning 29(3), 92–101.Google Scholar
Dyab, A.K. & Paunov, V.N. (2010). Particle stabilised emulsions studied by WETSEM technique. Soft Matter 6(12), 2613–2615.CrossRefGoogle Scholar
Fang, Y., Sun, G., Wang, T., Cong, Q. & Ren, L. (2007). Hydrophobicity mechanism of non-smooth pattern on surface of butterfly wing. Chin Sci Bull 52(5), 711–716.Google Scholar
Ghiradella, H. (1991). Light and color on the wing: Structural colors in butterflies and moths. Appl Opt 30(24), 3492–3500.Google Scholar
Joy, D. & Joy, C. (2006). Scanning electron microscope imaging in liquids—Some data on electron interactions in water. J Microsc 221(2), 84–88.Google Scholar
Karmouch, R. & Ross, G.G. (2010). Experimental study on the evolution of contact angles with temperature near the freezing point. J Phys Chem C 114(9), 4063–4066.CrossRefGoogle Scholar
Katz, A., Bentur, A. & Kovler, K. (2007). A novel system for in-situ observations of early hydration reactions in wet conditions in conventional SEM. Cement Concrete Res 37(1), 32–37.Google Scholar
Kolmakova, N. & Kolmakov, A. (2010). Scanning electron microscopy for in situ monitoring of semiconductor—Liquid interfacial processes: Electron assisted reduction of Ag ions from aqueous solution on the surface of TiO2 rutile nanowire. J Phys Chem C 114(40), 17233–17237.Google Scholar
Manero, J., Gil, F., Padros, E. & Planell, J. (2003). Applications of environmental scanning electron microscopy (ESEM) in biomaterials field. Microsc Res Tech 61(5), 469–480.Google Scholar
Mei, H., Luo, D., Guo, P., Song, C., Liu, C., Zheng, Y. & Jiang, L. (2011). Multi-level micro-/nanostructures of butterfly wings adapt at low temperature to water repellency. Soft Matter 7(22), 10569–10573.CrossRefGoogle Scholar
Nosonovsky, M. (2007). Multiscale roughness and stability of superhydrophobic biomimetic interfaces. Langmuir 23(6), 3157–3161.Google Scholar
Potyrailo, R.A., Ghiradella, H., Vertiatchikh, A., Dovidenko, K., Cournoyer, J.R. & Olson, E. (2007). Morpho butterfly wing scales demonstrate highly selective vapour response. Nat Photonics 1(2), 123–128.Google Scholar
Potyrailo, R.A., Starkey, T.A., Vukusic, P., Ghiradella, H., Vasudev, M., Bunning, T., Naik, R.R., Tang, Z., Larsen, M. & Deng, T. (2013). Discovery of the surface polarity gradient on iridescent Morpho butterfly scales reveals a mechanism of their selective vapor response. Proc Natl Acad Sci USA 110(39), 15567–15572.Google Scholar
Rykaczewski, K., Scott, J. & Fedorov, A. (2011). Electron beam heating effects during environmental scanning electron microscopy imaging of water condensation on superhydrophobic surfaces. Appl Phys Lett 98(9), 093106-093101–093106-093103.Google Scholar
Rykaczewski, K. & Scott, J.H.J. (2011). Methodology for imaging nano-to-microscale water condensation dynamics on complex nanostructures. ACS Nano 5(7), 5962–5968.CrossRefGoogle ScholarPubMed
Stelmashenko, N., Craven, J., Donald, A., Terentjev, E. & Thiel, B. (2001). Topographic contrast of partially wetting water droplets in environmental scanning electron microscopy. J Microsc 204(2), 172–183.CrossRefGoogle ScholarPubMed
Thiberge, S., Nechushtan, A., Sprinzak, D., Gileadi, O., Behar, V., Zik, O., Chowers, Y., Michaeli, S., Schlessinger, J. & Moses, E. (2004). Scanning electron microscopy of cells and tissues under fully hydrated conditions. Proc Natl Acad Sci USA 101(10), 3346–3351.CrossRefGoogle ScholarPubMed
Thiberge, S., Zik, O. & Moses, E. (2004). An apparatus for imaging liquids, cells, and other wet samples in the scanning electron microscopy. Rev Sci Instrum 75(7), 2280–2289.Google Scholar
Tourkine, P., Le Merrer, M. & Quéré, D. (2009). Delayed freezing on water repellent materials. Langmuir 25(13), 7214–7216.Google Scholar
Vukusic, P. & Sambles, J.R. (2003). Photonic structures in biology. Nature 424(6950), 852–855.Google Scholar
Wagner, T., Neinhuis, C. & Barthlott, W. (1996). Wettability and contaminability of insect wings as a function of their surface sculptures. Acta Zoolog 77(3), 213–225.Google Scholar
Zheng, Y., Gao, X. & Jiang, L. (2007). Directional adhesion of superhydrophobic butterfly wings. Soft Matter 3(2), 178–182.CrossRefGoogle ScholarPubMed

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