Abstract:
Development of new functional nanomaterials and nanosystems play an important role on advancement of society through more efficient energy use, improvement on energy conversion processes, more efficient transportation and sustainable products with less environmental impact.
Properties of modern nanomaterials are controlled on an atomic scale and thus research and development of nanomaterials requires atomic scale imaging and analysis see for example [1]. The development of materials or devices with optimized functions often require to perform in situ studies of actual functional state of the materials at conditions other than the room temperature and standard high vacuum condition of electron microscope columns, in order to allow some processes like oxidation to be observed and analyzed at high spatial resolution.
Implementation of differential pumping apertures in an aberration corrected TEM (FEI Titan ETEM [2]) enables environmental studies, e.g. oxidation, reduction, or corrosion experiments [3]. On the other hand MEMS technology based in situ heating stages with more accurate knowledge and temperature control together with very fast settling time enables quantitative atomic scale studies at elevated temperatures [4]. Recent years have seen the rapid technological development which enables in situ studies of materials while maintaining high-resolution imaging and analysis at elevated temperatures, under electrical bias and gas environment [5-8].
In this contribution we will describe the path to have an accurate knowledge and control of experimental conditions in advanced in situ S/TEM experiments. Special attention will be given to the image resolution and sensitivity in ETEM gas environments and the temperature accuracy and uniformity provided by NanoEx™ heating stages [9]. Recent application examples will be presented to highlight these in situ S/TEM capabilities. Some aspects of more routine analytical experiments with ‘workhorse’ 200kV TEM/STEM systems will also be presented.
Keywords: HRTEM, HRSTEM, EDS, In-Situ, MEMS devices, environmental (S)TEM
References:
[1] K. W. Urban, Science, 2008, 321, 506–510
[2] http://www.FEI.com/ETEM
[3] E. P. Butler and K. F. Hale, in Practical Methods in Electron Microscopy, ed. M.
Glauert, Elsevier Science Ltd,Amsterdam, 1981, pp. 239–308.
[4] Allard, L. F. et al. Microscopy Research and Technique 72, 208-215P.
[5] P. L. Gai, R. Sharma and F. M. Ross, MRS Bull., 2008, 33, 107–114.
[6] H. Yoshida, Y. Kuwauchi, J. R. Jinschek, K. Sun, S. Tanaka, M. Kohyama, S. Shimada,
M. Haruta and S. Takeda, Science, 2012, 335, 317–319.
[7] J. F. Creemer, S. Helveg, G. H. Hoveling, S. Ullmann, A. M. Molenbroek, P. M.
Sarro and H. W. Zandbergen, Ultramicroscopy 2008, 108, 993–998
[8] Malladi, S.K.; Xu, X.; van Huis, M.A.; Tichelaar, F.D.; Batenburg, K.J.; Yücelen, E.;
Dubiel, B.; Czyrska-Filemonowicz, A.; Zandbergen, H.W. (2014) Nano letters, volume
14, pp. 384 – 389
[9] https://www.fei.com/accessories/nanoEx-i-v/
