6.1 Oberflächen- und Dünnschichtanalyse
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An inter-laboratory comparison on the surface charge, expressed as zeta potential ζ, of nanoscaled SiO2 has been performed using #14 BAM Silica (see D.5.41/5.42) nanoparticles. The comparability of results delivered by participants has been tested.
The Task 5.4 of NanoValid is designed to test, compare and validate current methods to measure and characterize physicochemical properties of selected engineered nanoparticles. The measurand is Surface charge expressed as zeta-Potential. The measurements are to be accompanied by estimates of the uncertainties at a confidence level of 95%, deduced from the standard uncertainties. Therefore an uncertainty budget comprising statistical (Type A) and systematic (Type B) errors has to be established and delivered for the measurand. The protocol comprises two Annexes addressing the establishment of uncertainty budgets following GUM. The final goal of the comparison is to identify those methods of measurement which have potential as reference methods in pc characterization of nanoparticles for the determination of a given measurand.
This Report describes an inter-laboratory comparison aiming on the establishment of the used method (BET) as a reference method. Another purpose was the certification of the porous reference material #15 BAM Titania as CRM BAM-P110 (cf. D 5.41/42). The certified values determined by nitrogen ad-sorption at 77.3 K according to the international standards ISO 15901-2 and ISO 9277 are summarized in the Table below.
An inter-laboratory comparison on the particle size, expressed as mean diameter d, of nanoscaled SiO2 (#14 BAM Silica (see NanoValid DoW, D.5.41/5.42)) has been performed. The majority of participants used Dynamic Light Scattering (DLS). A few used Electron Microscopy as method. Following methods had been applied by only one partner, respectively: Small Angle X-ray Scattering, Analytical Ultracentrifugation, Atomic Force Microscopy and Atomizer with electric mobility spectrometer.
As resistance to traditional drugs emerges for treatment of Virus infections, the need for new methods for virus inhibition increases. Graphene derivatives with large surface areas have shown strong activity against different viruses. However, the inability of current synthetic protocols to accurately manipulate the structure of graphene sheets in order to control their antiviral activity remains a major challenge. In this work, a series of graphene derivatives with defined polyglycerol sulfate and fatty amine functionalities have been synthesized and their interactions with herpes simplex Virus type 1 (HSV-1) are investigated. While electrostatic interactions between polyglycerol sulfate and virus particles trigger the binding of graphene to virus, alkyl chains induce a high antiviral activity by secondary hydrophobic interactions. Among graphene sheets with a broad range of alkyl chains, (C3–C18), the C12-functionalized sheets showed the highest antiviral activity, indicating the optimum synergistic effect between electrostatic and hydrophobic interactions, but this derivative was toxic against the Vero cell line.
In contrast, sheets functionalized with C6- and C9-alkyl chains showed low toxicity against Vero cells and a synergistic Inhibition of HSV-1. This study shows that antiviral agents against HSV-1 can be obtained by controlled and stepwise functionalization of graphene sheets and may be developed into antiviral agents for future biomedical applications.
Porous materials play an important role in several fields of technology, especially for energy applications like photovoltaics, electrolysis or batteries. The activity of porous films is affected by properties like porosity, film thickness, chemical composition of the material as well as the crystallinity of the framework. The complex morphology of such porous films constitutes a challenge even for modern analytical techniques and requires new approaches employing the combination/complementation of data of different analytical methods. In this contribution we characterize thin mesoporous iridium-titanium mixed oxide film properties by Electron Probe Microanalysis (EPMA) with energy dispersive X-ray spectroscopy (EDS) at an SEM.
Porous materials play an important role in several fields of technology, especially for energy applications like photovoltaics, electrolysis or batteries. The activity of porous films is affected by properties like porosity, film thickness, chemical composition of the material as well as the crystallinity of the framework. The complex morphology of such porous films constitutes a challenge even for modern analytical techniques and requires new approaches employing the combination/complementation of data of different analytical methods. In this contribution we characterize thin mesoporous iridium-titanium mixed oxide film properties by Electron Probe Microanalysis (EPMA) with energy dispersive X-ray spectroscopy (EDS) at an SEM.
Porous materials play an important role in several fields of technology, especially for energy applications like photovoltaics, electrolysis or batteries. The activity of porous films is affected by properties like porosity, film thickness, chemical composition of the material as well as the crystallinity of the framework. The complex morphology of such porous films constitutes a challenge even for modern analytical techniques and requires new approaches employing the combination/complementation of data of different analytical methods. In this contribution we characterize thin mesoporous iridium-titanium mixed oxide film properties by Electron Probe Microanalysis (EPMA) with energy dispersive X-ray spectroscopy (EDS) at an SEM.
