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The certified reference material BAM-L200, a nanoscale stripe pattern for length calibration and specification of lateral resolution, is described. BAM-L200 is prepared from a cross-sectioned epitaxially grown layer stack of AlxGa1–xAs and InxGa1–xAs on a GaAs substrate. The surface of BAM-L200 provides a flat pattern with stripe widths ranging down to 1 nm. Calibration distances, grating periods and stripe widths have been certified by TEM with traceability to the length unit. The combination of gratings, isolated narrow stripes and sharp edges of wide stripes offers plenty of options for the determination of lateral resolution, sharpness and calibration of length scale at selected settings of imaging surface-analytical instruments. The feasibility of the reference material for an analysis of the lateral resolution is demonstrated in detail by evaluation of ToF-SIMS, AES and EDX images. Other applications developed in the community are summarized, too. BAM-L200 fully supports the implementation of the revised International Standard ISO 18516 (in preparation) which is based on knowledge outlined in the Technical Report ISO/TR 19319:2013.
The fundamental properties of a polymeric material are ultimately governed by its structure, which mainly relies on monomercomposition and connection, topology, chain length, and polydispersity. Thus far, these structural characteristics are typicallyset ex situ by the specific polymerization procedure, eventually limiting the future design space for the creation of moresophisticated polymers. Herein, we report on a single photoswitchable catalyst system, which enables in situ remote controlover the ring-opening polymerization of l-lactide and further allows regulation of the incorporation of trimethylene carbonateand δ -valerolactone monomers in copolymerizations. By implementing a phenol moiety into a diarylethene-type structure,we exploit light-induced keto–enol tautomerism to switch the hydrogen-bonding-mediated monomer activation reversiblyON and OFF. This general and versatile principle allows for exquisite external modulation of ground-state catalysis of a livingpolymerization process in a closed system by ultraviolet and visible light and should thereby facilitate the generation of newpolymer structures.
Chemically modified bioactive glasses based on ICIE16 were prepared with the melt-quenching method using water as a quenching medium. The sinterability of these bioactive glasses was investigated and is discussed in this article. The sintering experiments were conducted with different sintering temperatures, sintering times and heating rates. Those parameters are crucial for dense glass with an amorphous structure. The particle size (d50) of the starting glass powder was determined at 88 μm and kept constant. The pre-pressed glass pellets were cold-isostatically pressed at 300 MPa to a green density of around 63 %. Density development, phase identification, shrinkage behavior and the microstructure were investigated to determine the sinterability of the developed glasses. The glass powders were sintered at different temperatures inside the processing window while crystallization was monitored. The results have shown that the sinterability of the developed glasses strongly dependsonthe proposed chemical additions. The highest density reached was 96 %, which belongs to BP1 glass with sintering conditions of 20 K/min heating rate for 60 min at 750 °C.
Chemical-free pest control by dielectric
heating with radio waves and microwaves:
Thermal effects
(2018)
Thermal pest control with hot air is widely accepted as an alternative to chemical methods. However, it requires relatively long treatment times owing to the low thermal conductivity of wood. Direct dielectric heating that applies radio waves or microwaves has the advantage of more homogeneous heating. However, Sound experimental data on this technique are currently rare. Therefore, the thermal treatment of wood-destroying insects with radio waves and microwaves was studied with two model pests, Anobium punctatum and Hylotrupes bajulus, and with Tenebrio molitor as a reference. The secure elimination of pests was achieved, and the corresponding treatment time was in the range of a few minutes. Temperature profiles were more homogeneous when applying radio waves.
The self-ignition of coal dust deposits and its subsequent smoldering combustion pose a high fire hazard to oxy-fuel power systems which burn fuels using pure oxygen for the sake of carbon capture and storage. The increasing risk of explosion in the gas-phase and self-ignition in the solid-phase for an oxygen enhanced combustion environment has not been well studied yet. In this work, the heterogeneous reactions of a bituminous coal dust are investigated by using a novel hot-basket apparatus with an emphasis on the roles of O2 and diluent gas in chemisorption and smoldering. Experiments show that increasing O2 mole fraction accelerates both self-ignition and the following smoldering combustion. On the other hand, the presence of CO2 increases the ignition temperature and reduces the maximum smoldering temperature. However, the promotion in the fire and explosion risk by elevating O2 mole fraction is substantially stronger than the retardation effected by presence of CO2. The emission-gas measurements show that the CO to CO2 ratio increases significantly after self-ignition, and CH4 counts for 1–8% of the total carbon emission. This research may help improve the understanding of heterogeneous coal combustion and the fire safety in oxy-fuel power systems.
