Filtern
Erscheinungsjahr
Dokumenttyp
- Zeitschriftenartikel (95)
- Beitrag zu einem Tagungsband (40)
- Beitrag zu einem Sammelband (17)
- Forschungsbericht (9)
- Posterpräsentation (4)
- Buchkapitel (2)
- Vortrag (2)
- Sonstiges (2)
- Corrigendum (1)
Sprache
- Englisch (125)
- Deutsch (44)
- Mongolisch (3)
Schlagworte
- Geruch (8)
- Drop test (6)
- XPS (6)
- Bauprodukte (5)
- Corrosion (5)
- Dangerous goods packagings (4)
- Structural dynamics (4)
- VOC (4)
- X-ray refraction (4)
- AgBB-Schema (3)
Organisationseinheit der BAM
- 8 Zerstörungsfreie Prüfung (19)
- 6 Materialchemie (11)
- 8.5 Röntgenbildgebung (9)
- 5 Werkstofftechnik (8)
- 5.6 Glas (8)
- 6.1 Oberflächen- und Dünnschichtanalyse (8)
- 1 Analytische Chemie; Referenzmaterialien (6)
- 4 Material und Umwelt (5)
- 7 Bauwerkssicherheit (5)
- 3 Gefahrgutumschließungen; Energiespeicher (4)
Paper des Monats
- ja (1)
Eingeladener Vortrag
- nein (2)
Metal-Assisted and Solvent-Mediated Synthesis of Two-Dimensional Triazine Structures on Gram Scale
(2020)
Covalent triazine frameworks are an emerging material class that have shown promising performance for a range of applications. In this work, we report on a metal-assisted and solvent-mediated reaction between calcium carbide and cyanuric chloride, as cheap and commercially available precursors, to synthesize two-dimensional triazine structures (2DTSs). The reaction between the solvent, dimethylformamide, and cyanuric chloride was promoted by calcium carbide and resulted in dimethylamino-s-triazine intermediates, which in turn undergo nucleophilic substitutions. This reaction was directed into two dimensions by calcium ions derived from calcium carbide and induced the formation of 2DTSs. The role of calcium ions to direct the two-dimensionality of the final structure was simulated using DFT and further proven by synthesizing molecular intermediates. The water content of the reaction medium was found to be a crucial factor that affected the structure of the products dramatically. While 2DTSs were obtained under anhydrous conditions, a mixture of graphitic material/2DTSs or only graphitic material (GM) was obtained in aqueous solutions. Due to the straightforward and gram-scale synthesis of 2DTSs, as well as their photothermal and photodynamic properties, they are promising materials for a wide range of future applications, including bacteria and virus incapacitation.
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.
The stress–strain behavior of ceramics, such as aluminum titanate, has certain features that are unusual for brittle materials—in particular, a substantial nonlinearity under uniaxial tension, and load–unload hysteresis caused by the sharp increase of the incremental stiffness at the beginning of unloading. These features are observed experimentally and are attributed to microcracking. Here we compare different degrees of stress–strain nonlinearity of aluminum titanate materials and quantitatively model them. We use advanced mechanical testing to observe the mechanical response at room and high temperature; electron microscopy, and X-ray refraction radiography to observe the microstructural changes. Experiments show that two types of microcracks can be distinguished: (i) microcracks induced by cooling from the sintering temperature (due to heterogeneity and anisotropy of thermal expansion), with typical sizes of the order of grain size, and (ii) much larger microcracks generated by the mechanical loading. The two microcrack types produce different effects on the stress–strain curves. Such microcracks and the features of the stress–strain behavior depend on the density of the cooling-induced microcracks and on the distribution of grain sizes. They are modeled analytically and numerically.
Messung der empfundenen Geruchsintensität mit Multigas-Sensorsystemen, das Forschungsvorhaben SysPAQ
(2007)
Measuring perceived air quality and intensity by a Sensor System, the European Project SysPAQ
(2008)
Die Bewertung von VOC-Emissionen aus Bauprodukten soll durch das AgBB-Schema vereinheitlicht werden und eine gesundheitsrelevante Komponente enthalten. Das Deutsche Institut für Bautechnik (DIBt) hat das AgBB-Schema in weiten Teilen für seine Grundsätze zur gesundheitlichen Bewertung von Bauprodukten in Innenräumen implementiert. Neben der üblichen chemischen Emissionsmessung soll auch der Geruch für die Bewertung des Produkts herangezogen werden. Um den Geruch als festen Bestandteil in die Produktprüfung zu integrieren, wurden vom Umweltbundesamt zwei Vorhaben initiiert. Erste Ergebnisse des zweiten Vorhabens (FKZ 37 07 62 300; Sensorische Bewertung der Emissionen aus Bauprodukten Integration in die Vergabegrundlagen für den Blauen Engel und das Bewertungsschema des Ausschusses zur gesundheitlichen Bewertung von Bauprodukten) werden hier dargestellt.
