A new HRSEM approach to observe fine structures of novel nanostructured materials

Asahina, Shunsuke; Uno, Shinobu; Suga, Mitsuo; Stevens, Sam M.; Klingstedt, Miia; Okano, Yasuyuki; Kudo, M.; Anderson, Michael W.; Adschiri, Tadafumi; Terasaki, Osamu

doi:10.1016/j.micromeso.2011.06.010

Cited by 9 publications

(4 citation statements)

References 23 publications

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“…33 For FE-SEM measurements, the samples were prepared by dispersing the powder samples in DI water, after which they were dropped onto the aluminium foil pieces and attached to a conductive carbon film on SEM mounts. The TEM specimens were dispersed in ethanol, and then transferred to a copper grid.…”

Section: Characterizationmentioning

confidence: 99%

“…The HRSEM was operated at a low accelerating voltage of 0.8-1.5 kV with 20% specimen bias. 33 For FE-SEM measurements, the samples were prepared by dispersing the powder samples in DI water, after which they were dropped onto the aluminium foil pieces and attached to a conductive carbon film on SEM mounts. The SEM mounts were baked in a vacuum oven at 70 1C for at least 8 hours before observation.…”

Section: Characterizationmentioning

confidence: 99%

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Synthesis of silica nanoparticles with controllable surface roughness for therapeutic protein delivery

Niu

Zhang

et al. 2015

J. Mater. Chem. B

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There is an increasing demand of efficient nano-carriers for intracellular delivery of therapeutic proteins.This study reports on a novel ''neck-enhancing'' approach to synthesize stable rough silica nanoparticles (RSNs) with controllable surface roughness. By increasing the shell particle size from 13 to 98 nm while fixing the core size at 211 nm, the interspace size between neighboring shell particles of RSNs is enlarged from 7 to 38 nm. Cytochrome c, IgG fragment and IgG antibody are preferably adsorbed onto one of the RSNs with the interspace size of 14, 21 and 38 nm, respectively. The binding activity of the IgG fragment loaded onto RSNs is maintained as confirmed by surface plasmon resonance. The hydrophobically modified RSN with the interspace size of 38 nm effectively deliver the therapeutic anti-pAkt antibody into breast cancer cells, causing significant cell inhibition by blocking pAkt and the downstream anti-apoptotic protein Bcl-2.

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Section: Characterizationmentioning

confidence: 99%

Section: Characterizationmentioning

confidence: 99%

Synthesis of silica nanoparticles with controllable surface roughness for therapeutic protein delivery

Niu

Zhang

et al. 2015

J. Mater. Chem. B

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“…One of the drawbacks of SEM is the spatial resolution of images. However, with the development of observation techniques at lower accelerating voltages and high voltage specimen bias, the resolution of SEM has been dramatically improved to directly observe the morphology and surface of nanocrystals, together with improvements in the lens detector [ 11 , 12 , 13 , 14 , 15 , 16 ]. In this study, we report the use of low-voltage high-resolution SEM and ultra-high solid angle energy-dispersive X-ray analyzer (EDS) to understand the 10–50 nm sized CeO 2 nanocrystals and nanoclusters that were synthesized by a hydrothermal reaction.…”

Section: Introductionmentioning

confidence: 99%

Direct Observation Techniques Using Scanning Electron Microscope for Hydrothermally Synthesized Nanocrystals and Nanoclusters

