AVS 56th International Symposium & Exhibition | |
In Situ Microscopy and Spectroscopy: Interfacial and Nanoscale Science Topical Conference | Friday Sessions |
Session IS+AS-FrM |
Session: | In-Situ Microscopy and Spectroscopy: Dynamic Nanoscale Processes |
Presenter: | T.C. Isabell, JEOL USA, Inc. |
Authors: | T.C. Isabell, JEOL USA, Inc. J. Brink, JEOL USA, Inc. B.L. Armbruster, JEOL USA, Inc. M. Kawasaki, JEOL USA, Inc. |
Correspondent: | Click to Email |
Few electron optical inventions have revolutionized the TEM/STEM as profoundly as the spherical aberration (Cs) corrector. Characterization of technologically important materials increasingly needs to be done at the atomic or even sub-atomic level. This characterization includes determination of atomic structure as well as structural chemistry. With Cs correctors the sub-Ångstrom imaging barrier has been passed, and fast atomic scale spectroscopy is possible. In addition to improvements in resolution, Cs correctors offer a number of other significant improvements and benefits.
One such benefit is that a larger pole piece gap can be used in the TEM, while still achieving sub-Angstrom image resolution. This means that there is more room around the sample for in-situ experimentation. This opens the door to a whole realm of dynamic experiments, done on a spatial scale never before possible.
There are a few ways in which in-situ experiments in the TEM can be carried out. The TEM can be dedicated to in-situ experimentation and modified to include an environmental cell around the specimen. Through a differential pumping system, the pressure around the sample can be modified and with gas injection systems, the chemistry around the sample can be controlled. Such E-cell TEM systems have existed for years, but recent improvements in design have expanded the usefulness of such systems. Modern E-cell TEMs are capable of not just TEM imaging, but also energy loss spectroscopy (EELS), scanning transmission electron microscopy (STEM) and in some cases energy dispersive spectroscopy (EDS). However, in fully dedicated E-cell TEMs, scanning techniques and EDS may be geometrically limited.
Alternatively, specially designed TEM specimen holders can be used in a conventional TEM for in-situ work. A variety of environmental holders have been developed for these kinds of experiments, including: heating, cooling, straining, and indentation holders; probe holders for electrical measurements; holders with an enclosed environmental cell so that the specimen can be examined under different gases and or liquids; and even holders with an integrated SPM tip for simultaneous TEM/SPM observation of the specimen. MEMS devices are being used for some of these holders to incorporate things such as rapid heating into the specimen holder.1 These holders can be used to study transport phenomena across interfaces, sintering phenomena in nanoparticles, and elevated temperature studies of catalysts.2,3
1 J. Damiano, D.P. Nackashi and S.E. Mick; Microsc Microanal 14(Suppl 2) 1332, 2008.
2 M. Briceno, et al., Microsc Microanal 14(Suppl 2) 1336, 2008.
3 J. Liu, J. Wang, L.F. Allard; Microsc Microanal 14(Suppl 2) 262, 2008.