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We report the results of a Versailles Project on Advanced Materials and Standards (VAMAS) interlaboratory study on the measurement of the shell thickness and chemistry of nanoparticle coatings. Peptide-coated gold particles were supplied to laboratories in two forms: a colloidal suspension in pure water and particles dried onto a silicon wafer. Participants prepared and analyzed these samples using either X-ray photoelectron spectroscopy (XPS) or low energy ion scattering (LEIS). Careful data analysis revealed some significant sources of discrepancy, particularly for XPS. Degradation during transportation, storage, or sample preparation resulted in a variability in thickness of 53%. The calculation method chosen by XPS participants contributed a variability of 67%. However, variability of 12% was achieved for the samples deposited using a single method and by choosing photoelectron peaks that were not adversely affected by instrumental transmission effects. The study identified a need for more consistency in instrumental transmission functions and relative sensitivity factors since this contributed a variability of 33%. The results from the LEIS participants were more consistent, with variability of less than 10% in thickness, and this is mostly due to a common method of data analysis. The calculation was performed using a model developed for uniform, flat films, and some participants employed a correction factor to account for the sample geometry, which appears warranted based upon a simulation of LEIS data from one of the participants and comparison to the XPS results.
Results are reported from a pilot study under the Consultative Committee for Amount of Substance (CCQM) to compare measurements of and resolve any relevant measurement issues in, the amount of thermal SiO2 oxide on (100) and (111) orientation Si wafer substrates in the thickness range 1.5 - 8 nm. As a result of the invitation to participate in this activity, 45 sets of measurements have been made in different laboratories using 10 analytical methods: medium-energy ion scattering spectrometry (MEIS), nuclear reaction analysis (NRA), RBS, elastic backscattering spectrometry (EBS), XPS, SIMS, ellipsometry, grazing-incidence x-ray reflectrometry (GIXRR), neutron reflectometry and transmission electron microscopy (TEM). The measurements are made on separate sets of 10 carefully prepared samples, all of which have been characterised by a combination of ellipsometry and XPS using carefully established reference conditions and reference parameters.
The results have been assessed against the National Physical Laboratory (NPL) data and all show excellent linearity. The remaining data sets correlate with the NPL data with average root-mean-square scatters of 0.15 nm, half being better than 0.1 nm and a few at or better than 0.05 nm. Each set of data allows a relative scaling constant and a zero thickness offset to be determined. Each method has an inherent zero thickness offset between 0 nm and 1 nm and it is these offsets, measured here for the first time, that have caused many problems in the past. There are three basic classes of offset: water and carbonadeous contamination equivalent to ~1 nm as seen by ellipsometry; adsorbed oxygen mainly from water at an equivalent thickness of 0.5 nm as seen by MEIS, NRA, RBS and possibly GIXRR; and no offset as seen by XPS using the Si 2p peaks. Each technique has a different uncertainty for the scaling constant and consistent results have been achieved. X-Ray photoelectron spectroscopy has large uncertainties for the scaling constant but a high precision and, critically, if used correctly, has zero offset. Thus, a combination of XPS and the other methods allows the XPS scaling constant to be determined with low uncertainty, traceable via the other methods. XPS laboratories returning results early were invited to test a new reference procedure. All showed very significant improvements. The reference attenuation lengths thus need scaling by 0.986 ± 0.009 (at an expansion factor of 2) deduced from the data for the other methods. Several other methods have small offsets and, to the extent that these can be shown to be constant or measurable, then these methods will also show low uncertainty. Recommendations are provided for parameters for XPS, MEIS, RBS and NRA to improve their accuracy.
To start the large-scale deployment of offshore wind in German waters, the German Federal Ministry for the Environment (BMU) supports the offshore test site "alpha ventus" in the North Sea with a research budget of about 50 million Euro in the next years. The overall objective of the research is to reduce the costs of offshore wind energy deployment in deep water. In order to provide all participating research projects with detailed data, the test site will be equipped with extensive measurement instrumentation.