et al. 2021

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Metal oxide nanocrystals have garnered significant attention owing to their unique properties, including luminescence, ferroelectricity, and catalytic activity. Among the various synthetic methods, hydrothermal synthesis is a promising method for synthesizing metal oxide nanocrystals and nanoclusters. Because the shape and surface structure of the nanocrystals largely affect their properties, their analytical methods should be developed. Further, the arrangement of nanocrystals should be studied because the properties of nanoclusters largely depend on the arrangement of the primary nanocrystals. However, the analysis of nanocrystals and nanoclusters remains difficult because of their sizes. Conventionally, transmission electron microscopy (TEM) is widely used to study materials in nanoscale. However, TEM images are obtained as the projection of three-dimensional structures, and it is difficult to observe the surface structures and the arrangement of nanocrystals using TEM. On the other hand, scanning electron microscopy (SEM) relies on the signals from the surface of the samples. Therefore, SEM can visualize the surface structures of samples. Previously, the spatial resolution of SEM was not enough to observe nanoparticles and nanomaterials with sizes of between 10 and 50 nm. However, recent developments, including the low-landing electron-energy method, improved the spatial resolution of SEM, which allows us to observe fine details of the nanocluster surface directory. Additionally, improved detectors allow us to visualize the elemental mapping of materials even at low voltage with high solid angle. Further, the use of a liquid sample holder even enabled the observation of nanocrystals in water. In this paper, we discuss the development of SEM and related observation technologies through the observation of hydrothermally prepared nanocrystals and nanoclusters.

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“…High-resolution SEM (HR-SEM) was developed with an improved objective lens capable of providing three-dimensional images of mesopore openings. The surface structure and pore system of SBA-15 and its carbon replica, CMK-5, have been studied by using HR-SEM and scanning transmission electron microscopy (STEM). − In addition, the deceleration method , and the Ar-ion-beam cross-sectioning technique , enable one to obtain cross-sectional images that represent fine surface structures.…”

Section: Introductionmentioning

confidence: 99%

Interconnected 3D Framework of CeO₂ with High Oxygen Storage Capacity: High-Resolution Scanning Electron Microscopic Observation

Lü

Asahina

Takami

et al. 2020

ACS Appl. Nano Mater.

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CeO 2 nanocasting in a mesoporous hard template provides a threedimensionally (3D) interconnected skeleton framework consisting of CeO 2 nanoparticles with particles smaller than 7 nm. Low-voltage high-resolution scanning electron microscopy with Ar-ion-beam cross-sectional polishing revealed numerous CeO 2 (∼250 nm) clusters distributed in the SBA-15 mesochannels. Each CeO 2 framework consists of CeO 2 primary nanocrystals that are mutually and coherently connected. The mesochannel walls of the mesoporous silica might confine the growth of the CeO 2 nanocrystals, resulting in a high oxygen storage capacity of the material. A series of cross-sectional images obtained by using damage-free Ar-ion-beam polishing revealed the mechanism of pore filling and CeO 2 structuring process: that from the nucleation and growth of the CeO 2 in the mesopores to the self-organization of nanocrystals that form multiple nanowires along the mesochannels. Furthermore, self-organized nanowires were arranged periodically and were mutually connected finally to form a negative replica of the ordered mesoporous SBA-15 silica.

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A new HRSEM approach to observe fine structures of novel nanostructured materials

Cited by 9 publications

References 23 publications

Synthesis of silica nanoparticles with controllable surface roughness for therapeutic protein delivery

Synthesis of silica nanoparticles with controllable surface roughness for therapeutic protein delivery

Direct Observation Techniques Using Scanning Electron Microscope for Hydrothermally Synthesized Nanocrystals and Nanoclusters

Interconnected 3D Framework of CeO₂ with High Oxygen Storage Capacity: High-Resolution Scanning Electron Microscopic Observation

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A new HRSEM approach to observe fine structures of novel nanostructured materials

Cited by 9 publications

References 23 publications

Synthesis of silica nanoparticles with controllable surface roughness for therapeutic protein delivery

Synthesis of silica nanoparticles with controllable surface roughness for therapeutic protein delivery

Direct Observation Techniques Using Scanning Electron Microscope for Hydrothermally Synthesized Nanocrystals and Nanoclusters

Interconnected 3D Framework of CeO2 with High Oxygen Storage Capacity: High-Resolution Scanning Electron Microscopic Observation

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Interconnected 3D Framework of CeO₂ with High Oxygen Storage Capacity: High-Resolution Scanning Electron Microscopic Observation