Ultrasonic Nebulization for TEM Sample Preparation on Single-Layer Graphene Grids

Hinman, Joshua G.; Hinman, Jordan J.; Janicek, Blanka E.; Huang, Pinshane Y.; Suslick, Kenneth S.; Murphy, Catherine J.

doi:10.1021/acs.nanolett.8b05117

Cited by 12 publications

(15 citation statements)

References 37 publications

Supporting

Mentioning

Contrasting

Order By: Relevance

“…Impressive progress in making electron guns, aberration correctors, cameras, imaging algorithms, detectors, and spectrometers with high precision and speed has greatly enhanced the spatial, temporal, and energy resolution capabilities of transmission electron microscopy (TEM) observations . What's more exciting, low acceleration voltage, environmental chambers (environmental TEM, ETEM), new sample preparation techniques, as well as various in situ methods allowing one to uncover many physical and chemical parameters are well adapted in TEM and scanning transmission electron microscopy (STEM), and thus the scope of research has been significantly expanded and intensified in recent years …”

Section: Introductionmentioning

confidence: 99%

Recent Progress of In Situ Transmission Electron Microscopy for Energy Materials

et al. 2019

View full text Add to dashboard Cite

replacing gasoline, diesel, or other types of fuels with electricity, it is expected that our world will become more environmentally friendly by storing energy directly from sustainable sources, such as solar, wind, geothermal, bioenergy, and the ocean. Even Australia, as a country with abundant energy resources, has identified energy as one of the key scientific research priorities. It is clear that the efficiency of energy harvesting and consumption must be improved, emissions must be reduced, and the integration of various energy sources into the electricity grid and chemical storage must be implemented. A desirable outlook is one with a variety of energy sources and mechanisms that significantly reduces carbon emissions and is economical for consumers and society. Recent fast-growing research should boost the development of reliable, highly efficient, low-cost, and sustainable energy materials that are effective for new technologies and that satisfy the growing demand for energy storage and climate change solutions.The progress in energy materials is indeed significant, however, as the expectations of energy materials research are always quite high, it is not sufficient. Particularly, the material performances are always theoretically predicted but are limited by the underlying mechanisms in real applications. As a wellknown example, silicon is expected to deliver a high theoretical capacity of 4200 mAh g −1 in the form of Li 4.4 Si, and is thought to replace the currently commercial graphite with a capacity of 372 mAh g −1 . However, in real applications, it is found that Si exhibits more than 360% of volume expansion during lithiation, which leads to battery anode failure. In the last few years, TEM, especially in situ TEM, has provided exceptional advantages in investigating the lithiation process of silicon anodes: direct imaging, full crystallography information, and real-time recording have all become possible. By directly observing the charge/discharge processes of Si anodes, the dynamics of expansion have been well understood. The research has then been focused on structural designs of composites containing Si to overcome the expansion. The Si composites (for instance, carbon-wrapped Si nanoparticles with different sizes) were directly analyzed by in situ TEM to determine the best structural design. [12] From 2012, in situ TEM became an essential tool to review and evaluate structural designs for high-capacity anodes with significant volume expansions. The same scenarios apply to similar research topics. In situ transmission electron microscopy (TEM) is one of the most powerfulapproaches for revealing physical and chemical process dynamics at atomic resolutions. The most recent developments for in situ TEM techniques are summarized; in particular, how they enable visualization of various events, measure properties, and solve problems in the field of energy by revealing detailed mechanisms at the nanoscale. Related applications include rechargeable batteries such as Li-ion, Na-ion, Li-O 2 , Na-O 2 , Li...

show abstract

Section: Introductionmentioning

confidence: 99%

Recent Progress of In Situ Transmission Electron Microscopy for Energy Materials

et al. 2019

View full text Add to dashboard Cite

show abstract

“…The resulting grids have monolayer graphene suspended over 2 μm holes, with approximately 70% of the holes covered across the entire 3 mm grid. 27 Figure 1b shows a low-magnification ADF-STEM image of silica-coated AuNRs deposited on the graphene substrate. A challenge in using CVD graphene substrates for colloidal nanoparticles is how to deposit nanoparticles from solution without damaging the fragile 1-atom thick substrate.…”

