In-Situ Electrochemical Transmission Electron Microscopy for Battery Research

2014 ◽  
Vol 20 (2) ◽  
pp. 484-492 ◽  
Author(s):  
B. Layla Mehdi ◽  
Meng Gu ◽  
Lucas R. Parent ◽  
Wu Xu ◽  
Eduard N. Nasybulin ◽  
...  
Keyword(s):  
Electron Beam ◽  
Silicon Nanowires ◽  
Electrochemical Processes ◽  
Transmission Electron ◽  
Experimental Parameters ◽  
Scanning Transmission ◽  
Electrode Interface ◽  
Electron Microscopes

AbstractThe recent development of in-situ liquid stages for (scanning) transmission electron microscopes now makes it possible for us to study the details of electrochemical processes under operando conditions. As electrochemical processes are complex, care must be taken to calibrate the system before any in-situ/operando observations. In addition, as the electron beam can cause effects that look similar to electrochemical processes at the electrolyte/electrode interface, an understanding of the role of the electron beam in modifying the operando observations must also be understood. In this paper we describe the design, assembly, and operation of an in-situ electrochemical cell, paying particular attention to the method for controlling and quantifying the experimental parameters. The use of this system is then demonstrated for the lithiation/delithiation of silicon nanowires.

Quantitative Electrochemical Measurements Using In Situ ec-S/TEM Devices

2014 ◽  
Vol 20 (2) ◽  
pp. 452-461 ◽  
Author(s):  
Raymond R. Unocic ◽  
Robert L. Sacci ◽  
Gilbert M. Brown ◽  
Gabriel M. Veith ◽  
Nancy J. Dudney ◽  
...  
Keyword(s):  
Electron Beam ◽  
Electrochemical Impedance ◽  
Electrochemical Measurements ◽  
Small Scale ◽  
Electrochemical Cells ◽  
Current Profile ◽  
Electrochemical Processes ◽  
Transmission Electron ◽  
Scanning Transmission

AbstractInsight into dynamic electrochemical processes can be obtained with in situ electrochemical-scanning/transmission electron microscopy (ec-S/TEM), a technique that utilizes microfluidic electrochemical cells to characterize electrochemical processes with S/TEM imaging, diffraction, or spectroscopy. The microfluidic electrochemical cell is composed of microfabricated devices with glassy carbon and platinum microband electrodes in a three-electrode cell configuration. To establish the validity of this method for quantitative in situ electrochemistry research, cyclic voltammetry (CV), choronoamperometry (CA), and electrochemical impedance spectroscopy (EIS) were performed using a standard one electron transfer redox couple [Fe(CN)6]3−/4−-based electrolyte. Established relationships of the electrode geometry and microfluidic conditions were fitted with CV and chronoamperometic measurements of analyte diffusion coefficients and were found to agree with well-accepted values that are on the order of 10−5 cm2/s. Influence of the electron beam on electrochemical measurements was found to be negligible during CV scans where the current profile varied only within a few nA with the electron beam on and off, which is well within the hysteresis between multiple CV scans. The combination of experimental results provides a validation that quantitative electrochemistry experiments can be performed with these small-scale microfluidic electrochemical cells provided that accurate geometrical electrode configurations, diffusion boundary layers, and microfluidic conditions are accounted for.

Reduction of Specimen Contamination in Electron-Beam Instruments

1976 ◽  
Vol 34 ◽  
pp. 576-577
Author(s):  
G. Lehmpfuhl ◽  
P. J. Smith
Keyword(s):  
Electron Beam ◽  
Cold Trap ◽  
Beam Diameter ◽  
Transmission Electron ◽  
Scanning Transmission ◽  
Hydrocarbon Molecules ◽  
Electron Microscopes ◽  
Combination Of Methods ◽  
Convergent Beam ◽  
Very High

Specimens being observed with electron-beam instruments are subject to contamination, which is due to polymerization of hydrocarbon molecules by the beam. This effect becomes more important as the size of the beam is reduced. In convergent-beam studies with a beam diameter of 100 Å, contamination was observed to grow on samples at very high rates. Within a few seconds needles began forming under the beam on both the top and the underside of the sample, at growth rates of 400-500 Å/s, severely limiting the time available for observation. Such contamination could cause serious difficulty in examining a sample with the new scanning transmission electron microscopes, in which the beam is focused to a few angstroms.We have been able to reduce the rate of contamination buildup by a combination of methods: placing an anticontamination cold trap in the sample region, preheating the sample before observation, and irradiating the sample with a large beam before observing it with a small beam.

Applications of In-situ Sample Preparation and Modeling of SEM-STEM Imaging

2008 ◽  
Author(s):  
R.J. Young ◽  
A. Buxbaum ◽  
B. Peterson ◽  
R. Schampers
Keyword(s):  
Sample Preparation ◽  
Focused Ion Beam ◽  
Ion Beam ◽  
Dual Beam ◽  
Transmission Electron ◽  
Scanning Transmission ◽  
Electron Microscopes ◽  
Scanning Electron Microscopes ◽  
Preparation Techniques

Abstract Scanning transmission electron microscopy with scanning electron microscopes (SEM-STEM) has become increasing used in both SEM and dual-beam focused ion beam (FIB)-SEM systems. This paper describes modeling undertaken to simulate the contrast seen in such images. Such modeling provides the ability to help understand and optimize imaging conditions and also support improved sample preparation techniques.

