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Eingeladener Vortrag
- nein (109)
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.
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.
Thermography is one on the most promising techniques for in-situ monitoring for metal additive manufacturing processes. The high process dynamics and the strong focus of the laser beam cause a very complex thermal history within the produced specimens, such as multiple heating cycles within single layer expositions. This complicates data interpretation, e.g., in terms of cooling rates. A quantity that is easily calculated is the time a specific area of the specimen is at a temperature above a chosen threshold value (TOT). Here, we discuss variations occurring in time-over-threshold-maps during manufacturing of a defect free cuboid specimen.
All over the world, microplastic (MP) particles (particle size: 1 - 1.000 µm) are found in water, soil, air, biota and even food products. But plenty of these discussed findings are based on a very low number of real datasets, which are extrapolated to general projections. Furthermore, most data are not comparable because the strategies for sampling, sample preparation and detection methods are not harmonised/ or standardised. This would require extensive proficiancy tests. Because of the ubiquity presence and the unclear risks, which might arise from those particles, various political and environmental organisations (i.e. OECD, UNEP, WHO) identify the reduction of plastic entry in the environment as a key challenge for now and the future. This challenge includes the identification of relevant entry pathways but also the demand of harmonised, meaningful and reliable analytical procedures.
Regarding this task within the last few years, a fast practical solution for MP analysis has been developed, which includes the steps of representative sampling, adequate sample preparation and fast detection. Sampling is done by fractional filtration over sieves with mesh sizes of 500, 100, 50 and 5 µm [1]. The received samples are measured by ThermoExtraction/Desorption-Gas Chromatography-Mass Spectrometry (TED-GC-MS) [1,2]. for the most abundant polymers used in practice, which are polyethylene (PE), polypropylene (PP), polystyrene (PS), polyethylene terephthalate (PET), polyamide (PA) and acrylate as well as styrene-butadiene-rubber (SBR), a main component of tires.
The present presentation will give first-time insight in a comprehensive dataset of microplastic analysis for an exemplary urban sewage system. MP mass contents of different waters at several days, such as greywater, stormwater retention tank, influent and effluent of a wastewater treatment plant (WWTP) within an urban sewage system in Germany are determined. Furthermore, the mass of the polymers found in dry weather and rain weather flow are compared. The use of these large datasets allows first expressive conclusions regarding the contribution of urban sewage system to the MP entry sources in the environments.
We found PP and PS in all different waters. Furthermore, there is SBR in influent and also in effluent of the WWTP. Surprisingly, we could also detect hugh amounts of PE in the effluent of the WWTP.
Microbiologically influenced corrosion (MIC) is a highly unpredictable process involving a complex group of microorganisms, including sulfate-reducing bacteria and methanogens. Standard laboratory MIC testing using static serum bottle enrichments is an easy but limited method, offering poor resolution on the biomineralization process of corrosion products. An example of this is the presumed corrosion product siderite by corrosive methanogens (Mi-MIC). Previous publications reported siderite was the sole corrosion product of M. maripaludis using metal coupons incubated under stationary conditions.
However, the formation of siderite is closely related to the surrounding environmental conditions, i.e. pH, CO2 concentration, flow and temperature. Thus, siderite as the sole corrosion product of Mi-MIC remain inconclusive and questionable. To study Mi-MIC effectively, a novel versatile multiport flow-column corrosion monitoring system (MFC) was developed. MFC allows sectional corrosion rate determination under flow conditions using different types of material, inoculum and packing material. MFC offers great flexibility, ease of operation and accurate corrosion measurements that can be combined with many other techniques. Using MFC, we studied multiple strains of methanogens and compared it with sulfate-reducing bacteria under neutral and low pH conditions. It was revealed by MFC that corrosive methanogens have equally high corrosion potential as sulfate-reducing bacteria. Additionally, siderite is not the dominant nor sole corrosion product of Mi-MIC. Thus, effective corrosion monitoring and establishing standard laboratory practices, i.e. incorporating MFC as part of regular testing process, will provide deeper understanding of MIC. This will allow further microbial electrophysiology understandings, contributing to effective mitigation strategy development.
Polyaniline/Silicon Dioxide Composite-Based Coating for Corrosion Protection in Geothermal Systems
(2020)
Geothermal energy is one of the cleanest renewable alternatives to reduce the dependency on fossil fuel [1, 2]. Despite its promising future, its implementation faces various challenges, one of them being corrosion processes. To implement this energy, hot fluids are pumped from a geothermal well. These hot fluids originate from deep within the earth, so consist of different ionic species and gases in a wide range of temperatures, which lead to their corrosive nature. In terms of geothermal energy resources, Indonesia is at the forefront, with the highest preserved geothermal energy in the world of about 29 GWe and 312 potential geothermal locations [3]. Geothermal wells in Sibayak (North Sumatera), Indonesia, belong to young stratovolcanoes and have operating temperatures varying from 36 °C at the near ground surface to 310 °C at the bottom of the well, which is liquid-dominated with acidic and saline properties [4, 5]. Therefore, this geothermal fluid creates an aggressive environment that is conducive to corrosion of the powerplant infrastructure.