This research initiative was named RAVE Research at Alpha VEntus and consists of a variety of projects in connection with the installation and operation of alpha ventus. As part of the RAVE initiative, so far the participating institutes and companies have prepared projects on the following topics:
Realization of the joint measurements and data management
Analysis of loads, modelling and further development of the different components of offshore wind turbines
Loads at offshore foundations and structures
Further development of LIDAR wind measuring techniques
Grid integration of offshore wind energy
Monitoring of the offshore wind energy deployment in Germany "Offshore WMEP"
Measurement of the operating noises and modelling of the sound propagation between tower and water
Ecologic research
Selective Catalytic Reduction of Nitric Oxide by Ammonia over Egg-Shell MnOx/NaY Composite Catalysts
(2002)
A novel composite catalyst system for the selective catalytic reduction (SCR) of NOx by NH3 is described operating at temperatures lower than 470 K in the presence of water with NO conversions of 80100% at space velocities of 30,00050,000 h-1. The catalyst is prepared by egg-shell precipitation of MnO2 on the external surface of zeolite NaY. Structural and thermal stability of precipitated MnO2 as well as of the MnO2/NaY composite catalyst were characterized by N2 adsorption, X-ray diffraction, laser Raman spectroscopy, temperature-programmed reduction, and electron microscopy. MnO2 precipitated on zeolite NaY (15 wt% loading) retained its amorphous state up to calcination temperatures of 775 K. The zeolite component remained structurally intact. Calcination at higher temperatures destroyed the zeolite structure and transformed MnO2 into Mn3O4. DRIFT spectroscopic investigations revealed the presence of symmetric O=NON=O species formally corresponding to N2O3 on the composite catalyst after contact with NO. Catalytic measurements under integral flow conditions showed that the catalyst performance is associated with a close coupling of nitrite formation and its drain off from equilibria with NO/NO2 and nitrate by ammonia. Several results are in line with the diazotation mechanism, including NH3 protonation to NH4+, whereas prevailing Lewis acid sites should enable NH3 activation via amide species, thus leading to a parallel amide/nitrosamide SCR reaction route. The activity-temperature profile fulfills the requirements of a low-temperature NOx reduction catalyst for mobile diesel engines if an ammonia supply is implemented on board, e.g., by urea decomposition.
The CuII complex of H4TETP (H4TETP = 1,4,8,11-tetraazatetradecane-1,4,8,11-tetrapropionic acid) is five-coordinate with a distorted square-pyramidal structure (τ = 0.45; i.e. the geometry is nearly half-way between square-pyramidal and trigonal-bipyramidal) and a relatively long Cu–N and a short Cu–O bond; the comparison between powder and solution electronic spectroscopy, the frozen solution EPR spectrum and ligand-field-based calculations (angular overlap model, AOM) indicate that the solution and solid state structures are very similar, i.e. the complex has a relatively low 'in-plane' and a significant axial ligand field with a dx²-y² ground state. The ligand-enforced structure is therefore shown to lead to a partially quenched Jahn–Teller distortion and to a relatively low complex stability, lower than with the corresponding acetate-derived ligand H4TETA. This is confirmed by potentiometric titration and by the biodistribution with 64Cu-labeled ligands which show that the uptake in the liver is significantly increased with the H4TETP-based system.
A liver biopsy specimen from a Wilson’s disease (WD) patient was analyzed by means of micro-X-ray fluorescence (mXRF) spectroscopy to determine the elemental distribution. First, bench-top mXRF was utilized for a coarse scan of the sample under laboratory conditions. The resulting distribution maps of copper and iron enabled the determination of a region of interest (ROI) for further analysis. In order to obtain more detailed elemental information, this ROI was analyzed by synchrotron radiation (SR)-based mXRF with a beam size of 4 mm offering a resolution at the cellular level. Distribution maps of additional elements to copper and iron like zinc and manganese were obtained due to a higher sensitivity of SR-mXRF. In addition to this, X-ray absorption near edge structure spectroscopy (XANES) was performed to identify the oxidation states of copper in WD. This speciation analysis indicated a mixture of copper(I) and copper(II) within the WD liver tissue.
