<i>In situ</i> liquid-cell transmission electron microscopy for direct observation of concentration-dependent growth and dissolution of silver nanoparticles

Ahn, Tai Young; Hong, Seungpyo; Kim, Seong‐Il; Kim, Yong Woon

doi:10.1039/c5ra14879k

Cited by 18 publications

(11 citation statements)

References 33 publications

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“…These results conrmed that the electron-dose-dependent LCTEM is reversible and correlates with the predictions of the TDR diagrams, where the Au NPs' precipitation or dissolution at an ambient temperature is positively correlated with the variations in the Au redox concentration ratio, i.e., [Au 0 ]/[Au + ] as a function of the electron dose rate. Similar precipitation/dissolution trends were observed in studies by Schneider et al 11 and Ahn et al 16 Fig . 7 shows TEM micrographs of the precipitation/ dissolution of the Au NPs as a function of temperature between 25 C and 40 C over a period of 1200 s. The electron dose rate was xed at 6 Â 10 8 Gy s À1 , at an initial temperature of 25 C, just below the experimentally determined boundary conditions for the Au NPs' precipitation.…”

Section: Model Verication Based On Au Precipitation/dissolution Liqusupporting

confidence: 89%

“…11,12,[15][16][17][18][19][20][21] Dynamic LCTEM has tremendous potential when it comes to probing and understanding the underlying mechanisms of nucleation and the early growth stages of nanomaterials. 9,16 On the other hand, there are major challenges related to the interaction effects between the electron beam and the solvent, which can modify the reaction kinetics to such an extent that they can no longer be directly related to the experiments. 21 It is well documented that these effects are the result of water radiolysis due to the interaction between water and the energyintense (80-300 keV) electron beam.…”

Section: Introductionmentioning

confidence: 99%

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Controlling the radical-induced redox chemistry inside a liquid-cell TEM

et al. 2019

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Section: Model Verication Based On Au Precipitation/dissolution Liqusupporting

confidence: 89%

Section: Introductionmentioning

confidence: 99%

Controlling the radical-induced redox chemistry inside a liquid-cell TEM

et al. 2019

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“…Liquid cell scanning/transmission electron microscopy (LC-S/TEM) is an emerging technology allowing direct and real-time observations of dynamic processes in solution. − Conventional LCs commonly consist of two 50 nm thick amorphous silicon nitride membranes, which confine the liquid sample in a volume determined by spacers, ranging from 50 nm to 5 μm. So far the method has successfully been applied to observe chemical reactions and the behavior of nanomaterials in solution at the nanometer scale, including nucleation, − growth, − self-assembly, − and particle degradation. − When the cell is inside the TEM, the pressure difference between the interior of the liquid cell and the microscope vacuum causes the ∼50 nm thick silicon nitride membranes to bulge out, resulting in a liquid thickness greater than the designed spacing between the two chips. Since the thickness of the LC determines the resolution, the bulging of the membranes further decreases the image resolution. , Alternatively, noncommercial graphene liquid cells (GLCs) provide the opportunity to observe nanoparticles at the true atomic level.…”

mentioning

confidence: 99%

Atomic Mechanisms of Nanocrystallization via Cluster-Clouds in Solution Studied by Liquid-Phase Scanning Transmission Electron Microscopy

et al. 2021

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The formation of nanocrystals is at the heart of various scientific disciplines, but the atomic mechanisms underlying the early stages of crystallization from supersaturated solutions are still rather unclear. Here, we used in situ liquid-phase scanning transmission electron microscopy to study at the atomic level the very early stages of gold nanocrystal growth, and the evolution of its crystallinity. We found that the nucleation is initiated by the formation of poorly crystalline nanoparticles. These are transformed into monocrystals via nanocrystallization governed by a complex process of multiple out-and-in exchanges of matter between a crystalline-core and a disordered-shell, referred to as the cluster-cloud. Our observations at the crystal/cluster-cloud interface during growth demonstrate that the initially formed nanocrystals expel the poorly crystallized phases as nanoclusters into the cluster-cloud, then readsorb it by two distinct pathways, namely, by (i) monomer attachments and (ii) nanocluster coalescence. This growth process eventually leads to the formation of monocrystalline nanoparticles.

