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Room temperature mechanical behavior of extruded Mg–Y–Zn alloys with varying fractions of LPSO phase was studied in tension and compression along the extrusion direction. The microstructure is characterized by elongated LPSO fibers along the extrusion direction within the magnesium matrix. Moreover, the magnesium matrix presents a bimodal grain structure with dynamically-recrystallized grains and deformed, elongated grains with the basal plane parallel to the extrusion direction. The beginning of plasticity depends on the volume fraction of deformed and DRX grains. Alloys with low volume fraction of LPSO phase(o10vol%),with a high volume fraction of deformed grains, show the typical behavior of extruded magnesium alloys where yield stress in tension is higher than in compression. This effect is, however, reversed as the volume fraction of the LPSO phase increases since DRX grains are majority.
Layer-by-layer (LbL) assembly coatings reduce the flammability of textiles and polyurethane foam but require extensive repetitive processing steps to produce the desired coating thickness and nanoparticle fire retardant content that translates into a fire retardant coating. Reported here is a new hybrid bi-layer (BL) approach to fabricate fire retardant coatings on polyurethane foam. Utilizing hydrogen bonding and electrostatic attraction along with the pH adjustment, a fast growing coating with significant fire retardant clay content was achieved. This hybrid BL coating exhibits significant fire performance improvement in both bench scale and real scale tests. Cone calorimetry bench scale tests show a 42% and 71% reduction in peak and average heat release rates, respectively. Real scale furniture mockups constructed using the hybrid LbL coating reduced the peak and average heat release rates by 53% and 63%, respectively. This is the first time that the fire safety in a real scale test has been reported for any LbL technology. This hybrid LbL coating is the fastest approach to develop an effective fire retardant coating for polyurethane foam.
KEY COMPARISON
At the October 2005 CCQM Organic Analysis Working Group Meeting (IRMM, Belgium), the decision was made to proceed with a Key Comparison study (CCQM-K47) addressing the calibration function for the determination of volatile organic compounds (VOCs) used for water quality monitoring. This was coordinated by CENAM and NIST. Benzene, o-xylene, m-xylene and p-xylene were chosen as representative VOCs. The solvent of choice was methanol.
Key Comparison CCQM-K47 demonstrated the capabilities of participating NMIs to identify and measure the four target VOCs in a calibration solution using GC-based methods. The measurement challenges in CCQM-K47, such as avoiding volatility loss, achieving adequate chromatographic resolution and isolating potential interferences, are typical of those required for value-assigning volatile reference materials. Participants achieving comparable measurements for all four VOCs in this Key Comparison should be capable of providing reference materials and measurements for VOCs in solutions when present at concentration levels greater than 10 µg/g.
The present study reports on results of analysis of the elemental composition of thin films by electron probe microanalysis with energy dispersive (ED-EPMA) X-ray spectrometry in conjunction with the dedicated thin-film analysis software package Stratagem and by X-ray fluorescence in its version with a micro-focus X-ray fluorescence (μ-XRF) source attached to a scanning electron microscope (SEM). Two thin-film systems have been analyzed: Fe1-xNix on silicon wafer and Si1-xGex on Al2O3 substrate, in both cases the layers being grown to a thickness of about 200 nm by ion beam sputter deposition. Samples of five different atomic fractions have been produced and analyzed for each thin-film system. Moreover, reference samples with certified elemental composition and thickness have been also available. This study is part of an interlaboratory comparison organized in the frame of standardization technical committee ISO/TC 201 “Surface chemical analysis.” Two laboratories have been analyzed by ED-EPMA (one laboratory standardless and one laboratory using both standardless and with standards variants) and one laboratory by μ-XRF (standardless and with standards). All the elemental compositions obtained with different methods are in very good agreement for the complete two sets of five samples each.