The Theoretical Contrast in Scanning and Conventional High Resolution Microscopes

1969 ◽  
Vol 27 ◽  
pp. 170-171
Author(s):  
E. Zeitler ◽  
M. G. R. Thomson
Keyword(s):  
Small Volume ◽  
Volume Element ◽  
Optical Processing ◽  
Image Construction ◽  
Object Interaction ◽  
Transmission Electron ◽  
Scanning Transmission ◽  
Optical Treatment ◽  
Electron Microscopes ◽  
Intensity Contrast

In the formation of an image each small volume element of the object is correlated to an areal element in the image. The structure or detail of the object is represented by changes in intensity from element to element, and this variation of intensity (contrast) is determined by the interaction of the electrons with the specimen, and by the optical processing of the information-carrying electrons. Both conventional and scanning transmission electron microscopes form images which may be considered in this way, but the mechanism of image construction is very different in the two cases. Although the electron-object interaction is the same, the optical treatment differs.

Remote On-Line Control of a High-Voltage in situ Transmission Electron Microscope with A Rational User Interface

1996 ◽  
Vol 54 ◽  
pp. 384-385
Author(s):  
M.A. O’Keefe ◽  
J. Taylor ◽  
D. Owen ◽  
B. Crowley ◽  
K.H. Westmacott ◽  
...  
Keyword(s):  
Electron Microscopy ◽  
Electron Microscope ◽  
User Interface ◽  
Transmission Electron Microscope ◽  
High Voltage ◽  
Materials Science ◽  
Transmission Electron ◽  
On Line ◽  
Electron Microscopes

Remote on-line electron microscopy is rapidly becoming more available as improvements continue to be developed in the software and hardware of interfaces and networks. Scanning electron microscopes have been driven remotely across both wide and local area networks. Initial implementations with transmission electron microscopes have targeted unique facilities like an advanced analytical electron microscope, a biological 3-D IVEM and a HVEM capable of in situ materials science applications. As implementations of on-line transmission electron microscopy become more widespread, it is essential that suitable standards be developed and followed. Two such standards have been proposed for a high-level protocol language for on-line access, and we have proposed a rational graphical user interface. The user interface we present here is based on experience gained with a full-function materials science application providing users of the National Center for Electron Microscopy with remote on-line access to a 1.5MeV Kratos EM-1500 in situ high-voltage transmission electron microscope via existing wide area networks. We have developed and implemented, and are continuing to refine, a set of tools, protocols, and interfaces to run the Kratos EM-1500 on-line for collaborative research. Computer tools for capturing and manipulating real-time video signals are integrated into a standardized user interface that may be used for remote access to any transmission electron microscope equipped with a suitable control computer.

Methods to Monitor and Improve the Performance of Specimen Holders for Transmission Electron Cryomicroscopy

1996 ◽  
Vol 54 ◽  
pp. 454-455
Author(s):  
B. L. Armbruster ◽  
B. Kraus ◽  
M. Pan
Keyword(s):  
Electron Microscopy ◽  
Electron Beam ◽  
Electron Beam Irradiation ◽  
Beam Irradiation ◽  
Quality Of Data ◽  
Electron Cryomicroscopy ◽  
Thermal Equilibration ◽  
Transmission Electron ◽  
Electron Microscopes

One goal in electron microscopy of biological specimens is to improve the quality of data to equal the resolution capabilities of modem transmission electron microscopes. Radiation damage and beam- induced movement caused by charging of the sample, low image contrast at high resolution, and sensitivity to external vibration and drift in side entry specimen holders limit the effective resolution one can achieve. Several methods have been developed to address these limitations: cryomethods are widely employed to preserve and stabilize specimens against some of the adverse effects of the vacuum and electron beam irradiation, spot-scan imaging reduces charging and associated beam-induced movement, and energy-filtered imaging removes the “fog” caused by inelastic scattering of electrons which is particularly pronounced in thick specimens.Although most cryoholders can easily achieve a 3.4Å resolution specification, information perpendicular to the goniometer axis may be degraded due to vibration. Absolute drift after mechanical and thermal equilibration as well as drift after movement of a holder may cause loss of resolution in any direction.

scholarly journals In Situ Observation of Electron-Beam-Induced Formation of Nano-Structures in PbTe

Nanomaterials ◽  
2021 ◽  
Vol 11 (1) ◽  
pp. 163
Author(s):  
Iryna Zelenina ◽  
Igor Veremchuk ◽  
Yuri Grin ◽  
Paul Simon
Keyword(s):  
Electron Beam ◽  
Gas Phase ◽  
Threshold Current ◽  
Threshold Current Density ◽  
Atomic Scale ◽  
In Situ Observation ◽  
Nano Structures ◽  
Transmission Electron ◽  
Initial Crystal

Nano-scaled thermoelectric materials attract significant interest due to their improved physical properties as compared to bulk materials. Well-shaped nanoparticles such as nano-bars and nano-cubes were observed in the known thermoelectric material PbTe. Their extended two-dimensional nano-layer arrangements form directly in situ through electron-beam treatment in the transmission electron microscope. The experiments show the atomistic depletion mechanism of the initial crystal and the recrystallization of PbTe nanoparticles out of the microparticles due to the local atomic-scale transport via the gas phase beyond a threshold current density of the beam.

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