mentioning

confidence: 99%

“…Chemical vapor deposition (CVD) grown graphene was transferred to a TEM grid using a polymer-based transfer followed by a series of cleaning steps (see Supporting Information (SI)). The resulting grids have monolayer graphene suspended over 2 μm holes, with approximately 70% of the holes covered across the entire 3 mm grid …”

mentioning

confidence: 99%

Quantitative Imaging of Organic Ligand Density on Anisotropic Inorganic Nanocrystals

et al. 2019

Self Cite

View full text Add to dashboard Cite

A longstanding challenge in nanoparticle characterization is to understand anisotropic distributions of organic ligands at the surface of inorganic nanoparticles. Here, we show that using electron energy loss spectroscopy in an aberration-corrected scanning transmission electron microscope we can directly visualize and quantify ligand distributions on gold nanorods (AuNRs). These experiments analyze dozens of particles on graphene substrates, providing insight into how ligand binding densities vary within and between individual nanoparticles. We demonstrate that the distribution of cetyltrimethylammonium bromide (CTAB) on AuNRs is anisotropic, with a 30% decrease in ligand density at the poles of the nanoparticles. In contrast, the distribution of (16-mercaptohexadecyl)trimethylammonium bromide (MTAB) is more uniform. These results are consistent with literature reported higher reactivity at the ends of CTAB-coated AuNRs. Our results demonstrate the impact of electron spectroscopy to probe molecular distributions at soft–hard interfaces and how they produce spatially heterogeneous properties in colloidal nanoparticles.

show abstract

“…Assuming a modestly electrically conducting suspension (0.1 mS cm –1 ), droplet diameter scaling theories , suggest that with this flow rate a 50:50 water–methanol mixture yields droplets 1.2 μm in diameter and smaller. At this droplet size, the average number of nanoparticles per droplet was less than 1.0 (particle liquid phase mass concentrations were near 1.25 mg mL −1 ), reducing aerosolization based aggregation. , In addition to UMNs, size standard polystyrene latex particles (PSL) and SiO 2 particles with a reported size of 100 nm were aerosolized with a home-built pneumatic atomizer for IM-MS analysis. Aerosolization was followed by charge conditioning with a Kr-85 radioactive source, bringing the particles to a charge state distribution which is largely material independent and at which the majority of particles have charge states of −2, −1, 0, + 1, or +2. , The particles subsequently entered an atmospheric-pressure ion mobility instrument, i.e.…”

Section: Experimental Sectionmentioning

confidence: 99%

Multidimensional Nanoparticle Characterization through Ion Mobility-Mass Spectrometry

Lee

Chen

et al. 2020

Anal. Chem.

View full text Add to dashboard Cite

Multidimensional techniques that combine fully or partially orthogonal characterization methods in a single setup often provide a more comprehensive description of analytes. When applied to nanoparticles, they have the potential to reveal particle properties not accessible to more conventional 1D techniques. Herein, we apply recently developed 2D characterization techniques to nanoparticles using atmospheric-pressure ion mobility-mass spectrometry (IM-MS), and we demonstrate the analytical capability of this approach using ultraporous mesostructured silica nanoparticles (UMNs). We show that IM-MS yields a 2D particle size-mass distribution function, which in turn can be used to calculate not only important 1D distributions, i.e. particle size distributions, but also nanoparticle structural property distributions not accessible by other methods, including sizedependent particle porosity and the specific pore volume distribution function. IM-MS measurement accuracy was confirmed by measurement of NIST-certified polystyrene latex particle standards. For UMNs, comparison of IM-MS results with TEM and N 2 physisorption yields quantitative agreement in particle size and qualitative agreement in average specific pore volume. IM-MS uniquely shows how within a single UMN population, porosity increases with increasing particle size, consistent with the proposed UMN growth mechanism. In total, we demonstrate the potential of IM-MS as a standard approach for the characterization of structurally complex nanoparticle populations, as it yields size-specific structural distribution functions.

show abstract

Ultrasonic Nebulization for TEM Sample Preparation on Single-Layer Graphene Grids

Cited by 12 publications

References 37 publications

Recent Progress of In Situ Transmission Electron Microscopy for Energy Materials

Recent Progress of In Situ Transmission Electron Microscopy for Energy Materials

Quantitative Imaging of Organic Ligand Density on Anisotropic Inorganic Nanocrystals

Multidimensional Nanoparticle Characterization through Ion Mobility-Mass Spectrometry

Contact Info

Product

Resources

About