Emissionen aus Bauprodukten beeinträchtigen die Qualität der Innenraumluft erheblich. Mit Hilfe des AgBB-Schemas werden die Emissionen flüchtiger organischer Verbindungen (VOC) aus Bauprodukten bewertet. Die gesundheitliche Bewertung nach dem AgBB-Schema erfordert produktspezifische Messverfahren.
Diese gibt es mittlerweile für eine Reihe von Produkten. Sie wurden durch Beteiligung verschiedener Forschungseinrichtungen und Messinstitute validiert und u. a. in die Vergabekriterien des Umweltzeichens Blauer Engel übernommen. Die Bewertung ist allerdings mit zumeist niedrigeren Grenzwerten strenger. VOC-Emissionen und Gerüche können beide zu gesundheitlichen Belastungen führen. So ist die sensorische Prüfung ein weiteres wichtiges Element bei der Bewertung von Bauprodukten und vorsorglich auch im AgBB-Schema verankert.
Hauptziel des Projektes ist es, eine Methode der sensorischen Bewertung und Grenzen für die Vergabe des Blauen Engels und für das AgBB-Schema abzuleiten. Auf Grundlage der durchgeführten Untersuchungen (siehe Kapitel 5 Ergebnisse und Diskussion) wird als Bewertungsmethode die empfundene Intensität und die Hedonik vorgeschlagen. Die Ableitung der Grenzwerte für die sensorische Bewertung am 28. Tag erfolgt über die zusätzliche Befragung der Probanden im Rahmen der vorliegenden Studie nach der Zumutbarkeit einer Probe.
Für den Blauen Engel könnte es je Produktgruppe unterschiedliche Grenzen der empfundenen Intensität und der Hedonik geben. Ein erster Vorschlag für mögliche Grenzen, hier zunächst einheitlich für alle
Produktgruppen, ist für die empfundene Intensität 7 pi (5 pi + 2 pi als Sicherheit, Kapitel 5.1.5) und für die Hedonik -1 (0 +/-0,8, gerundet auf -1) (siehe dazu Abbildung 6-2).
Emissions from building products can considerably impair the quality of indoor air. The AgBB scheme is employed to evaluate the emissions of volatile organic compounds (VOC) from building products. The hygienic evaluation according to the AgBB scheme requires product-specific measuring procedures.
These are available for a range of products. They have been validated in co-operation with several research and testing institutes and have been included in the criteria for awarding the Blue Angel ecolabel.
The evaluation is, however, stricter and generally has lower limits. VOC emissions and odours can cause health problems so testing using sensors is an important element in the evaluation of building products and has – for reasons of precaution – been set down in the AgBB scheme. The main goal of the project was to derive a method of evaluation using sensors and limits for awarding the Blue Angel and for the AgBB scheme. Based on the research conducted (see Chapter 5 Results and Discussion), perceived intensity and hedonics were suggested as a suitable Evaluation method. The derivation of limits for the evaluation using sensors on the 28th day was effected in the present study through the additional questioning of the test subjects on the reasonability of a sample.
For the Blue Angel, there could be different limits of perceived intensity and hedonics for each group of products. A preliminary suggestion for possible limits – for all product groups – is a perceived intensity of 7 pi (5 pi + 2 pi as confidence coefficient, Chapter 5.1.5) and -1 (0+/-0.8, rounded to -1) for the hedonic value.
There is a strong need for cost-effective mitigation measures for
turnouts. SBB has initiated a series of examinations using different methodologies to gain a deeper understanding of the excitation mechanisms at low frequencies, in addition to that obtained in the RIVAS project. To date it is not yet clear what constitutes a complete measurement data set that would enable understanding most of the vibration excitation mechanisms in turnouts. Increasing vibration at turnouts in comparison to normal track is observed for all measured frequencies.
The different methodologies are presented in the paper. Under-sleeper pads (USP) are a cost-effective method to reduce vibration at frequencies above 63 Hz (1/3 octave), but there is probably no improvement for frequencies below 63 Hz. A first test of new frog geometry did not show relevant improvements in Vibration emission in comparison to a reference frog geometry. Axle box acceleration measurements are an interesting method to identify defects in a turnout. A specialized measurement system of rail roughness could identify certain geometry Problem areas for some frogs. Noise increases also are observed at turnouts for frequencies ranging between 80 to 1000 Hz. The use of railway source models to calculate
contact forces for ballasted track and turnouts seems promising, in particular for understanding the influence of ground.
