Dynamics of gold nanoparticle clusters observed with liquid-phase electron microscopy

Cepeda-Pérez, Elisa; Jonge, Niels de

doi:10.1016/j.micron.2018.11.006

Cited by 15 publications

(15 citation statements)

References 25 publications

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“…These fluxes (Supporting Information Note 6) are low compared to typical values of 1 − 100e − /(Å 2 × s) in the LPTEM literature focusing on NP dynamics. 15,16,24,28,32,33 In a slow scanning STEM image (Figure 1b), we found that many NPs stuck to the top ( 1 ) and bottom membranes ( 2 ), as in previous studies. 28 Slow "sticky" motion was present for NPs (Figure 1b, 3 ) interacting with a membrane, as earlier reported.…”

supporting

confidence: 86%

“…28 Slow "sticky" motion was present for NPs (Figure 1b, 3 ) interacting with a membrane, as earlier reported. 15,16,23,[28][29][30][31][32][33][34][35][36] Freely moving NPs are not readily observed in a slow-scan STEM image, as they diffuse too fast compared to the acquisition time. Only an occasional NP moving favorably with respect to the raster scan direction of the beam may be observed as a short streak (Figure 1b, 4 )…”

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confidence: 99%

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Unhindered Brownian Motion of Individual Nanoparticles in Liquid-Phase Scanning Transmission Electron Microscopy

et al. 2020

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Liquid phase transmission electron microscopy (LPTEM) offers label-free imaging of nanoparticle (NP) processes in liquid with sub-nanometer spatial and millisecond temporal resolution. However, LPTEM studies have reported only on NPs moving ordersof-magnitude slower than expected from bulk aqueous liquid conditions, likely due to strong interactions with the LPTEM liquid-enclosing membranes. We demonstrate how scanning transmission electron microscope (STEM) imaging can be used to measure the motion of individual NPs and agglomerates, which are not hindered by such interactions. Only at low electron flux do we find that individual NPs exhibit Brownian motion consistent with optical control experiments and theoretical predictions for unhindered passive diffusive motion in bulk liquids. For increasing electron flux, we find increasingly faster-than-passive motion that still appears effectively Brownian. We discuss the 1 Page 1 of 23 ACS Paragon Plus Environment Nano Letters possible origins of this beam-sample interaction. This establishes conditions for the use of STEM as a reliable tool for imaging nanoscale hydrodynamics in situ TEM.

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confidence: 86%

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confidence: 99%

Unhindered Brownian Motion of Individual Nanoparticles in Liquid-Phase Scanning Transmission Electron Microscopy

et al. 2020

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“…Several prior works by our group and others have demonstrated irreversible electron beam induced aggregation of polymer ligand capped nanoparticles during LP-TEM. 4,57,64 It is plausible that electron beam induced intermolecular crosslinking and chain scission of polymer ligands will contribute to nanoparticle aggregation by reducing nanoparticle colloidal stability or covalently linking nanoparticles together. An important implication of this process is that irreversible electron beam induced aggregation of nanoparticles is a kinetically controlled process driven by radical reactions, making it distinct from selfassembly, which is a reversible process driven by interparticle interactions.…”

Section: Discussionmentioning

confidence: 99%

Visualizing Electron Beam-Capping Ligand Reactions for Controlled Nanoparticle Imaging with Liquid Phase Transmission Electron Microscopy