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“…It is noted that besides nanoparticle growth, etching of nanoparticles has also been observed in liquid cells , Schneider et al and others − showed that the electron beam plays an important role in crystallization as well as etching. Thus, quantitative studies of the effects of the electron beam are necessary to elucidate the growth mechanisms observed in a liquid cell under TEM.…”

Section: Nucleation and Growth Of Colloidal Nanocrystalsmentioning

confidence: 99%

Visualization of Colloidal Nanocrystal Formation and Electrode–Electrolyte Interfaces in Liquids Using TEM

Zeng

Zheng

2017

Acc. Chem. Res.

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Transmission electron microscopy (TEM) has become a powerful analytical tool for addressing unique scientific problems in chemical sciences as well as in materials sciences and other disciplines. There has been a lot of recent interest in the development and applications of liquid phase environmental TEM. In this Account, we review the development and applications of liquid cell TEM for the study of dynamic phenomena at liquid-solid interfaces, focusing on two areas: (1) nucleation, growth, and self-assembly of colloidal nanocrystals and (2) electrode-electrolyte interfaces during charge and discharge processes. We highlight the achievements and progress that have been made in these two topical areas of our studies. For example, tracking single platinum particle growth trajectories revealed that two different pathways of growth, either by monomer attachment or coalescence between nanoparticles, led to the same particle size. With the improved spatial resolution and fast electron detection, we were able to trace individual facet development during platinum nanocube platinum nanocube growth. The results showed that different from the surface energy minimization rule prediction, the growth rates of all low-energy facets, such as {100}, {110}, and {111}, were similar. The {100} facets stopped growth early, and the continuous growth of the rest facets resulted in a nanocube. Density functional theory calculations showed that the amine ligands with low mobility on the {100} facets blocked the further growth of the facets. The effect of the ligand on nanoparticle shape evolution were further studied systematically using a Pt-Fe nanoparticle system by changing the oleylamine concentration. With 20%, 30%, or 50% oleylamine, Pt-Fe nanowires or nanoparticles with different morphologies and stabilities were achieved. Real-time imaging of nanoparticles in solution also enabled the study of interactions between nanoparticles during self-assembly. We further compared the study of noble-metal nanoparticles and transition-metal oxides in a liquid cell to elucidate the nanoparticle formation mechanisms. In the second part of this Account, we review the study of electrolyte-electrode interfaces by the development of electrochemical liquid cell TEM. The formation of single-crystalline Pb dendrites from polycrystalline branches and Li dendrite growth in a commercial electrolyte for Li ion batteries were observed. We also studied lithiation reactions of MoS and Au electrodes. MoS nanoflakes on the Ti electrode underwent irreversible decomposition, resulting in the vanishing of the MoS active nanoflakes. More detailed study using nanobeam diffraction indicated that the MoS nanoflakes were broken down into small nanoparticles as a result of the fast discharge. For the lithiation of Au electrodes, three distinct types of morphology changes during reactions were revealed, including gradual dissolution, explosive reaction, and local expansion/shrinkage. Additionally, we studied electrolyte decomposition reactions such as bubble formation a...

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In situ liquid-cell transmission electron microscopy for direct observation of concentration-dependent growth and dissolution of silver nanoparticles

Cited by 18 publications

References 33 publications

Controlling the radical-induced redox chemistry inside a liquid-cell TEM

Controlling the radical-induced redox chemistry inside a liquid-cell TEM

Atomic Mechanisms of Nanocrystallization via Cluster-Clouds in Solution Studied by Liquid-Phase Scanning Transmission Electron Microscopy

Visualization of Colloidal Nanocrystal Formation and Electrode–Electrolyte Interfaces in Liquids Using TEM

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