The most profound consequences of the presence of Ca–Mg carbonates (CaCO3–MgCO3) in the Earth’s upper mantle may be to lower the melting temperatures of the mantle and control the melt composition.
Low-degree partial melting of a carbonate-bearing mantle produces CO2-rich, silica-poor melts compositionally imposed by the melting relations of carbonates. Thus, understanding the melting relations in the CaCO3–MgCO3 system facilitates the interpretation of natural carbonate-bearing silicate systems.
We report the melting relations of the CaCO3–MgCO3 system and the partition coefficient of trace elements between carbonates and carbonate melt from experiments at high pressure (6 and 9 GPa) and temperature (1300–1800 ◦C) using a rocking multi-anvil press. In the absence of water, Ca–Mg carbonates are stable along geothermal gradients typical of subducting slabs. Ca–Mg carbonates (∼ Mg0.1–0.9Ca0.9–0.1CO3) partially melt beneath mid-ocean ridges and in plume settings. Ca–Mg carbonates melt incongruently, forming periclase crystals and carbonate melt between 4 and 9 GPa. Furthermore, we show that the rare earth element (REE) signature of Group-I kimberlites, namely strong REE fractionation and depletion of heavy REE relative to the primitive mantle, is resembled by carbonate melt in equilibrium with Ca-bearing magnesite and periclase at 6 and 9 GPa. This suggests that the dolomite–magnesite join of the CaCO3–MgCO3 system might be useful to approximate the REE signature of carbonate-rich melts parental to kimberlites.
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.
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.
Bioresorbable carriers for subchondral anchoring of tissue-engineered cartilage in articular defects
(2000)
Zusammenfassung Im Rahmen eines Forschungsvorhabens an der RWTH Aachen wurden mehrere Spannbetondurchlaufträger bis zum Versagen belastetet. Neben umfangreicher konventioneller Messtechnik wurden zusätzlich innovative Messmethoden durch die Bundesanstalt für Materialforschung und –prüfung (BAM) getestet. Darunter waren eingebettete Ultraschall-Transducer, deren Daten mit einer neuartigen Methode, der Codawelleninterferometrie (CWI), ausgewertet wurden. Dieses Verfahren detektiert auch kleinste Änderungen im Signal und in der Wellengeschwindigkeit gegenüber einer Referenzmessung. Hiermit können Belastungs- und Strukturänderungen sowie Schäden sehr viel sensibler angezeigt werden als bei konventionellen Ultraschallmessungen. Durch eine Modifikation des Verfahrens mit gleitender Referenz können aber auch starke Veränderungen im Material, wie sie bei Bruchversuchen auftreten, erfasst werden. In den Versuchen gelang es mit Netzwerken aus bis zu 20 Ultraschall-Transducern, Spannungskonzentrationen und Rissbildungen qualitativ zu detektieren und zu verfolgen, ohne dass die Sensoren direkt am Ort der Änderung angebracht sein müssen.
The hydrogen tightness of high-pressure hydrogen storage is a Basic criterion for long-term storage. The H2 permeation coefficients of epoxy resin and a glass lacquer were determined to enable the geometric optimization of a glass capillary storage. It was found that the curing conditions have no significant influence on the H2 permeation coefficient of resin.
The H2 permeation coefficient of epoxy resin is only about three orders of Magnitude greater than that of borosilicate glass. This suggests that the initial pressure of 700 bar takes about 2.5 years to be halved in capillary array storage. Therefore, a high-pressure hydrogen storage tank based on glass capillaries is ideally suited for long-term storage in mobile applications.
. Hard coated steel components are used in a wide application range, mostly for protective, wear resistant and decorative purposes. Despite of these coatings being regarded as relatively dense, there is always a high risk of localized corrosion when a coated low alloyed steel component encounters a surrounding high humidity atmosphere or even an aqueous medium. An approach to enhance the corrosion properties is the addition of magnesium to physical vapor deposited hard coatings, like TiN. It has been found that there is a remarkable increase in corrosion resistance in dependence of magnesium content of the TiMgN coating and its surface properties. In this work the authors will explain the underlying corrosion protection mechanisms by means of electrochemical and analytical studies. The positive impact of magnesium in the coating relates on its preferred dissolution vs. steel. This causes the potential to shift to more negative direction with respect to the steel substrate and additionally leads to a temporarily passivation of the steel due to alkalization of the surrounding electrolyte by formation of magnesium hydroxide.