Dissanayake¹,

Wang²,

Woehl

2021

Preprint

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Liquid phase transmission electron microscopy (LP-TEM) enables real-time imaging of nanoparticle self-assembly, formation, and etching with single nanometer resolution. Despite the importance of organic nanoparticle capping ligands in these processes, the effect of electron beam irradiation on surface bound and soluble capping ligands during LP-TEM imaging has not been investigated. Here we use correlative LP-TEM and fluorescence microscopy (FM) to demonstrate that polymeric nanoparticle ligands undergo competing crosslinking and chain scission reactions that non-monotonically modify ligand coverage over time. Branched polyethylenimine (BPEI) coated silver nanoparticles were imaged with dose-controlled LP-TEM followed by labeling their primary amine groups with fluorophores to visualize the local thickness of adsorbed capping ligands. FM images showed that free ligands crosslinked in the LP-TEM image area over imaging times of tens of seconds, enhancing local capping ligand coverage on nanoparticles and silicon nitride membranes. Nanoparticle surface ligands underwent chain scission over irradiation times of minutes to tens of minutes, which depleted surface ligands from the nanoparticle and silicon nitride surface. Conversely, solutions of only soluble capping ligand underwent successive crosslinking reactions with no chain scission, suggesting nanoparticles enhanced the chain scission reactions by acting as radiolysis hotspots. The addition of a hydroxyl radical scavenger, tert-butanol, eliminated chain scission reactions and slowed the progression of crosslinking reactions. These experiments have important implications for performing controlled and reproducible LP-TEM nanoparticle imaging as they demonstrate the electron beam can significantly alter ligand coverage on nanoparticles in a non-intuitive manner. They emphasize the need to understand and control the electron beam radiation chemistry of a given sample to avoid significant perturbations to the nanoparticle capping ligand chemistry, which are invisible in electron micrographs.<br>

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“…However, it was shown that electron beams could induce damage to the nanomaterial and lead to aggregations, which was not observed by the conventional TEM. Similarly, Cepeda-Peŕeza et al 47 also found that electron beams can alter gold nanoparticle (Au-NPs) dynamics. Under low electron flux, Au-NPs clusters tended to shift and rotate over time.…”

Section: Different Levelsmentioning

confidence: 94%

“…In the microscope, differential pumps and apertures are used to change the pressure along the column, in order to maintain a relatively higher pressure within the chamber to achieve imaging of liquid specimens . As for another technique, closed-cell TEM, SiN is used as a cell membrane to prevent a liquid sample from being evaporated in a high-vacuum system, while allowing the full penetration of electrons. , Liquid-phase TEM is a hybrid method that combines an advanced sample carrying technique and electron microscope setup which allows the following: (i) samples protected from the high-vacuum system and electron beams; (ii) in situ characterization of engineered nanomaterials in a liquid state, and (iii) real-time recording of nanomaterial physical and chemical processes. − …”

Section: Electron Microscopymentioning

confidence: 99%

Engineered Nanomaterials’ Fate Assessment in Biological Matrices: Recent Milestones in Electron Microscopy

Cota-Ruíz

Cantu

et al. 2021

ACS Sustainable Chem. Eng.

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Engineered nanomaterials undergo a dynamic interaction with matrices such as soil, water, and biological tissues in their lifetime. The investigation and assessment of these interactions is the key to understand the implications that nanotechnology has on different aspects, including biotoxicity, therapeutic efficacy, and overall environmental sustainability. Electron microscopy (EM) is a high-resolution imaging technique that has been rapidly developed to achieve in situ, in vitro, and realtime imaging of nanomaterials in biological matrices. This perspective is the first to review the recent progress on assessing nanobio interaction at different biological levels using EM. We provide a clear picture of different EM configurations with their overall properties and a systematic summary of three main sample preparation methods, such as nanomaterials in dehydrated, frozen, and hydrated matrices. This perspective also provides a thorough discussion on the findings of the past five years on nanobio assessments using EM, such as the identification of nanocorona formation inside seeds during nanoagricultural studies; near-native structural analysis of lipid nanoparticles in nanomedicine studies; and the real-time observation of tumor cell internalization of gold nanoparticle in cancer research. Solving how engineered nanomaterials behave in a biological matrix has made a qualitative leap in nanoresearch. By summarizing recent studies, this perspective discusses the benefits and overall pitfalls of EM in aspects such as the resolution, sampling, and cost.

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Dynamics of gold nanoparticle clusters observed with liquid-phase electron microscopy

Cited by 15 publications

References 25 publications

Unhindered Brownian Motion of Individual Nanoparticles in Liquid-Phase Scanning Transmission Electron Microscopy

Unhindered Brownian Motion of Individual Nanoparticles in Liquid-Phase Scanning Transmission Electron Microscopy

Visualizing Electron Beam-Capping Ligand Reactions for Controlled Nanoparticle Imaging with Liquid Phase Transmission Electron Microscopy

Engineered Nanomaterials’ Fate Assessment in Biological Matrices: Recent Milestones in Electron Microscopy

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