The Nanoaquarium: A Platform for <i>In Situ</i> Transmission Electron Microscopy in Liquid Media

Grogan, Joseph M.; Bau, Haim H.

doi:10.1109/jmems.2010.2051321

Cited by 125 publications

(124 citation statements)

References 31 publications

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“…The spacer may be a solid layer with a channel, or spherical particles. The liquid may be inserted through an entry port etched into one chip (14)(15)(16)(17)(18) or flowed in through the gap between the chips (19). Electrodes can be patterned lithographically inside the closed cell and controlled by an external potentiostat (14).…”

Section: The Rapidly Developing Liquid Cell Microscopy Techniquementioning

confidence: 99%

“…Electrodes can be patterned lithographically inside the closed cell and controlled by an external potentiostat (14). In each design, the electrode materials and geometry can be customized for the particular applications (14,16,18,(20)(21)(22). A heating element (23) or cooling capability (24) can be integrated, and the silicon nitride surfaces can be patterned or chemically modified to enable reactions with species in solution (25)(26)(27)(28).…”

Section: The Rapidly Developing Liquid Cell Microscopy Techniquementioning

confidence: 99%

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Opportunities and challenges in liquid cell electron microscopy

Ross

2015

Science

511

438

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Advances in seeing small things Electron microscopes, particularly those with aberration correction, can view materials at the subnanometer scale. Additional improvements make it possible to obtain images at lower electron doses, thus minimizing the damage to the sample. However, for a number of materials, particularly those of biological origin, samples need to be imaged in solution. Ross reviews recent advances that have made it possible to do liquid cell electron microscopy, which opens up the possibility of studying problems such as the changes inside a battery during operation, the growth of crystals from solution, or biological molecules in their native state. Science , this issue p. 10.1126/science.aaa9886

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Section: The Rapidly Developing Liquid Cell Microscopy Techniquementioning

confidence: 99%

Section: The Rapidly Developing Liquid Cell Microscopy Techniquementioning

confidence: 99%

Opportunities and challenges in liquid cell electron microscopy

Ross

2015

Science

511

438

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“…The past few years have seen a flare of efforts to develop devices that allow real-time, in situ imaging of dynamical, nanoscale processes in fluids with the resolution of a TEM or STEM (scanning TEM) [1][2][3][4][5][6][7][8][9][10][11][12]. Liquid-cell TEM-STEM devices confine a thin slice of liquid sample in a sealed chamber sandwiched between two electron-transparent membranes, thus preventing evaporation while allowing the electron beam to pass through the sample to produce an image.…”

Section: Introductionmentioning

confidence: 99%

In situliquid-cell electron microscopy of colloid aggregation and growth dynamics

2011

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We report on real-time observations of the aggregation of gold nanoparticles using a custom-made liquid cell that allows for in situ electron microscopy. Process kinetics and fractal dimension of the aggregates are consistent with three-dimensional cluster-cluster diffusion-limited aggregation, even for large aggregates, for which confinement effects are expected. This apparent paradox was resolved through in situ observations of the interactions between individual particles as well as clusters at various stages of the aggregation process that yielded the large aggregates. The liquid cell described herein facilitates real-time observations of various processes in liquid media with the high resolution of the electron microscope. Disciplines Engineering | Mechanical Engineering CommentsSuggested Citation: We report on real-time observations of the aggregation of gold nanoparticles using a custom-made liquid cell that allows for in situ electron microscopy. Process kinetics and fractal dimension of the aggregates are consistent with three-dimensional cluster-cluster diffusion-limited aggregation, even for large aggregates, for which confinement effects are expected. This apparent paradox was resolved through in situ observations of the interactions between individual particles as well as clusters at various stages of the aggregation process that yielded the large aggregates. The liquid cell described herein facilitates real-time observations of various processes in liquid media with the high resolution of the electron microscope.

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“…Recently, the development of TEM holders that encapsulate thin liquid layers promise in situ imaging and spectroscopy on the nanoscale. [4][5][6][7][8] Incorporating electrodes 9,10 enables in situ imaging of electrochemical processes, 11-13 electrodeposition 9 and dendrite growth. 14 However, quantitative electrochemistry in the microscope remains a major challenge: standard silicon fabrication techniques introduce electrochemically active species into the environment, and unconventional electrode shapes and configurations may lead to species migration, large background currents, and large uncompensated resistances.…”

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confidence: 99%

Nanoscale Imaging of Lithium Ion Distribution During In Situ Operation of Battery Electrode and Electrolyte

et al. 2014

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The integration of renewable, and often intermittent, energy sources such as solar and wind into the energy landscape, as well as the electrification of transportation, requires dramatic advances in electrical energy conversion and storage technologies including fuel cells, batteries and supercapacitors. TEM detection of lithium through a liquid is difficult, because lithium is a weak elastic scatterer and multiple scattering from the liquid overwhelms the inelastic core-loss signal in electron energy-loss spectroscopy (EELS). In this work, we successfully observed the lithiation state by valence energy-filtered TEM (EFTEM), which probes the low-energy regime (~1-10 eV), and allows us to work in thicker liquid layers than core-level A Baseline for Electrochemistry in the TEMWe use a liquid cell holder developed by Protochips using chips we designed to mimic a typical electrochemical cell (Figure 1a-b). The tip of the holder is a microfluidic flow cell with silicon nitride viewing membranes that confine a liquid, shown in cross section in Figure 1a. Figure 1b illustrates the top chip, with three patterned electrodes optimized for electrochemical cycling and imaging. Traditional silicon-processing methods use a chromium adhesion layer and gold electrodes. However, chromium diffuses rapidly 6 through gold (especially at grain boundaries) and can affect and even dominate the electrochemical signal. In addition, high-atomic-number electrodes such as Pt and Au obscure imaging. Instead, we used a carbon working electrode which only weakly scatters electrons and is commonly used in bulk electrochemistry, and titanium adhesion layers under platinum reference and counter electrodes. This allows us to image through the electrode with little loss in spatial resolution and contrast, which is dominated by scattering in the liquid instead. As a practical matter, and discussed below, spatial resolution is often limited by the low doses needed to control radiation damage than by beam spreading in the cell.To demonstrate that in situ electrochemistry reproduces well-established criteria, we performed cyclic voltammetry of a film of platinum, shown in Figure 1c-d, in the TEM.This control experiment represents a test case for quantitative electrochemistry, since the features are surface effects -including hydrogen adsorption and desorption and oxide formation and reduction -which are sensitive to contaminants at the sub-monolayer level.The in situ electrochemistry reproduced the characteristic voltametric profile of a polycrystalline platinum electrode at an appropriate current scale, regardless of the electron beam. In thin liquid layers, the ohmic drop in the solution becomes significant, as evidenced by the slanted curve in Figure 1d. This implies an inherent compromise between the highest spatial resolution imaging and quantitative electrochemistry.Accounting for ohmic drops in solution, this setup replicates results of a conventional electrochemical cell while obtaining nanometer resolution. 7Having established the electroch...

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The Nanoaquarium: A Platform for In Situ Transmission Electron Microscopy in Liquid Media

Cited by 125 publications

References 31 publications

Opportunities and challenges in liquid cell electron microscopy

Opportunities and challenges in liquid cell electron microscopy

In situliquid-cell electron microscopy of colloid aggregation and growth dynamics

Nanoscale Imaging of Lithium Ion Distribution During In Situ Operation of Battery Electrode and Electrolyte

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