Processing ultrasonic data by coda wave interferometry to monitor load tests of concrete beams
(2018)
Ultrasonic transmission measurements have been used for decades to monitor concrete elements, mostly on a laboratory scale. Recently, coda wave interferometry (CWI), a technique adapted from seismology, was introduced to civil engineering experiments. It can be used to reveal subtle changes in concrete laboratory samples and even large structural elements without having a transducer directly at the place where the change is taking place. Here, several load tests until failure on large posttensioned concrete beams have been monitored using networks of embedded transducers. To detect subtle effects at the beginning of the experiments and cope with severe changes due to cracking close to failure, the coda wave interferometry procedures had to be modified to an adapted step-wise approach. Using this methodology, we were able to monitor stress distribution and localize large cracks by a relatively simple technique. Implementation of this approach on selected real structures might help to make decisions in infrastructure asset management.
Hard coated steel components are used in a wide application range, mostly for protective, wear resistant and decorative purposes. Despite of these coatings being regarded as relatively dense, there is always a high risk of localized corrosion when a coated low alloyed steel component encounters a surrounding high humidity atmosphere or even an aqueous medium. An approach to enhance the corrosion properties is the addition of magnesium to physical vapor deposited hard coatings, like TiN. It has been found that there is a remarkable increase in corrosion resistance in dependence of magnesium content of the TiMgN coating and its surface properties. In this work the authors will explain the underlying corrosion protection mechanisms by means of electrochemical and analytical studies. The positive impact of magnesium in the coating relates on its preferred dissolution vs. steel. This causes the potential to shift to more negative direction with respect to the steel substrate and additionally leads to a temporarily passivation of the steel due to alkalization of the surrounding electrolyte by formation of magnesium hydroxide.
Hard and wear resistant coatings deposited by PVD techniques have been characterized for decades for their capabilities to protect steel substrates from corrosion. In the present work the effect of Mg incorporated into TiN coatings is described in terms of the corrosion behavior as well as the mechanical and structural properties.
TiN and TiMgN films with Mg contents between 10 and 35 at.% were deposited onto mirror polished 100Cr6 (1.3505) steel samples with 2.5 and 5 μm thickness by using DC magnetron sputtering. The corrosion protection capabilities of the coatings were characterized by neutral salt spray (NSS) test, considering the amounts and sizes of growth defects inherent in each coated sample as determined by a recently developed optical scan method (Large Area High Resolution mapping). The defect data were statistically analyzed for improved interpretation of NSS test results. Chosen growth defects were additionally analyzed by focused ion beam technique. Furthermore the coating composition and morphology, the hardness and the tribological behavior were characterized.
Polished steel samples coated with 2.5 μm TiMgN containing about 35 at.% Mg were in the plane free of corrosion after 24 h in a NSS test. TiMgN with 10 or 20 at.% Mg only provided a slightly improved corrosion protection in relation to pure TiN coatings, which was limited to certain types of growth defects. The highest Mg containing coatings exhibited a decreased hardness down to 1200 or 1800 HV depending on type of deposition (HV 1200: Ti- and Mg-target with rotating substrate holder, 1800: Mg-plugged Ti-target with static substrate holder), but also showed a strongly improved wear resistance against Al2O3 related to pure TiN. By analyzing the NSS test results it was found that the corrosion behavior of the coated samples did not only depend strongly on the Mg content, but also on the sample individual defect concentrations. Therefore this subject is extensively discussed.
We present a handheld fiber-coupled terahertz spectrometer operating at a center wavelength of 1550 nm. The key elements are a fs-fiber laser, a fiber stretcher delay line and fiber-coupled antennas, which contain novel InAlAs-InGaAs multi layer chips. First experimental data obtained with this system demonstrates its great potential and robustness. In addition, we investigate different hazardous and harmless liquids in reflection geometry. These experiments show that liquids are in principle distinguishable by terahertz spectroscopy. Finally, first steps towards an algorithm that allows for an extraction of the liquids dielectric properties are discussed. The algorithm works for the analysis of reflection data even if the liquid is located inside a container.
