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Paper des Monats
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Herein, two polyurethane oligomers were successfully synthesized using a prepolymer mixing process. The prepolymers were synthesized based on the step-growth addition polymerization of polypropylene glycol, Methylene diphenyl diisocyanate and 2-hydroxyethyl methacrylate or 2-hydroxyethyl acrylate. Isopropanol was functioned as the isocyanate blocking agent. Thereafter, different terpolymer emulsions were prepared by the emulsion graft copolymerization with the vinyl acetate monomer in presence of 2-ethylhexyl acrylate as a vinyl monomer. The chemical structures of the synthesized oligomeric monomers were probed by FTIR spectroscopy and found to vary with the content of acrylic monomer used in the oligomer synthesis phase (i.e.hydroxyethyl acrylate or hydroxyethyl methacrylate). The topography, thermal stability, and particle size of terpolymers were investigated by SEM, TGA, and zeta potential, respectively. The TGA results demonstrated marked enhancement in thermal stability of the synthesized terpolymers up to ca. 600°C, which was concurrent with enhanced surface homogeneity and film properties as evidenced by the SEM images. These terpolymers showed also property enhancement as binders for textile pigment printing in terms of rubbing resistance, color strength and fastness to washing when compared to the commercial binders.
These judgments would provide a new competent synthesis route by introducing polyurethane acetate vinyl acrylate as the binder for use in pigment printing of cotton fabrics.
Over the years, industrial and human activities and agricultural practices have caused a serious threat to human health and the environment. Indeed, it has been demonstrated that these activities are responsible for the presence of pollutants in the soil, air and water.
Water is one of the most strategic issues today, as it is associated with the living world. Therefore, water pollution is becoming a universal scourge that leads to environmental degradation, decrease of water quality and threatens public health.
Water pollution is mainly due to the discharge of certain harmful chemical compounds that are not very or not at all biodegradable (phenolic compounds, heavy metals, hydrocarbons, dyes, pesticides, etc.) by various industries: chemical, pharmaceutical, textile, food processing, etc. The impact of these industrial effluents on fauna and flora is very harmful. A sensitization of the socio-economic actors and the public, accompanied by a severe regulation in relation to the discharges, would contribute to fight against this drift, but also, by the development of effective methods allowing to remove these pollutants, not only in an analytical purpose but also of depollution.
Thus and within the framework of the preservation of an environment with regard to any anthropogenic activity, our research topic relates to the use of original biosourced polymeric phases for the extraction of the organic compounds and the heavy metals in aqueous mediums.
Therefore, we have proceeded to the synthesis and characterization of a large variety of monomers, polymers and cross-linked materials. These products, partially derived from biomass, contain various functional groups with the ability to interact with chemical components without discriminating effect.
The developed polymer phases have been successfully used for the adsorption of some organic pollutants and heavy metals in synthetic aqueous solutions.
Iron aluminides depict a sustainable and light-weight material class which could be employed in many applications requiring high strength at intermediate to high temperatures. According to first results, the alloy Fe-26Al-4Mo-0.5Ti-1B surpasses conventional materials in wet corrosion resistance and creep resistance up to 650 °C. For these reasons, the AiF research project “WAFEAL – Materials applications for iron aluminides” was initiated to transfer these findings into a standardised materials dataset and to derive best practices for processing. In the first place, a set of different microstructures adjusted by varying casting methods, wall thicknesses and heat treatments was investigated and correlated with hardness on macro and micro scale. Correlations were drawn between solidification rates and resulting grain sizes and hardness. The effect of vacancy hardening was only verified for wall thickness as low as 2.5 mm. Moreover, a common decrease of macrohardness after a heat treatment at 1000 °C for 100 h was observed irrespective of casting process or wall thickness. This effect was linked with an unexpected decrease of the complex boride phase fraction which acts as a hardening phase.
Due to the increasing scarcity of critical raw materials current high-temperature materials are sought to be replaced by alloys based on more abundant metals. One possibility within the class of intermetallics are iron aluminides, which combine sustainability and cost-efficiency with the prospect of mass savings. Iron aluminides show competitive specific strength up to 700 °C and excellent creep and wet corrosion resistance by small additions of Mo, Ti and B. Nevertheless, a Mo content of above 2 at.% which is needed for optimum corrosion resistance results in enhanced brittleness, especially at room temperature. This is why alloys with these Mo fractions were only mechanically tested under compressive loading so far. Still, testing of static and creep properties under tensile loading is required for reliable component design. Besides high standards for crack-free processing, data acquisition for tensile loads is especially complicated by environmental embrittling effects for iron aluminides. To cope with these challenges, the AiF research project “WAFEAL – Materials applications for iron aluminides” was initiated. The main goal is to collect standardised data on ambient and high-temperature tensile properties and creep properties. Samples with a nominal composition of Fe-26Al-4Mo-0.5Ti-1B [at.%] were manufactured via centrifugal casting in ceramic shell moulds followed by machining. Heat treatment for homogenisation and final polishing were carried out where appropriate. A summary of the achieved tensile and creep properties such as yield and tensile strength, maximum elongation, secondary creep rate and stress exponents will be given. Results will be also discussed regarding the influence of temperature, stress level and microstructure on the damage mechanisms. Furthermore, the effect of different alloy concentrations on the mechanical response at different temperatures will be outlined within a small experimental series.