Advanced peptide-based nanomaterials composed of self-assembling peptides (SAPs) are of emerging interest in pharmaceutical and biomedical applications. The introduction of fluorine into peptides, in fact, offers unique opportunities to tune their biophysical properties and intermolecular interactions. In particular, the degree of fluorination plays a crucial role in peptide engineering as it can be used to control the characteristics of fluorine-specific interactions and, thus, peptide conformation and self-assembly. Here, we designed and explored a series of amphipathic peptides by incorporating the fluorinated amino acids (2S)-4-monofluoroethylglycine (MfeGly), (2S)-4,4-difluoroethylglycine (DfeGly) and (2S)-4,4,4-trifluoroethylglycine (TfeGly) as hydrophobic components. This approach enabled studying the impact of fluorination on secondary structure formation and peptide self-assembly on a systematic basis. We show that the interplay between polarity and hydrophobicity, both induced differentially by varying degrees of side chain fluorination, does affect peptide folding significantly. A greater degree of fluorination promotes peptide fibrillation and subsequent formation of physical hydrogels in physiological conditions. Molecular simulations revealed the key role played by electrostatically driven intra-chain and inter-chain contact pairs that are modulated by side chain fluorination and give insights into the different self-organization behaviour of selected peptides. Our study provides a systematic report about the distinct features of fluorinated oligomeric peptides with potential applications as peptide-based biomaterials.
"Ullmann's Encyclopedia of Industrial Chemistry" is the benchmark reference in chemistry and chemical and life science engineering, covering inorganic and organic chemicals, advanced materials, pharmaceuticals, polymers and plastics, metals and alloys, biotechnology and biotechnological products, food chemistry, process engineering and unit operations, analytical methods, environmental protection, and much more.
The present article is part of the topic collection "Environmental Protection and Industrial Safety". It covers plant and process safety, focusing on hazardous materials and process conditions.
Material extrusion of thermoplastic polymers enables the realization of complex specific designs with high performance composites. The present study aims at evaluating the mechanical properties of carbon fiberreinforced semi-crystalline thermoplastic polymer polyether ether ketone (CFR-PEEK) manufactured by material extrusion and correlating them with results obtained by micro-CT. Samples in the shape of small bars were provided by Kumovis (Munich, Germany). The determination of surface roughness and density was followed by three-point bending tests. To reveal the pore distribution as well as the fusion quality of CFR PEEK when applied with external forces, micro-CT scans were performed with an X-ray microscope before and after the mechanical test to localize the sites where the fracture is generated. The density of CFR-PEEK bars indicated that they had superior mechanical properties compared with our previous study on unfilled 3D printed PEEK (bending modulus: (5.4 ± 0.5) GPa vs. (1.05 ± 0.05) GPa to (1.48 ± 0.10) GPa; bending strength: (167 ± 11) MPa vs. (51 ± 15) to (193 ± 7) MPa). Micro-CT analyses revealed the local 3D-distribution of voids. Voids of 30 μm diameter are nearly spherical and make up the main part of the total porosity. The larger the voids, the more they deviate from a spherical shape. Significant lack-of-fusion voids are located between the deposited filaments. By growing and merging, they act as seeds for the forming fracture line in the region of the flexural specimens where the maximum local tensile stresses occurred under bending load. Our work provides a detailed analysis of printed PEEK with fiber additive and relates this with mechanical properties.
Polymers that help tailoring rheological properties during the casting process have become inevitable constituents for all kinds of high-performance concrete technologies. Due to lacking industries, these typically crude-oil based admixtures are not readily available in many parts of the world, which limits the implementation of more sustainable high-performance construction technologies in these regions. Alternative polymers, which often demand for less processing, can be derived from local plant-based resources. The paper provides experimental data of flow tests of cement pastes with polysaccharides from Triumfetta pendrata A. Rich, acacia gum and cassava without and in the presence of polycarboxylate ether superplasticizer. The flow tests are amended by observations of the zeta potentials and the hydrodynamic diameters in the presence of and without calcium ions in the dispersion medium. The results show that in the presence of and without calcium ions all polysaccharides provide negative zeta potentials, yet, they affect flowability and thixotropy in different ways. Cassava starch, acacia gum, and the gum of Triumfetta pendrata A. Rich qualified well for robustness improvement, strong stiffening, and additive manufacturing, respectively. The reason for the different effects can be found in their average sizes and size distribution. Due to the promising results, a flow chart for local value chains is derived on the example of yet unused cassava wastes, which can be converted in parallel.
