Factors influencing quantitative liquid (scanning) transmission electron microscopy

Abellán, Patricia; Woehl, Taylor J.; Parent, Lucas R.; Browning, Nigel D.; Evans, James E.; Arslan, Ilke

doi:10.1039/c3cc48479c

Cited by 155 publications

(214 citation statements)

References 33 publications

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“…18,21,22,27,28 However, recent experimental observations have shown that these effects can be quantified, controlled and mitigated using calibrated electron doses. [28][29][30] As a result, in situ TEM observations can be used as an accurate starting point for understanding nanoparticle behavior in liquids.…”

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confidence: 99%

Understanding the Role of Solvation Forces on the Preferential Attachment of Nanoparticles in Liquid

Welch¹,

Woehl²,

Park

et al. 2015

ACS Nano

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Optimization of colloidal nanoparticle synthesis techniques requires an understanding of underlying particle growth mechanisms. Non-classical growth mechanisms are particularly important as they affect nanoparticle size and shape distributions which in turn influence functional properties. For example, preferential attachment of nanoparticles is known to lead to the formation of mesocrystals, although the formation mechanism is currently not well understood. Here we employ in situ liquid cell scanning transmission electron microscopy (STEM) and steered molecular dynamics (SMD) simulations to demonstrate that the experimentally observed preference for end-to-end attachment of silver nanorods is a result of weaker solvation forces occurring at rod ends. SMD reveals that when the side of a nanorod approaches another rod, perturbation in the surface bound water at the nanorod surface creates significant energy barriers to attachment. Additionally, rod morphology (i.e. facet shape) effects can explain the majority of the side attachment effects that are observed experimentally.

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Understanding the Role of Solvation Forces on the Preferential Attachment of Nanoparticles in Liquid

Welch¹,

Woehl²,

Park

et al. 2015

ACS Nano

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“…Such changes may not always be visible immediately, but can have long term consequences for the dynamic behavior of the sample in the gas environment [31]. Observations from liquid cell in situ TEM furthermore show that ionized species formed outside the imaged area when using an overly expanded illumination can have large effects on the observed reactions [32,33]. For these reasons, we suggest that the best practice will be to always report the areal dose-rate and illumination area and keeping the latter as closely matched to the imaged area as possible.…”

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confidence: 99%

On the role of the gas environment, electron-dose-rate, and sample on the image resolution in transmission electron microscopy

Jespersen

Damsgaard

et al. 2016

Adv Struct Chem Imag

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The introduction of gaseous atmospheres in transmission electron microscopy offers the possibility of studying materials in situ under chemically relevant environments. The presence of a gas environment can degrade the resolution. Surprisingly, this phenomenon has been shown to depend on the electron-dose-rate. In this article, we demonstrate that both the total and areal electron-dose-rates work as descriptors for the dose-rate-dependent resolution and are related through the illumination area. Furthermore, the resolution degradation was observed to occur gradually over time after initializing the illumination of the sample and gas by the electron beam. The resolution was also observed to be sensitive to the electrical conductivity of the sample. These observations can be explained by a charge buildup over the electron-illuminated sample area, caused by the beam-gas-sample interaction, and by a subsequent sample motion induced by electrical capacitance in the sample.

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“…In this way platinum [3], gold [4], [5], and lead sulfide [6], for example, have been synthesized in situ. In these systems the electron beam facilitates reduction of an aqueous metallic salt precursor, so calibration and control of electron dose is crucial [7]. There has been some investigation of surfactant mediated nanoparticle growth [8], but for the most part in situ TEM techniques have not been applied to the wide variety of organic-phase nanoparticle syntheses.…”

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confidence: 99%

“…

For many nanomaterials, for example the synthesis iron oxide nanoparticles, organic phase reactions provide the necessary synthetic control [9].

…”

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confidence: 99%

Ex Situ and In Situ (S)TEM of Iron Oxide Nanoparticles Synthesized by Decomposition of an Organometallic Precursor

et al. 2015

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Developments in in situIn these systems the electron beam facilitates reduction of an aqueous metallic salt precursor, so calibration and control of electron dose is crucial [7]. There has been some investigation of surfactant mediated nanoparticle growth [8], but for the most part in situ TEM techniques have not been applied to the wide variety of organic-phase nanoparticle syntheses.For many nanomaterials, for example the synthesis iron oxide nanoparticles, organic phase reactions provide the necessary synthetic control [9]. Superparamagnetic iron oxide nanoparticles have desirable magnetic properties, combined with general biocompatibility and abundance in nature, making them attractive for a variety of biomedical applications [10]. Because properties are dependent on, for example, particle size, size distribution, morphology, crystallinity, and immediate environment [11], it is important to understand how synthetic conditions affect the growth and nucleation of nanoparticles. The most direct method for characterizing these effects is in situ TEM. Comparing the results of in situ syntheses, driven by electron beam reduction, to ex situ thermal decomposition can provide insight into the relationship between electron dose and temperature. Superparamagnetic iron oxide nanoparticles can also be expected to display unique behavior in solution; in addition to the usual solvation forces and electron beam effects, magnetic forces are also present in this system, increasing the complexity of nanoparticle interactions.Superparamagnetic iron oxide nanoparticles were synthesized by the thermal decomposition of iron(III) oleate, in 1-octadecene, with excess oleic acid acting as a surfactant. Thermal characteristics of the precursor were evaluated using thermal gravimetric analysis (TGA), differential scanning calorimetry (DSC) (both TA Instruments). Nanoparticle phase has been characterized ex situ using θ -2θ powder Xray diffraction (Bruker F8 Focus), and Raman spectroscopy (Renishaw inVia). Size and size distribution have been determined by fitting Vibrating Sample Magnetometry (VSM) results, and with TEM. Scanning TEM (STEM), bight field TEM, and selected area diffraction were performed on a 300kV Cscorrected FEI Titan with HAADF detector and GATAN CCD. For ex situ syntheses, nanoparticles in organic solvents are deposited on carbon films. In situ experiments were performed using a Hummingbird Scientific (Lacey, WA) liquid stage, with 50nm Si 3 N 4 chips.

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Factors influencing quantitative liquid (scanning) transmission electron microscopy

Cited by 155 publications

References 33 publications

Understanding the Role of Solvation Forces on the Preferential Attachment of Nanoparticles in Liquid

Understanding the Role of Solvation Forces on the Preferential Attachment of Nanoparticles in Liquid

On the role of the gas environment, electron-dose-rate, and sample on the image resolution in transmission electron microscopy

Ex Situ and In Situ (S)TEM of Iron Oxide Nanoparticles Synthesized by Decomposition of an Organometallic Precursor

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