In situ conversion of nanostructures from solid to hollow in transmission electron microscopes using electron beam

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.

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Reduction of Specimen Contamination in Electron-Beam Instruments

Proceedings, annual meeting, Electron Microscopy Society of America ◽

10.1017/s0424820100092840 ◽

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.

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

Proceedings, annual meeting, Electron Microscopy Society of America ◽

10.1017/s0424820100164386 ◽

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.

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

Proceedings, annual meeting, Electron Microscopy Society of America ◽

10.1017/s0424820100164738 ◽

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.

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

Nanomaterials ◽

10.3390/nano11010163 ◽

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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In situ experiments in the new transmission electron microscopes

Microscopy Microanalysis Microstructures ◽

10.1051/mmm:0199300402-3011100 ◽

1993 ◽

Vol 4 (2-3) ◽

pp. 111-117 ◽

Cited By ~ 6

Author(s):

J. Pelissier ◽

P. Debrenne

Keyword(s):

Transmission Electron ◽

In Situ Experiments ◽

Electron Microscopes

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In situ observation of the motion of ferroelectric domain walls in Bi4Ti3O12 single crystals

Journal of Applied Crystallography ◽

10.1107/s1600576716012267 ◽

2016 ◽

Vol 49 (5) ◽

pp. 1645-1652 ◽

Cited By ~ 6

Author(s):

Wanneng Ye ◽

Lingli Tang ◽

Chaojing Lu ◽

Huabing Li ◽

Yichun Zhou

Keyword(s):

Electron Beam ◽

Electron Microscope ◽

Single Crystals ◽

Transmission Electron Microscope ◽

Domain Walls ◽

Domain Switching ◽

Ferroelectric Domain ◽

In Situ Observation ◽

Transmission Electron

Five types of ferroelectric domain walls (DWs) are present in Bi4Ti3O12 single crystals (Ye et al., 2015). Here their motion was investigated in situ using transmission electron microscopy and optical microscopy. The motion of P (a)-90° DWs, P (a)-180° DWs and P (c)-180° DWs was observed through electron beam poling in a transmission electron microscope. The growth of new P s(a)-180° nanodomains was frequently seen and they tended to nucleate at preexisting P s(a)-90° DWs. Irregularly curved P (c)-180° DWs exhibit the highest mobility, while migration over a short range occurs occasionally for faceted P s(a)-90° DWs. In addition, the motion of P s(a)-90° DWs and the growth/annihilation of new needle-like P s(a)-90° domains in a 20 µm-thick crystal were observed under an external electric field on an optical microscope. Most of the new needle-like P s(a)-90° domains nucleate at preexisting P s(a)-90° DWs and the former are much smaller than the latter. This is very similar to the situation for P s(a)-180° domain switching induced by electron beam poling in a transmission electron microscope. Our observations suggest the energy hierarchy for different domains of P s(c)-180° ≤ P s(a)-180° ≤ P s(a)-90° ≤ new needle-like P s(a)-90° in ferroelectric Bi4Ti3O12.

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Coalescence between Au nanoparticles as induced by nanocurvature effect and electron beam athermal activation effect

Nanoscale ◽

10.1039/c7nr09710g ◽

2018 ◽

Vol 10 (17) ◽

pp. 7978-7983 ◽

Cited By ~ 1

Author(s):

Liang Cheng ◽

Xianfang Zhu ◽

Jiangbin Su

Keyword(s):

Electron Beam ◽

Electron Microscope ◽

Transmission Electron Microscope ◽

Room Temperature ◽

Electron Beam Irradiation ◽

Au Nanoparticles ◽

Beam Irradiation ◽

Activation Effect ◽

Transmission Electron

The coalescence of two single-crystalline Au nanoparticles on surface of amorphous SiOxnanowire, as induced by electron beam irradiation, wasin situstudied at room temperature in a transmission electron microscope.

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Computer-Controlled Polishing System For Preparing Multiple Pre-FIB TEM Specimens

Microscopy Today ◽

10.1017/s1551929500061952 ◽

2007 ◽

Vol 15 (6) ◽

pp. 38-39

Author(s):

D. J. MacMahon ◽

E. Raz-Moyal

Keyword(s):

Focused Ion Beam ◽

Ion Beam ◽

Product Yield ◽

Interface Layer ◽

Ex Situ ◽

Advantages And Disadvantages ◽

Transmission Electron ◽

Invaluable Tool ◽

Electron Microscopes

Semiconductor manufacturers are increasingly turning to Transmission Electron Microscopes (TEMs) to monitor product yield and process control, analyze defects, and investigate interface layer morphology. To prepare TEM specimens, Focused Ion Beam (FIB) technology is an invaluable tool, yielding a standard milled TEM lamella approximately 15 μm wide, 5 μm deep and ~100 nm thick. Several techniques have been developed to extract these tiny objects from a large wafer and view it in the TEM. These techniques, including ex-situ lift-out, H-bar, and in-situ lift-out, have different advantages and disadvantages, but all require painstaking preparation of one specimen at a time.

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