With an increasing demand in more efficient fuel consumption to reduce CO2 emissions, weight reductions in high-temperature materials at affordable costs gain increasing attention. One potential candidate is the intermetallic material class of iron aluminides, combining the advantages in mass savings, high temperature performance and recyclability of resources. The alloy Fe-26Al-4Mo-0.5Ti-1B was selected to study the microstructural features evolving from two casting processes, five wall thicknesses and three final conditions. Conclusions are drawn upon the correlations of processing variables, grain sizes and hardness.
Iron aluminides, already reported in the late 19th century, did not cease to attract the interest of scientists and engineers ever since. Besides good oxidation resistance, low density and resource availability, potentials for hightemperature strengths that compete with high-alloy steels were unlocked by low alloy contents. Still, research on alloy design continues, as alloying usually comes at the price of brittleness in low-temperature regimes. A potential candidate is the quinary Fe–Al–Mo–Ti–B system which is strengthened by solid solution and eutectic borides. It was shown to have good strength and outstanding creep resistance under compressive loading up to elevated temperatures. Although the individual effect of alloy additions is well understood in iron aluminides, little is known about the combined effects of alloying concentrations on microstructure, phase stability and mechanical properties. Therefore a systematic study of two Ti-doped near-Fe3Al alloys with varying contents of Mo (2–4 at.%) and B (0.5–1 at.%) was conducted. In total eight different alloys were fabricated by investment casting into ceramic shell molds. Alloys were characterized and compared by grain size, phase transitions, microstructure evolution as well as elemental compositions and volume fractions of phases. For mechanical characterization, macrohardness and microhardness tests as well as tensile tests at ambient and high tempera tures were conducted. Independent of alloy additions, alloys with 24–25 at.% Al exhibit superior proof strength due to a higher matrix hardness. Decreasing B content generally decreases strength by lower secondary phase fractions which contribute via particle hardening. Reducing Mo content decreases both the solute concentration in the matrix and secondary phase fractions. Surprisingly, strength is similar or even superior to alloys with higher Mo content. Strength relations are discussed with a focus on solid-solution hardening theory and other competing strengthening mechanisms.
The increasing importance of resource availability and closed-loop material cycles are driving materials research to reduce alloying content in conventional materials or even substitute them with more sustainable alternatives. Intermetallic iron aluminide alloys (FeAl) present a potential alternative. Many alloy concepts for improved high-temperature properties or ductility have already been successfully implemented in casting technologies on a laboratory scale. However, successful testing of FeAl alloys on an industrial scale was still pending at the beginning of the project.
Therefore, the aim of the project was to develop simulation-based casting concepts for industrial casting processes using the base alloy Fe-26Al-4Mo-0.5Ti-1B and to narrow down process limits by means of hot cracking tests. Findings were transferred into practice-oriented guidelines for casting of iron aluminides, which is accessible to future applicants in SMEs. The focus was placed on centrifugal casting combined with investment casting or die casting. In addition to numerous design and casting process parameters, heat treatments and alloying additions (Al, Mo, B) were varied to determine the influence of alloying elements on castability, microstructure and mechanical properties. Data from microstructure analyses (microscopic imaging, determination of grain sizes as well as phase compositions and volume fractions, fractography), mechanical tests (hardness measurements, compression tests, ambient and high-temperature tensile tests, creep tests) as well as measurements of thermophysical properties could be generated on the base alloy. Correlations of materials data with process variables allowed conclusions to be drawn on strengthening mechanisms and ductility of the alloy and how they can be controlled in terms of processing and component design. Successful casting of highly complex components with thin wall thicknesses and optimised alloy compositions points out prospects for new fields of application.
The increasing importance of resource availability and closed-loop material cycles are driving materials research to reduce alloying content in conventional materials or even substitute them with more sustainable alternatives. Intermetallic iron aluminide alloys (FeAl) present a potential alternative. Many alloy concepts for improved high-temperature properties or ductility have already been successfully implemented in casting technologies on a laboratory scale. However, successful testing of FeAl alloys on an industrial scale was still pending at the beginning of the project.