Other than commonly assumed the relaxation times observed in the electrical low-frequency range (1 mHz – 40 kHz) of natural porous media like sandstones and tuff stones cannot be directly related to the dominant (modal) pore throat sizes, measured (e.g.) with mercury intrusion porosimetry (MIP). Working with a great variety of sandstones from very different origins and featuring great variations in textural and chemical compositions as well as in geometrical pore space properties, it was observed that particularly samples with narrow pore throats were characterized by long (low-frequency) relaxations. These, however, can (following the current theories) be rather explained by long “characteristic length scales” in these media or low diffusion coefficients along the electrical double layer. However, there is no straightforward way (or single approved method) of getting reliable numbers for properties such as the lengths of pore throats, the diameter and length of the wide pores and their respective distributions. Consequently we follow a multi-methodical approach and combine the benefits of MIP, micro-computed tomography (μ-CT) and nuclear magnetic resonance (NMR) to achieve much deeper insight due to the different resolutions and sensitivities to either pore constrictions (throats) or wide pores. This helps us to understand, whether the observed electrical relaxation phenomena actually depend on geometric length scales or rather on other properties such as chemical composition, clay content, clay type or cation exchange capacity. In this paper, we showcase selected results of a systematic study of a total of 16 sandstones and three tuffs. Findings and the particular advantage of the used method combination are discussed and shown in detail for a representative sample selection.
Glass-ceramics are noted for their unusual combination of properties and manifold commercialized products for consumer and specialized markets. Evolution of novel glass and ceramic processing routes, a plethora of new compositions, and unique exotic nano- and microstructures over the past 60 years led us to review the Definition of glass-ceramics. Well-established and emerging processing methods, such as co-firing, additive manufacturing, and laser patterning are analyzed concerning the core requirements of processing glass-ceramics and the Performance of the final products. In this communication, we propose a revised, updated definition of glass-ceramics, which reads “Glass-ceramics are inorganic, non-metallic materials prepared by controlled crystallization of glasses via different processing methods. They contain at least one type of functional crystalline phase and a residual glass. The volume fraction crystallized may vary from ppm to almost 100%”.
Glasses with compositions of 21Gd2O3-63MoO3-(16-x)B2O3-xTeO2 (mol%) (x= 0, 2, 4, 8) were prepared using a conventional melt quenching technique, and the crystallization behavior of ferroelastic β′-Gd2 MoO4)3 Crystals was examined to clarify the mechanism of self-powdering phenomenon and to design bulk crystallized glasses. It was found that the self-powdering phenomenon appeared significantly during the crystallization at temperatures near the crystallization peak temperature, but the phenomenon is suppressed in the crystallization at temperatures much higher than the glass transition temperature. It was also found that the substitution of TeO2 for B2O3 in the base glasses suppresses the self-powdering phenomenon and consequently bulk crystallized glasses were obtained in the glass with x=8 mol%. The densities at room temperature of the base glasses are d =4.755–4.906 g/cm3, being much higher than the value of d=4.555 g/cm3 for β′-Gd2(MoO4)3 crystal. It is proposed that the stresses in the inside of crystals induced by large density differences (i.e., large molar volume differences) between the glassy phase and crystals might be relaxed effectively in the glasses containing TeO2 with weak TeeO bonds and fragile character.
Condensed-phase mechanisms play a major role in fire-retardant polymers. Generations of development have followed the concept of charring to improve fire properties. Whereas the principal reactions are believed to be known, the specific description for multicomponent systems is lacking, as is the picture across different systems. A two-step approach is proposed in general, and also presented in greater detail. The second step covers the specific reactions controlling charring, whereas the actual reactants are provided in the preceding step. This model consistently incorporates the variety of structureproperty relationships reported. A comprehensive case study is presented on seven phosphorus flame retardants in two epoxy resins to breathe life into the two-step approach.
Hierarchically porous, high‐surface‐area silica materials are excellent candidates for multiple applications like catalysis and environmental remediation. Shaping these materials with additive manufacturing (AM) techniques, like robocasting, could enable their use with the benefit of on‐demand, customized shaping and maximizing performance. Herein, ordered mesoporous silica COK‐12 slurries were robocasted into monoliths, containing different ratios of uncalcined COK‐12 and sodium bentonite (0–25 wt.%). The rheology of the mixed slurries is characterized by lower flow indexes (0.69 vs. 0.32) and higher yield stresses (96 vs. 259 Pa) compared to pure COK‐12 ones. Monoliths were printed in woodpile structures and calcined at 600°C. Micro‐CT measurements showed a linear shrinkage of 25% after calcination. Mechanical characterization showed increased uniaxial strength (0.20 ± 0.07 to 1.0 ± 0.3 MPa) with increasing binder/solids ratio from 13 to 25%. The amorphous, mesoporous structure of COK‐12 was retained. The structures exhibited open porosities of 52 ± 4% and showed higher specific mesopore volumes, and increased average mesopore size (6 vs. 8 nm) compared to COK‐12. Small‐angle x‐ray scattering analysis revealed an increased lattice parameter (10.3 vs. 11.0 nm) and reduced wall thickness (3.1 nm vs. 4.1 nm) of the COK‐12 in the monoliths. These properties indicate suitability for their application as porous supports and adsorbents.