Structural build-up describes the stability and early-age strength development of fresh mortar used in 3D printing. lt is influenced by several factors, i.e. the composition of the print able material, the printing regime, and the ambient conditions. The existing modelling approaches for structural build-up usually define the model parameters for a specific material composition with out considering the influence of the ambient conditions. The goal of this contribution is to explicitly include the temperature dependency in the modelling approach. Temperature changes have signifi cant impact on the structural build-up process: an increase of the temperature leads to a faster dissol ution of cement phases and accelerates hydration. The proposed extended model includes temperature dependency using the Arrhenius theory. The new model parameters are successfully calibrated based on Viskomat measurement data using Bayesian inference. Furthermore, a higher impact of the temperature in the re-flocculation as in the structuration stage is observed.
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.
Design : and use of engineered recycled mineral admixtures obtained from industrial and mineral waste are promising strategies to increase the range of materials suitable for use in cement-based composites. In this work, Portland cement-blended pastes containing mineral admixtures designed for improving particle packing were evaluated in the presence of low- and high-charge polycarboxylate-based superplasticizers. The powders were obtained from basic oxygen furnace slag, iron ore tailings, quartz mining tailings, and quartzite mining tailings. The zeta-potentials of the particles were obtained via electrophoretic mobility. The flow properties were evaluated by rheological tests performed in a Couette type rheometer. The hydration kinetics was evaluated by isothermal calorimetry and an adapted method based on the Vicat needle test. The high-charge PCE and the finer mineral admixtures produced more stable blends. Coarser mineral admixtures led to increased flowability and delayed hydration compared to finer ones. Steel slag powders presented the most significant plasticizer effects, but also the largest setting delays and segregation tendency. Quartz-rich superfines reduced the setting delays caused by the superplasticizers. In summary, both superplasticizers were effective in improving flow properties, but the high-charge PCE was effective in preventing segregation in pastes containing mineral admixtures coarser and heavier than cement.
Flowable concretes can differ significantly from traditional vibrated concrete. Concrete types like self-compacting concrete (SCC), ultra high performance concrete (UHPC) and high performance fibre reinforced cementitious composites (HPFRCCs) require novel mix design approaches. This has consequences for the production and the performance in the hardened state. Mix designs for flowable concretes can incorporate a wide variety of innovative admixtures or components: e.g. superplasticisers increase the flowability and allow for significant reduction of the water content, shrinkage compensating admixtures or superabsorbent polymers support sound and damage free curing processes, viscosity modifying admixtures enhance the robustness, and new fibre types allow for sophisticated and tailored structural performance.
The new Model Code has limitations regarding the application of flowable concrete, e.g. thresholds for the minimum aggregate size and the maximum strength. Provisions are added to include fibres for structural design. fib Task Group 4.3 aims at facilitating the use of innovative flowable materials for designing concrete structures and considers three aspects of flowable concrete: material properties, production effects and structural boundary conditions and performance. This paper reports about the progress of fib TG 4.3 related to the mix design of flowable concrete and discusses the present state-of-the-art concerning admixtures and robustness.
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.
Ordered mesoporous silica materials such as COK-12, analogous to the well-known SBA-15, are characterized by high surface areas and unique features such as defined pore sizes in the meso-size range and high pore ordering.
The aim of this work was to prove the washing step and choice of calcination and aging temperature during the COK-12 synthesis as effective tools in tailoring, markedly improving the specific surface area, pore size, and pore volume. By controlling the aging temperature, the pore size was linearly adjusted between 5.7 and 8.1 nm, while preserving the hexagonal ordering of the pores. The synthesized COK-12 powders possess pore volumes and specific surface areas up to 1.23 cm3 g−1 and 860m2 g−1, respectively, which is markedly higher than what has previously been reported about COK-12. The presented results and the environmentally friendly character of the synthesis will make COK-12 more interesting for future adaption to the industrial processes, for example in catalysis, adsorption, or drug delivery.
Covalent bridges play a crucial role in the folding process of sequence-defined biopolymers. This feature, however, has not been recreated in synthetic polymers because, apart from some simple regular arrangements (such as block co-polymers), these macromolecules generally do not exhibit a controlled primary structure—that is, it is difficult to predetermine precisely the sequence of their monomers. Herein, we introduce a versatile strategy for preparing foldable linear polymer chains. Well-defined polymers were synthesized by the atom transfer radical polymerization of styrene. The controlled addition of discrete amounts of protected maleimide at precise times during the synthesis enabled the formation of polystyrene chains that contained positionable reactive alkyne functions. Intramolecular reactions between these functions subsequently led to the formation of different types of covalently folded polymer chains. For example, tadpole (P-shaped), pseudocyclic (Q-shaped), bicyclic (8-shaped) and knotted (α-shaped) macromolecular origamis were prepared in a relatively straightforward manner.