Therefore, the aim of the project was to develop simulation based casting concepts for industrial casting processes using the base alloy Fe-26Al-4Mo-0.5Ti-1B and to narrow down process limits by means of hot cracking tests. Findings were transferred into practice-oriented guidelines for casting of iron aluminides, which is accessible to future applicants in SMEs. The focus was placed on centrifugal casting combined with investment casting or die casting. In addition to numerous design and casting process parameters, heat treatments and alloying additions (Al, Mo, B) were varied to determine the influence of alloying elements on castability, microstructure and mechanical properties. Data from microstructure analyses (microscopic imaging, determination of grain sizes as well as phase compositions and volume fractions, fractography), mechanical tests (hardness measurements, compression tests, ambient and high-temperature tensile tests, creep tests) as well as measurements of thermophysical properties could be generated on the base alloy. Correlations of materials data with process variables allowed conclusions to be drawn on strengthening mechanisms and ductility of the alloy and how they can be controlled in terms of processing and component design. Successful casting of highly complex components with thin wall thicknesses and optimised alloy compositions points out prospects for new fields of application.
The tetragonal crystal- structure type of chalcopyrites (chemical formula AIBIIICVI2) is a superstructure of sphalerite type. The c/a ratio differs generally from the ideal value 2, i.e., the crystal structure is pseudocubically distorted. For CuInSe2 and CuGaSe2 thin films, simulations demonstrate that it is theoretically possible to reveal the tetragonality in electron backscatter-diffraction (EBSD) patterns for CuGaSe2, whereas it may not be possible for CuInSe2. EBSD experiments on CuGaSe2 thin films using the ”Advanced Fit” band-detection method show that it is possible to extract accurate misorientation-angle distributions from the CuGaSe2 thin film. Pole figures revealing the texture of the CuGaSe2 thin film are shown, which agree well with X-ray texture measurements from the same layer.
Monodisperse iron oxide nanoparticles as reference material candidate for particle size measurements
(2020)
In order to utilize and rationally design materials at the nanoscale the reliable characterization of their physico-chemical properties is highly important, especially with respect to the assessment of their environmental or biological impact. Furthermore, the European Commission’s REACH Regulations require the registration of nanomaterials traded in quantities of at least 1 ton. Powders or dispersions where 50% (number distribution) of the constituent particles have sizes ≤ 100 nm in at least one dimension are defined as nanomaterials. This creates a need for industrial manufacturers and research or analytical service facilities to reliably characterize potential nanomaterials. Currently, BAM is developing reference nanoparticles, which shall expand the scarce list of worldwide available nano reference materials certified for particle size distribution and will also target other key parameters like shape, structure, porosity or functional properties. In this respect, materials like iron oxide or titanium dioxide are considered as candidates to complement the already available silica, Au, Ag, and polystyrene reference nanoparticles.
The thermal decomposition of iron oleate precursors in high boiling organic solvents can provide large quantities of iron oxide nanoparticles that can be varied in size and shape.[1, 2] The presence of oleic acid or other hydrophobic ligands as capping agents ensures stable dispersion in nonpolar solvents. Such monodisperse, spherical particles were synthesized at BAM and pre-characterized by electron microscopy (TEM, SEM including the transmission mode STEM-in-SEM) and dynamic light scattering comparing cumulants analysis and frequency power spectrum.
1. REACH regulations and nanosafety concerns create a strong need for nano reference materials with diverse properties.
2. Iron oxide nanoparticles are under development as new candidate reference material at BAM.
3. Narrow particle size distribution confirmed by light scattering and electron microscopy.
Tracking waterborne microplastic (MP) in urban areas is a challenging task because of the various sources and transport pathways involved. Since MP occurs in low concentrations in most wastewater and stormwater streams, large sample volumes need to be captured, prepared, and carefully analyzed. The recent research in urban areas focused mainly on MP emissions at wastewater treatment plants (WWTPs), as obvious entry points into receiving waters. However, important transport pathways under wet-weather conditions are yet not been investigated thoroughly. In addition, the lack of comprehensive and comparable sampling strategies complicated the attempts for a deeper understanding of occurrence and sources. The goal of this paper is to (i) introduce and describe sampling strategies for MP at different locations in a municipal catchment area under dry and wet-weather conditions, (ii) quantify MP emissions from the entire catchment and two other smaller ones within the bigger catchment, and (iii) compare the emissions under dry and wet-weather conditions. WWTP has a high removal rate of MP (>96%), with an estimated emission rate of 189 kg/a or 0.94 g/[population equivalents (PEQ · a)], and polyethylene (PE) as the most abundant MP. The specific dry-weather emissions at a subcatchment were ≈30 g/(PEQ · a) higher than in the influent of WWTP with 23 g/(PEQ · a). Specific wet-weather emissions from large sub-catchment with higher traffic and population densities were 1952 g/(ha · a) higher than the emissions from smaller catchment (796 g/[ha · a]) with less population and traffic. The results suggest that wet-weather transport pathways are likely responsible for 2–4 times more MP emissions into receiving waters compared to dry-weather ones due to tire abrasion entered from streets through gullies. However, more investigations of wet-weather MP need to be carried out considering additional catchment attributes and storm event characteristics.