Room temperature mechanical behavior of extruded Mg–Y–Zn alloys with varying fractions of LPSO phase was studied in tension and compression along the extrusion direction. The microstructure is characterised by elongated LPSO fibers along the extrusion direction within the magnesium matrix. Moreover, the magnesium matrix presents a bimodal grain structure with dynamically-recrystallized grains and deformed, elongated grains with the basal plane parallel to the extrusion direction. The beginning of plasticity depends on the volume fraction of deformed and DRX grains. Alloys with low volume fraction of LPSO phase (<10 vol%), with a high volume fraction of deformed grains, show the typical behavior of extruded magnesium alloys where yield stress in tension is higher than in compression. This effect is, however, reversed as the volume fraction of the LPSO phase increases since DRX grains are majority.
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.zeige mehr
The primary crystallite size of titania powder relates to its properties in a number of applications. Transmission electron microscopy was used in this interlaboratory comparison (ILC) to measure primary crystallite size and shape distributions for a commercial aggregated titania powder. Data of four size descriptors and two shape descriptors were evaluated across nine laboratories. Data repeatability and reproducibility was evaluated by analysis of variance. One-third of the laboratory pairs had similar size descriptor data, but 83% of the pairs had similar aspect ratio data. Scale descriptor distributions were generally unimodal and were well-described by lognormal reference models. Shape descriptor distributions were multi-modal but data visualization plots demonstrated that the Weibull distribution was preferred to the normal distribution. For the equivalent circular diameter size descriptor, measurement uncertainties of the lognormal distribution scale and width parameters were 9.5% and 22%, respectively. For the aspect ratio shape descriptor, the measurement uncertainties of the Weibull distribution scale and width parameters were 7.0% and 26%, respectively. Both measurement uncertainty estimates and data visualizations should be used to analyze size and shape distributions of particles on the nanoscale.
The continual increase in energy demand and inconsistent supply have attracted attention towards sustainable energy storage/conversion devices, such as electrochemical capacitors with high energy densities and power densities. Perovskite oxides have received significant attention as anion-intercalation electrode materials for electrochemical capacitors. In this study, hollow nanospheres of nonstoichiometric cubic perovskite fluorides, KNi1-xCoxF3-delta (x = 0.2; delta = 0.33) (KNCF-0.2) have been synthesized using a localized Ostwald ripening. The electrochemical performance of the non-stoichiometric perovskite has been studied in an aqueous 3 M KOH electrolyte to categorically investigate the fluorine-vacancy-mediated charge storage capabilities. High capacities up to 198.55 mA h g-1 or 714.8 C g-1 (equivalent to 1435 F g-1) have been obtained through oxygen anion-intercalation mechanism (peroxide pathway, O-). The results have been validated using ICP (inductively coupled Plasma mass spectrometry) analysis and cyclic voltammetry. An asymmetric supercapacitor device has been fabricated by coupling KNCF-0.2 with activated carbon to deliver a high energy density of 40 W h kg-1 as well as excellent cycling stability of 98 % for 10,000 cycles. The special attributes of hollow-spherical, non-stoichiometric perovskite (KNCF-0.2) have exhibited immense promise for their usability as anion-intercalation type electrodes in supercapacitors.
ACEnano is an EU-funded project which aims at developing, optimising and validating methods for the detection and characterisation of nanomaterials (NMs) in increasingly complex matrices to improve confidence in the results and support their use in regulation. Within this project, several interlaboratory comparisons (ILCs) for the determination of particle size and concentration have been organised to benchmark existing analytical methods. In this paper the results of a number of these ILCs for the characterisation of NMs are presented and discussed. The results of the analyses of pristine well-defined particles such as 60 nm Au NMs in a simple aqueous suspension showed that laboratories are well capable of determining the sizes of these particles. The analysis of particles in complex matrices or formulations such as consumer products resulted in larger variations in particle sizes within technologies and clear differences in capability between techniques. Sunscreen lotion sample analysis by laboratories using spICP-MS and TEM/SEM identified and confirmed the TiO2 particles as being nanoscale and compliant with the EU definition of an NM for regulatory purposes. In a toothpaste sample orthogonal results by PTA, spICP-MS and TEM/SEM agreed and stated the TiO2 particles as not fitting the EU definition of an NM. In general, from the results of these ILCs we conclude that laboratories are well capable of determining particle sizes of NM, even in fairly complex formulations.