Mobility particle size spectrometers (MPSS) belong to the essential instruments in aerosol science that determine the particle number size distribution (PNSD)in the submicrometer size range. Following calibration procedures and target uncertainties against standards and reference instruments are suggested for a complete MPSS quality assurance program: a) calibration of the CPC counting efficiency curve (within 5% for the plateau counting efficiency; within 1 nm for the 50% detection efficiency diameter), b) sizing calibration of the MPSS, using a certified polystyrene latex (PSL) particle size standard at 203 nm (within 3%), c) intercomparison of the PNSD of the MPSS (within 10% and 20% of the dN/dlogDP concentration for the particle size range 20 – 200 nm and 200 to 800 nm, respectively), and d) intercomparison of the integral PNC of the MPSS (within 10%). Furthermore, following measurement uncertainties have been investigated: a) PSL particle size standards in the range from 100-500nm match within 1% after sizing calibration at 203 nm. b) Bipolar diffusion chargers based on the radioactive nuclides Kr85, Am241 and Ni63 and a new ionizer based on corona discharge follow the recommended bipolar charge distribution, while soft X-ray-based charges may alter faster than expected. c) The use of a positive high voltage supply show a 10% better performance than a negative one. d) The intercomparison of the integral PNC of an MPSS against the total number concentration is still within the target uncertainty at an ambient pressure of approximately 500 hPa.
Mechanically stable structures with interconnected hierarchical porosity combine the benefits of both small
and large pores, such as high surface area, pore volume, and good mass transport capabilities. Hence, lightweight micro-/meso-/macroporous monoliths are prepared from ordered mesoporous silica COK-12 by means of spark plasma sintering (SPS, S-sintering) and compared to conventionally (C-) sintered monoliths. A multi-scale model is developed to fit the small angle X-ray scattering data and obtain information on the hexagonal lattice parameters, pore sizes from the macro to the micro range, as well as the dimensions of the silica population. For both sintering techniques, the overall mesoporosity, hexagonal pore ordering, and amorphous character are preserved. The monoliths' porosity (77–49%), mesopore size (6.2–5.2 nm), pore volume (0.50–0.22 g cm-3
), and specific surface area (451–180 m2 g-1) decrease with increasing processing temperature and pressure. While the difference in porosity is enhanced, the
structural parameters between the C-and S-sintered monoliths are largely converging at 900 C, except for the mesopore size and lattice parameter, whose dimensions are more extensively preserved in the
S-sintered monoliths, however, coming along with larger deviations from the theoretical lattice. Their higher mechanical properties (biaxial strength up to 49 MPa, 724 MPa HV 9.807 N) at comparable porosities and ability to withstand ultrasonic treatment and dead-end filtration up to 7 bar allow S-sintered monoliths to reach a high permeance (2634 L m-2 h-1 bar-1), permeability (1.25 x 10^-14 m2), and ability to reduce the chemical oxygen demand by 90% during filtration of a surfactant-stabilized oil in water emulsion, while indicating reasonable resistance towards fouling.
In many industrial sectors, Structural Health Monitoring (SHM) is considered as an addition to Non-Destructive Testing (NDT) that can reduce maintenance effort during lifetime of a technical facility, structural component or vehicle. A large number of SHM methods is based on ultrasonic waves, whose properties change depending on structural health. However, the wide application of SHM systems is limited due to the lack of suitable methods to assess their reliability. The evaluation of the system performance usually refers to the determination of the Probability of Detection (POD) of a test procedure. Up to now, only few limited methods exist to evaluate the POD of SHM systems, which prevent them from being standardised and widely accepted in industry. The biggest hurdle concerning the POD calculation is the large amount of samples needed. A POD analysis requires data from numerous identical structures with integrated SHM systems. Each structure is then damaged at different locations and with various degrees of severity. All of this is connected to high costs. Therefore, one possible way to tackle this problem is to perform computer-aided investigations. In this work, the POD assessment procedure established in NDT according to the Berens model is adapted to guided wave-based SHM systems. The approach implemented here is based on solely computer-aided investigations. After efficient modelling of wave propagation phenomena across an automotive component made of a carbon fibre-reinforced composite, the POD curves are extracted. Finally, the novel concept of a POD map is introduced to look into the effect of damage position on system reliability.
Kunststoff- und Kunststoffrasenflächen kommt bei intensiv genutzten Flächen als Allwetterbeläge eine große Bedeutung zu. Sie leisten einen wichtigen Beitrag zur Absicherung eines ganzjähriger Sportangebote.