Im Vorhaben wurde eine forcierte Prüfmethode zur Bestimmung der Beständigkeit von metallenen Werkstoffen gegenüber Brennstoffen aus Mitteldestillaten und Gemischen aus Mitteldestillat und paraffinischen Kohlenwasserstoffen, die jeweils Fettsäuremethylester (FAME) als biogene Komponente enthalten, entwickelt. Bei der Prüfmethode werden Prüfkörper des jeweiligen Werkstoffes in speziellen Prüfmedien ausgelagert. Die Zusammensetzung von zwei Prüfmedien wurde im Vorhaben erarbeitet. Diese Prüfmedien erfassen die Effekte der Alterung des FAME, die zu erwarten sind, wenn der Brennstoff länger als 2 Jahre im Feld lagert. Sie decken den Bereich bis 20 % (V/V) FAME-Anteil ab. Die Auslagerung kann bei geringem Aufwand unter Atmosphärendruck durchgeführt werden.
Die Eignung einer Auswahl von metallenen Werkstoffen und Polymerwerkstoffen, die für Versorgungsanlagen für Mitteldestillat relevant sind, wurde durch Auslagerung in folgenden nicht gealterten Brennstoffen bestimmt: Heizöl EL schwefelarm (B0), Heizöl EL schwefelarm mit 20 % (V/V) FAME (B20), FAME (B100) und hydriertes Pflanzenöl (HVO). Die Werkstoffe wurden auch in einem 1 Jahr gealterten B20 und einem 8 Jahre gealtertem B10 ausgelagert. Die Temperatur bei der Auslagerung betrug 50 °C für die metallenen Werkstoffe und 40 °C und 70 °C für die Polymerwerkstoffe. Die Ergebnisse der Beständigkeitsbewertung wurden in Beständigkeitslisten zusammengefasst. Die mit B20 erhaltenen Bewertungen gelten generell für Gemische aus Heizöl EL schwefelarm und FAME mit einem FAME-Gehalt bis 20 % (V/V). Sie sind auch auf Gemische aus Dieselkraftstoff und FAME mit einem FAME-Gehalt bis 20 %(V/V) übertragbar.
Die forcierte Prüfmethode kann insbesondere KMUs bei der Weiterentwicklung von bestehenden Produkten und der Entwicklung von neuen Produkten als ein kostengünstiger Schnelltest zur Überprüfung der Werkstoff- und Bauteilbeständigkeit gegenüber Mitteldestillaten mit hohem FAME-Anteil dienen. Sie kann für die Hersteller die Sicherheit erhöhen, dass Bauteile die Freigabeprüfungen der Bauaufsicht bestehen, wobei die Freigabe jedoch nur für Deutschland gültig ist.
Die Erkenntnisse des Forschungsvorhabens können in eine harmonisierte Europäische Norm für alternative Brenn- und Kraftstoffe einfließen. Diese ist für die Bauteilhersteller die Voraussetzung für die Erschließung des europäischen Marktes.
In dem Projekt soll die vollständige Wiederverwertbarkeit der Schlacke und ihrer Bestandteile demonstriert werden. Dazu gehören die vollständige Rückgewinnung der metallischen Phase, die in die Edelstahlherstellung zurückgeführt werden kann, sowie die Aufwertung der mineralischen Fraktion, die ihre uneingeschränkte Verwendung als Zementzumahlstoff oder mineralischer Baustoff erlaubt. Bei geeigneter Prozessführung des elektrischen Lichtbogenofens können durch „reduzierendes Schmelzen“ die chromhaltigen Wertstoffe zusammen mit anderen Schwermetallen zu 97% in einer Metalllegierung angereichert und separiert werden. Diese kann als Rohstoff in der Metallurgie eingesetzt werden. Der Chromgehalt der mineralischen Komponte der Schlacke konnte von ca. 3% auf unter 0,1% verringert werden. Die mineralische Fraktion lässt sich durch entsprechende Zuschläge während des Schmelzbetriebes und eine anschließende Granulation der schmelzflüssigen Phase zu einem Material aufwerten, das in seiner Zusammensetzung und seinen Eigenschaften typischen Zementkomponenten entspricht und als Rohstoff in der Zementproduktion eingesetzt werden kann. Dafür müssen allerdings noch die rechtlichen Voraussetzungen geschaffen werden, da der Rohstoffeinsatz gerade im Zement strengen Auflagen unterliegt und die Zemente bestimmte Normen erfüllen müssen.