Analysis of elemental composition of Fe1-xNix and Si1-xGex alloy thin films by EPMA and µ-XRF
(2019)
The present study reports on measurements on thin Fe-Ni films on silicon and first-time results of analysis on Si-Ge thin films deposited on a non-conductive aluminium oxide Substrate by electron probe microanalysis (EPMA). Standard-based and standardless EPMA (with EDS) results were used in combination with the thin film analysis software Stratagem for the quantification.
Further, X-ray fluorescence analysis (XRF) can be used for the determination of elemental composition and thickness of such films as well. In this case, XRF with a μ-focus X-ray source (μ-XRF) attached to a SEM was applied. For quantification, a fundamental parameter (FP) approach has been used to calculate standard-based and standardless results.
Both thin film systems have been chosen as samples of an international round robin test (RRT) organised in the frame of standardisation technical committee ISO/TC 201 ‘Surface chemical analysis’, under the lead of KRISS. The main objective of the RRT is to compare the results of atomic fractions of Fe1-xNix and Si1-xGex alloy films obtained by different surface Analysis techniques, such as X-ray photoelectron spectroscopy (XPS), Auger electron spectroscopy (AES), and secondary ion mass spectrometry (SIMS) applied in the depth-profiling operation mode.
Five samples of different atomic fractions of each thin film system, i.e., Fe1-xNix and Si1-xGex, have been grown by ion beam sputter deposition on silicon and Al2O3 wafers, respectively. Reference FeNi and SiGe films with well-known elemental composition and thickness have been also supplied for standard-based analysis. An excellent agreement has been obtained between the atomic fractions determined by EPMA and µ-XRF with the KRISS certified values.
Secondary fluorescence is an inevitable effect that has to be taken into account in any algorithm for quantitative electron probe microanalysis (EPMA) as an additional correction. Moreover, secondary fluorescence worsens spatial resolution of EPMA, as discussed once more in two recent papers. Secondary fluorescence is excited both by characteristic radiation and by the X-ray continuum. In most cases the correction is small. There are, however, cases, e.g. the determination of low heavy metal concentration in a light matrix, where the contribution of secondary fluorescence exceeds 10% of the measured X-ray line intensity.
For secondary fluorescence correction the measured X-ray line intensity has to be divided by the correction factor (1+I_flchar/I_p +I_flcont/I_p )≈(1+I_flchar/I_p )(1+I_flcont/I_p ) in order to get those intensity I_p, which is excited only by the primary electrons and enables the determination of specimen composition. I_flchar and I_flcont mean the calculated characteristic and continuums fluorescence intensities. In order to get the intensity of fluorescence radiation, the absorption of the exciting radiation in the specimen, the photoionization probability and the self-absorption of the emitted line must be calculated. This can be performed in a straightforward way. The critical quantity is the X-ray yield of the exciting atoms in case of fluorescence by characteristic radiation and the bremsstrahlung yield of the specimen in case of continuum fluorescence. In the former case it is reasonable to apply the same physical model to calculate I_flchar and I_p.
There are different ways how to prove the quality of the results obtained by electron microscopy and related microanalysis techniques, e.g. use of validated standard operation procedures, participation in proficiency testing exercises, use of certified reference materials, etc. International standards are able to provide requirements, specifications, guidelines or characteristics of methods, instruments or samples with the final goal that these can be used consistently in accredited laboratories. In the field of electron microscopy and microbeam analysis standardization and metrology are terms which are encountered rather seldom at major conferences and scientific publications. Nevertheless, spectra formats like EMSA/MSA for spectral-data exchange or tagged image file format (TIFF) for SEM, guidelines for performing quality assurance procedures or for the specification of X-ray spectrometers as well as of certified reference materials (CRMs) in EPMA, or measurement of average grain size by electron backscatter diffraction (EBSD), or guidelines for calibrating image magnification in SEM or TEM are ISO standards already published and used successfully by a large part of the electron microscopy and microbeam analysis community. A main and continuous task of ISO/TC 202 and its subcommittees is to identify and evaluate feasible projects/proposals needed to be developed into new international standards, particularly in respect to recent but established technology, such the silicon drift detector (SDD) EDS one.
Another international platform in the frame of which pre-standardization work can be organized is VAMAS (Versailles Project on Advanced Materials and Standards). International collaborative projects involving aim at providing the technical basis for harmonized measurements, testing, specifications, and standards to be further developed at ISO level. One key point of VAMAS activities is constituted by inter-laboratory comparisons for high-quality data. In the field of microbeam analysis, the technical working area (TWA) 37 Quantitative Microstructural Analysis deals with corresponding projects. Good ideas, e.g. on analysis of low-Z materials/elements and at low energies are particularly encouraged by directly contacting the author. Support and already available guidance will be supplied.