Gerade Kunststoffrasen ist aber in den letzten Jahren häufig in die Kritik geraten, insbesondere durch gefährliche Inhaltsstoffe und andere negative Einflüsse auf die Umwelt. Dies hat bei Bauherren zu einer Verunsicherung geführt und Fragen aufgeworfen, die erst teilweise beantwortet sind. Die Diskussionen rund um diesen Allwetterbelag haben bereits dazu geführt, dass von Seiten der Industrie viel verändert wurde und neue innovative Lösungen gefunden werden.
Der Fachbericht stellt eine Handreichung für Fachleute und interessierte Laien dar, um mehr Klarheit besonders hinsichtlich der Umweltanforderungen zu erzielen.
The water management in proton exchange membrane fuel cells (PEMFC) is strongly influenced by the design of the gas diffusion layers (GDL). Limiting current measurements in small-scale cells operating at high stoichiometries are useful to determine the oxygen transport resistance. The oxygen transport resistance increases, once water condenses inside the GDL. In this study a new electrochemical method for voltage loss estimation of GDL induced oxygen transport losses are presented. This new method, referred to as “transient limiting current” (TLC), is compared with the literature method. TLC allows a direct estimation of oxygen transport resistance at an arbitrarily conditioned state. This study also presents a case study of liquid water visualization of a PEM fuel cell with varying GDLs types.
With the help of quasi in-situ synchrotron X-ray computed tomography and time resolved radiography measurements we investigate appearance and distribution of liquid water inside the GDLs under limiting current conditions.
The present work shows results on elemental distribution analyses in Cu(In,Ga)Se2 thin films for solar cells performed by use of wavelength-dispersive and energy-dispersive X-ray spectrometry (EDX) in a scanning electron microscope, EDX in a transmission electron microscope, X-ray photoelectron, angle-dependent soft X-ray emission, secondary ion-mass (SIMS), time-of-flight SIMS, sputtered neutral mass, glow-discharge optical emission and glow-discharge mass, Auger electron, and Rutherford backscattering spectrometry, by use of scanning Auger electron microscopy, Raman depth profiling, and Raman mapping, as well as by use of elastic recoil detection analysis, grazing-incidence X-ray and electron backscatter diffraction, and grazing-incidence X-ray fluorescence analysis. The Cu(In,Ga)Se2 thin films used for the present comparison were produced during the same identical deposition run and exhibit thicknesses of about 2 µm. The analysis techniques were compared with respect to their spatial and depth resolutions, measuring speeds, availabilities, and detection limits.
Accurate and reproducible measurement of the structure and properties of high-value nanoparticles is extremely important for their commercialization. A significant proportion of engineered nanoparticle systems consist of some form of nominally core-shell structure, whether by design or unintentionally. Often, these do not form an ideal core-shell structure, with typical deviations including polydispersity of the core or shell, uneven or incomplete shells, noncentral cores, and others. Such systems may be created with or without intent, and in either case an understanding of the conditions for formation of such particles is desirable. Precise determination of the structure, composition, size, and shell thickness of such particles can prove challenging without the use of a suitable range of characterization techniques. Here, the authors present two such polymer core-shell nanoparticle systems, consisting of polytetrafluoroethylene cores coated with a range of thicknesses of either polymethylmethacrylate or polystyrene. By consideration of surface energy, it is shown that these particles are expected to possess distinctly differing coating structures, with the polystyrene coating being incomplete. A comprehensive characterization of these systems is demonstrated, using a selection of complementary techniques including scanning electron microscopy, scanning transmission electron microscopy, thermogravimetric analysis, dynamic light scattering, differential centrifugal sedimentation, and X-ray photoelectron spectroscopy. By combining the results provided by these techniques, it is possible to achieve superior characterization and understanding of the particle structure than could be obtained by considering results separately.
The incorporation of colloidal quantum dots (QDs) into solid matrices, especially ionic salts, holds several advantages for industrial applications. Here, we demonstrated via absolute measurements of photoluminescence quantum yields (PL-QY) that the photoluminescence of aqueous CdTe QDs can be considerably increased upon incorporation into a salt matrix with a simple crystallization procedure. Enhancement factors of up to 2.8 and a PL-QY of 50 to 80%, both in NaCl crystals and incorporated in silicone matrices, were reached. The fact that the achievable PL enhancement factors depend strongly on PL-QY of the parent QDs can be described by the change of the dielectric surrounding and the passivation of the QD surface, modifying radiative and nonradiative rate constants. Time-resolved PL measurements revealed noncorrelating PL lifetimes and PL-QY, suggesting that weakly emissive QDs of the ensemble are more affected by the enhancement mechanism, thereby influencing PL-QY and PL lifetime in a different manner.