Durch die in RECARC aufgezeigte Möglichkeit der Wiederverwertung können somit Stoffkreisläufe geschlossen werden, die ansonsten zu einem Verlust wertvoller Rohstoffe führen. Vor allem die steigenden Rohstoffkosten, aber auch die immer stärker limitierten CO2-Emissionen zeigen die hohe Relevanz im Umgang mit metallurgischen Reststoffen. Eine Überführung des in RECARC demonstrierten Verfahrens in die Industrie könnte einen wichtigen Beitrag zur nachhaltigen Schonung der natürlichen Ressourcen und der Umwelt leisten.
A technical-safety evaluation of the detonation effects of pyrotechnic compositions can be performed on the basis of TNT/PETN equivalence. The equivalence determination can be carried out by characterization of the blast wave generated because of detonation in free field tests, which however can be highly resource intensive and prone to uncertainties. Here, we present underwater ‘small-scale’ experiments for the determination of such equivalents.
Underwater experiments, as described in the European standard EN 13763-15:2004, are performed to test the capability of detonators to initiate secondary explosives by determining the released energy. At BAM this test was modified to compare the energy output of the pyrotechnic mixtures (those used in air bag gas generators and firework flash compositions) and thus to determine their equivalents of high explosives like TNT or PETN. In the modified tests, small cylindrical copper containers were filled with pyrotechnic substances, which were then attached to standard detonators. This explosive charge assembly was then lowered into a water tank of about 1000 l capacity. At the same depth as the charge assembly, a piezoelectric pressure sensor was immersed in the water at a horizontal distance of about 400 mm from the charge. By recording the time-dependent pressure during the test, the shock energy as well as the energy associated with the expanding gas bubble were determined.
Solar glass in arid and semi-arid regions is exposed to sand storms which can affect the durability of PV modules. Related erosion processes have been extensively studied but the results given are difficult to compare due to being obtained by different variables like particle speed and sand mass. This study correlates the damage of solar panels to the cumulative impact energy as a global parameter.
The manufacture of sintered glasses and glass-ceramics, glass matrix composites, and glass-bounded ceramics or pastes is often affected by gas bubble formation. Against this background, we studied sintering and foaming of barium silicate glass powders used as SOFC sealants using different powder milling procedures. Sintering was measured by means of heating microscopy backed up by XPD, differential thermal analysis, vacuum hot extraction (VHE), and optical and electron microscopy. Foaming increased significantly as milling progressed. For moderately milled glass powders, subsequent storage in air could also promote foaming. Although the powder compacts were uniaxially pressed and sintered in air, the milling atmosphere significantly affected foaming. The strength of this effect increased in the order Ar ≈ N2 < air < CO2. Conformingly, VHE studies revealed that the pores of foamed samples predominantly encapsulated CO2, even for powders milled in Ar and N2. Results of this study thus indicate that foaming is caused by carbonaceous species trapped on the glass powder surface. Foaming could be substantially reduced by milling in water and 10 wt% HCl.
Surface roughness, RZ, normal transmittance, ΤN, total transmittance, ΤT, and photovoltaic (PV) module efficiency, ηS, were measured for commercial solar glass plates and PV test modules identically sandblasted with different loads of quartz sand (200–400 μm), impact inclination angles, and sand particle speed. Measured data are presented versus the specific energy uptake during sand blasting, E (J/m2). Cracks, adhering particles, and scratch-like textures probably caused by plastic flow phenomena could be observed after sand blasting. Their characteristic size was much smaller than that of sand particles. After blasting and subsequent cleaning, the glass surface was still covered with adhering glass particles. These particles, cracks, and scratch-like textures could not be removed by cleaning. For sand blasting with α = 30° inclination angle and E = 30 000 J/m2, normal transmittance, total transmittance, and relative module efficiency decreased by 29%, 2% and ∽2%, respectively. This finding indicates that diffusive transmission of light substantially contributes to PV module efficiency and that the module efficiency decrease caused by sand erosion can be better estimated from total than by normal transmittance measurements.