Performance of High-Resolution SEM/EDX Systems Equipped with Transmission Mode (TSEM) for Imaging and Measurement of Size and Size Distribution of Spherical Nanoparticles

Abstract

The analytical performance of high-resolution scanning electron microscopy/energy dispersive X-ray spectroscopy (SEM/EDX) for accurate determination of the size, size distribution, qualitative elemental analysis of nanoparticles (NPs) was systematically investigated. It is demonstrated how powerful high-resolution SEM is by using both mono- and bi-modal distributions of SiO2 airborne NPs collected on appropriate substrates after their generation from colloidal suspension. The transmission mode of the SEM (TSEM) is systematically employed for NPs prepared on thin film substrates such as transmission electron microscopy grids. Measurements in the transmission mode were performed by using a "single-unit" TSEM transmission setup as manufactured and patented by Zeiss. This alternative to the "conventional" STEM detector consists of a special sample holder that is used in conjunction with the in-place Everhart-Thornley detector. In addition, the EDX capabilities for imaging NPs, highlighting the promising potential with respect to exploitation of the sensitivity of the new large area silicon drift detector energy dispersive X-ray spectrometers were also investigated. The work was carried out in the frame of a large prenormative VAMAS (Versailles Project on Advanced Materials and Standards) project, dedicated to finding appropriate methods and procedures for traceable characterization of NP size and size distribution.

Shape engineered TiO2nanoparticles in Caenorhabditis elegans: a Raman imaging based approach to assist tissue-specific toxicological studies

“…More details on this method and instrumental approach, with advantages and disadvantages, have already been reported. [26][27][28] Dynamic laser scattering (DLS) analysis. DLS measurements were made using a Delsa Nano™ C Analyzer (Beckman Coulter) equipped with a 638 nm diode laser and a temperature control.…”

Analysis of Nanoscale Wear Particles from Lubricated Steel–Steel Contacts

“…At such low PE voltages, the particles at the nanoscale are no longer transparent for the electrons and the resulting contrast in the transmission T-SEM micrographs is superior to that corresponding to the high-resolution micrographs obtained e.g., with an in-lens detector. More details on the performance of the T-SEM mode used in this paper can be found in [13][14][15]. A representative example is shown in Fig.…”

Erratum to: Lateral resolution of nanoscaled images delivered by surface-analytical instruments: application of the BAM-L200 certified reference material and related ISO standards

“…This is the volume where the detected X-ray photons originate from and is typically in the range of roughly 1 μm 3 . However, recently, it has been demonstrated that SEM working in the transmission mode (TSEM) enables traceable determination of nanoparticle size distribution [23,24]. Coupling EDX to TSEM and employing thin electron transparent samples, e.g.…”