Addressing some of the technical challenges associated with liquid phase S/TEM studies of particle nucleation, growth and assembly

Zhu, Guomin; Reiner, Holger; Cölfen, Helmut; Yoreo, James J. De

doi:10.1016/j.micron.2018.12.001

Cited by 28 publications

(29 citation statements)

References 47 publications

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“…Here, a (S)TEM device operated at an acceleration voltage of 300 kV is utilized. Use a low dose to minimize beam-induced artifacts and a short exposure time to avoid movementrelated blurring 34 .…”

mentioning

confidence: 99%

“…In case of long-term experiments, block the beam to reduce radiation damage. NOTE: Due to a better temporal resolution, TEM is to be preferred over STEM for kinetic analyses 34 and reduced ion reduction…”

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confidence: 99%

“…. STEM, however, is preferred for investigation into thick liquid layers and high-Z elements due to its higher spatial resolution in thick specimens 34…”

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confidence: 99%

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Preparation of Graphene-Supported Microwell Liquid Cells for <em>In Situ</em> Transmission Electron Microscopy

Hutzler

Fritsch

Jank

et al. 2019

JoVE

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The fabrication and preparation of graphene-supported microwell liquid cells (GSMLCs) for in situ electron microscopy is presented in a stepwise protocol. The versatility of the GSMLCs is demonstrated in the context of a study about etching and growth dynamics of gold nanostructures from a HAuCl 4 precursor solution. GSMLCs combine the advantages of conventional silicon-and graphene-based liquid cells by offering reproducible well depths together with facile cell manufacturing and handling of the specimen under investigation. The GSMLCs are fabricated on a single silicon substrate which drastically reduces the complexity of the manufacturing process compared to two-wafer-based liquid cell designs. Here, no bonding or alignment process steps are required. Furthermore, the enclosed liquid volume can be tailored to the respective experimental requirements by simply adjusting the thickness of a silicon nitride layer. This enables a significant reduction of window bulging in the electron microscope vacuum. Finally, a state-of-the-art quantitative evaluation of single particle tracking and dendrite formation in liquid cell experiments using only open source software is presented. Video Link The video component of this article can be found at https://www.jove.com/video/59751/ Here, we present the fabrication and handling of a liquid cell approach for high-performance in situ LCTEM via static graphene-supported microwell liquid cells (GSMLCs) for TEM analyses. A sketch of the GSMLC is presented in Figure 1. GSMLCs have proven to be capable of enabling in situ high-resolution transmission electron microscopy (HRTEM) results 6 and are also feasible for in situ scanning electron microscopy 29. Their Si technology-based frame allows for mass production of reproducibly shaped cells with tailored liquid thickness and extrathin membranes from a single wafer. The graphene membrane covering these cells also mitigates electron beam-induced perturbations 8,30,31

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Preparation of Graphene-Supported Microwell Liquid Cells for <em>In Situ</em> Transmission Electron Microscopy

Hutzler

Fritsch

Jank

et al. 2019

JoVE

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“…[400][401][402][403][404][405] Other related elds such as superlattice self-assembly from NPs are also treated. 406 Though some studies dealing with HNSs exist, 407,408 we envision that a more extensive application of these techniques would thrive, mainly when applied to lowertemperature reactions and some technical limitations (see, for example, a tutorial by De Yoreo and co-workers) 409 are solved.…”

Section: Perspectivementioning

confidence: 99%

Metal/semiconductor interfaces in nanoscale objects: synthesis, emerging properties and applications of hybrid nanostructures

Volokh

Mokari

2020

Nanoscale Adv.

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“…The surface scanning technique has limitations to observe the crystallization process in a solution. Upon this demand, the liquid phase electron microscope was developed, which combines the temporal and spatial resolution of electron microscopy with the ability to image events occurring in bulk solutions [17,18]. With the use of the liquid phase electron microscope, the crystallization of barium tungstate was monitored, which indicated that the complex morphologies grow through a classical growth mechanism, rather than the long-term supposing nonclassical crystallization [19].…”

Section: Introductionmentioning

confidence: 99%

In Situ Investigation of Dynamic Silver Crystallization Driven by Chemical Reaction and Diffusion

Liu

Dou

et al. 2020

Research

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Rational synthesis of materials is a long-term challenging issue due to the poor understanding on the formation mechanism of material structure and the limited capability in controlling nanoscale crystallization. The emergent in situ electron microscope provides an insight to this issue. By employing an in situ scanning electron microscope, silver crystallization is investigated in real time, in which a reversible crystallization is observed. To disclose this reversible crystallization, the radicals generated by the irradiation of electron beam are calculated. It is found that the concentrations of radicals are spatiotemporally variable in the liquid cell due to the diffusion and reaction of radicals. The fluctuation of the reductive hydrated electrons and the oxidative hydroxyl radicals in the cell leads to the alternative dominance of the reduction and oxidation reactions. The reduction leads to the growth of silver crystals while the oxidation leads to their dissolution, which results in the reversible silver crystallization. A regulation of radical distribution by electron dose rates leads to the formation of diverse silver structures, confirming the dominant role of local chemical concentration in the structure evolution of materials.

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Addressing some of the technical challenges associated with liquid phase S/TEM studies of particle nucleation, growth and assembly

Cited by 28 publications

References 47 publications

Preparation of Graphene-Supported Microwell Liquid Cells for <em>In Situ</em> Transmission Electron Microscopy

Preparation of Graphene-Supported Microwell Liquid Cells for <em>In Situ</em> Transmission Electron Microscopy

Metal/semiconductor interfaces in nanoscale objects: synthesis, emerging properties and applications of hybrid nanostructures

In Situ Investigation of Dynamic Silver Crystallization Driven by Chemical Reaction and Diffusion

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