Um eine gute Luftqualität in Gebäuden zu erreichen, müssen Reinigungslasten durch Lüften aus Räumen abgeführt bzw. vermieden oder verringert werden. Wird der Luftwechsel verringert, verschlechtert sich die Raumluftqualität, und die Zufriedenheit der Nutzer nimmt ab. An Arbeitsplätzen kann es bei schlechter Luftqualität und der daraus resultierenden Unzufriedenheit zu einer geringeren Produktivität der Beschäftigten kommen. Um die Reinigungslasten und deren Wirkung auf den Raumnutzer überdas Geruchsempfinden zu verringern, ist neben einer messtechnischen Erfassung der Verunreinigungen auch eine sensorische Prüfung in Innenräumen und von Bauprodukten notwendig. In diesem Artikel wird die Entwicklung der Bewertungsmethodik von Gerüchen im Innenraum erläutert und auf Anwendungen eingegangen.
Aim: To observe the variation in accumulation of Fusarium and Alternaria mycotoxins across a topographically heterogeneous field and tested biotic (fungal and bacterial abundance) and abiotic (microclimate) parameters as explanatory variables.
Methods and Results: We selected a wheat field characterized by a diversified topography, to be responsible for variations in productivity and in canopy-driven microclimate. Fusarium and Alternaria mycotoxins where quantified in wheat ears at three sampling dates between flowering and harvest at 40 points.
Tenuazonic acid (TeA), alternariol (AOH), alternariol monomethyl ether (AME), tentoxin (TEN), deoxynivalenol (DON), zearalenone (ZEN) and deoxynivalenol-3-Glucoside (DON.3G) were quantified. In canopy temperature, air and soil humidity were recorded for each point with data-loggers. Fusarium spp. as trichothecene producers, Alternaria spp. and fungal abundances were assessed using qPCR. Pseudomonas fluorescens bacteria were quantified with a culture based method. We only found DON, DON.3G, TeA and TEN to be ubiquitous across the whole field, while AME, AOH and ZEN were only occasionally detected. Fusarium was more abundant in spots with high soil humidity, while Alternaria in warmer and drier spots. Mycotoxins correlated differently to the observed explanatory variables: positive correlations between DON accumulation, tri 5 gene and Fusarium abundance were clearly detected.
The correlations among the others observed variables, such as microclimatic conditions, varied among the sampling dates. The results of statistical model identification do not exclude that species coexistence could influence mycotoxin production.
Conclusions: Fusarium and Alternaria mycotoxins accumulation varies heavily across the field and the sampling dates, providing the realism of landscapescale studies. Mycotoxin concentrations appear to be partially explained by biotic and abiotic variables.
Significance and Impact of the Study: We provide a useful experimental design and useful data for understanding the dynamics of mycotoxin biosynthesis in wheat.
27Al nuclear magnetic resonance spectra of polycrystalline aluminium borate 9Al2O3 · 2B2O3 have been measured in double rotation at 11.7 and 7.0 T and high-speed magic-angle spinning at 7.0, 9.4, 11.7, 14.1 and 17.6 T. Spinning sidebands from the satellite transitions were observed at 7.0 and 14.1 T. Each of the four structural aluminium sites [Al(IV), Al(V)(1), Al(V)(2) and Al(VI)] are observed, characterised and assigned in the spectra. The obtained parameter set gives a fully consistent interpretation in agreement with the crystal structure of the compound.
We propose a model to describe the sintering kinetics of polydispersed glass particles, having no adjustable parameter. The model is based on three sintering stages: a pure Frenkel' (F) first step, a mixed Frenkel/MackenzieShuttleworth' stage, and a third, pure MackenzieShuttleworth' (MS) step. The model considers sample shrinkage as the sum of the partial shrinkage of several clusters, each consisting of equally sized particles and each showing independent F or MS behavior. The overall set of clusters mimics the specimen's real particle size distribution. We then introduce the concept of neck forming ability, which allows the formation of necks among particles of different sizes, relaxing the clustering condition. Using experimental physical parameters: particle size distribution, viscosity, surface energy, and the theoretical neck forming ability, the model describes well the sintering kinetics of an alumino-borosilicate glass powder having polydispersed, irregular shaped particles in a variety of temperatures. The sintering kinetics of the real powder is slower, but not far from the calculated kinetics of a monodispersed distribution containing only particles of average size. Thus the model provides a tool for estimating the sintering kinetics of real glass powders, for any size distribution and temperature, thus minimizing the number of laboratory experiments.