This is a corrigendum to the original article "Determining the thickness and completeness of the shell of polymer core-shell nanoparticles by X-ray photoelectron spectroscopy, secondary ion mass spectrometry, and transmission scanning electron microscopy" that was published in "The journal of physical chemistry C", vol. 123 (2019), no. 49 pp. 29765-29775.
Core–shell nanoparticles (CSNPs) have become indispensable in various industrial applications. However, their real internal structure usually deviates from an ideal core–shell structure. To control how the particles perform with regard to their specific applications, characterization techniques are required that can distinguish an ideal from a nonideal morphology. In this work, we investigated poly(tetrafluoroethylene)–poly(methyl methacrylate) (PTFE–PMMA) and poly(tetrafluoroethylene)–polystyrene (PTFE–PS) polymer CSNPs with a constant core diameter (45 nm) but varying shell thicknesses (4–50 nm). As confirmed by transmission scanning electron microscopy (T-SEM), the shell completely covers the core for the PTFE–PMMA nanoparticles, while the encapsulation of the core by the shell material is incomplete for the PTFE–PS nanoparticles. X-ray photoelectron spectroscopy (XPS) was applied to determine the shell thickness of the nanoparticles. The software SESSA v2.0 was used to analyze the intensities of the elastic peaks, and the QUASES software package was employed to evaluate the shape of the inelastic background in the XPS survey spectra. For the first time, nanoparticle shell thicknesses are presented, which are exclusively based on the analysis of the XPS inelastic background. Furthermore, principal component analysis (PCA)-assisted time-of-flight secondary-ion mass spectrometry (ToF-SIMS) of the PTFE–PS nanoparticle sample set revealed a systematic variation among the samples and, thus, confirmed the incomplete encapsulation of the core by the shell material. As opposed to that, no variation is observed in the PCA score plots of the PTFE–PMMA nanoparticle sample set. Consequently, the complete coverage of the core by the shell material is proved by ToF-SIMS with a certainty that cannot be achieved by XPS and T-SEM.
Die nicht ionisierende elektromagnetische Strahlung im Bereich von Terahertz-Frequenzen ermöglicht berührungslose und zerstörungsfreie Mess- und Prüftechnik in zahlreichen Bereichen. Nach ersten Anwendungen in der Astronomie und der Atmosphärenforschung wurden in letzter Zeit Anwendungsfelder in der Sicherheitstechnik, der Medizintechnik, der Nachrichtentechnik und der zerstörungsfreien Prozess- und Qualitätskontrolle erschlossen. Dielektrische Materialien wie Kunststoffe und Keramiken können von Terahertz-Wellen durchdrungen werden. Das ermöglicht Untersuchungen des Objektinneren ohne spezielle Schutzmaßnahmen, wie sie z.B. beim Röntgen notwendig sind. Die Richtlinie erleichtert die Verständigung zwischen Nutzern, Herstellern und dem Vertrieb von Terahertz-Systemen. In der Richtlinie werden bekannte Einsatzgebiete sowie die eingesetzten Verfahren und Funktionsprinzipien aufgeführt, um den Leser bei der Auswahlentscheidung zu unterstützen. Nach einer kurzen Einführung in die physikalischen Grundlagen und Hinweisen zur elektromagnetischen Verträglichkeit, zum Strahlenschutz und zur regulierten Frequenzvergabe werden die verschiedenen Geräteklassen von Terahertz-Systemen ausführlich vorgestellt. Die Richtlinie gibt Hinweise zur messtechnischen Charakterisierung von Terahertz-Wellen. Einsatzgebiete von Terahertz-Systemen, wie die zerstörungsfreie Prüfung, die Dicken- und Abstandsmessung, die Tomografie und die chemische Analytik, werden mit ihren spezifischen Eigenschaften im Detail beschrieben. Umfangreiche Literaturverweise vereinfachen eine vertiefte Beschäftigung mit den Themen der Richtlinie. Eine tabellarische Übersicht mit einer Zusammenfassung, welche Terahertz-Systeme für welche Anwendungsfelder eingesetzt werden können, vervollständigt die Richtlinie.