Parts of the geothermal powerplant infrastructure, such as pipelines and heat exchangers, are commonly made of metals, e.g. carbon steel and stainless steel. Consequently, they may undergo corrosion and scaling when exposed to the geothermal fluid, especially for carbon steel. To ensure the safety and longevity of a geothermal powerplant, the infrastructure is constructed of expensive corrosion resistant alloys [6–10], e.g., titanium and Ni-Cr based alloys, or carbon steel which needs to be protected by coatings or inhibitors.
To address the corrosion of carbon steel in the geothermal environment, artificial geothermal water was used to simulate a geothermal well in Sibayak, Indonesia, with pH 4 and a saline composition of 1,500 mg/l Cl-, 20 mg/l SO42-, 15 mg/l HCO3-, 200 mg/l Ca2+, 250 mg/l K+, and 600 mg/l Na+. Carbon steel underwent the most severe corrosion at 150°C in an oxygen-containing solution with a corrosion rate of 0.34 mm/year, which is approximately ten times higher than that in the absence of dissolved oxygen. In all conditions, pitting corrosion was observed, which necessitate a protection strategy on carbon steel. In order to promote a cost effective and locally available option, this work focused on an easily applicable coating which utilized local resources.
Toward developing such protective coating based on the locally available resources in Indonesia which can yield good corrosion resistance and thermal stability in geothermal environment, two additional components, i.e. polyaniline (PANI) and silicon dioxide, were used to modify an alkyd-based commercial coating. The selection of the alkyd-based coating as a matrix focused on the industrial convenience basis, where the coating application procedure should be simple and easy to apply within reasonable costs. The alkyd-based coating underwent severe blistering when exposed to the artificial geothermal water at 70 and 150°C due to the reaction between CaCO3 (as one of its components) and the artificial geothermal water, as well as a possible alkyd hydrolysis in the initial stage of exposure. In the oxygen-free solution, the degradation was controlled by chemical and thermal reactions, whereas in the aerated condition, oxidization at the coating surface further accelerated polymer degradation.
PANI was chosen as one of the anticorrosion pigments which was widely developed over the past decades. To investigate the interaction between PANI and the artificial geothermal water, PANI film was electrochemically deposited on the carbon steel surface and exposed to the artificial geothermal water. Electrochemically synthesized oxalate-doped PANI was protective against corrosion of carbon steel in artificial geothermal water at room temperature. The mechanism involved an exchange of electroactive species within the coating layer, as confirmed by electrochemical impedance spectra. Interaction of ionic species, such as Cl-, Na+, Ca2+ from the artificial geothermal water, with the outer layer of PANI is suggested both at 25°C and 150°C, based on the EDX spectra of the coating surface after exposure to the artificial geothermal water. Thus, the protection mechanism of PANI is not solely based on the physical barrier layer properties, but rather associated with the redox mediated properties of PANI, which selectively allow ionic species intrusion from the electrolyte into the PANI layer. Although PANI is a promising candidate as an anticorrosion coating, its morphological characterization reveals that electrochemically deposited PANI is not stable for an application at 150°C. Therefore, another approach was used to promote better protective behavior of PANI by dispersing chemically synthesized PANI in the alkyd-based coating.
To enhance the thermal stability of the coating, silicon dioxide (SiO2) was added, which was able to prolong the sustainability of coated metals until 28 days compared to the unmodified alkyd-based coating, which underwent a change in color to brown/orange only within 7 days of exposure. This improvement might be associated with the role of SiO2 to proportionate the thermal expansion coefficient of the coating system to be compatible with that of carbon steel. Although the coating is thermally enhanced, the electrolyte might still intrude through the coating resulting in the change of coating color after 28 days of exposure in the artificial geothermal water. When PANI was added, the coating system provided an active corrosion protection on the carbon steel surface. The chemical and morphological characterization of the PANI-alkyd and SiO2-alkyd coating system showed that coatings were improved, and no blisters were observed, albeit the degradation continued. Based on the results of exposure tests, the combined coating system was further investigated.
The combinational coating of PANI/SiO2-alkyd was used with 2 wt% of PANI and 15 wt% of SiO2. Electrochemical tests indicated cathodic protection at 150°C, as the Ecorr of PANI/SiO2 remained approximately 400 mV lower than the carbon steel potential. The impedance spectra of the combinational coating of PANI/SiO2 showed a continuous decrease in the absolute impedance value over time. A significant decrease was observed within one day of exposure, followed by a slow gradual decrease, which might be associated with water absorption in the coating. FTIR spectra revealed that several peaks associated with the organic portion of the coatings were reduced after the specimens were exposed for 6 months. However, the absorption peaks related to the inorganic portion of the coatings remained stable until 6 months. Morphological characterization of the combinational coating of PANI/SiO2 showed that there were no blisters or significant discoloration of coatings after long-term exposure for 6 months in artificial geothermal water at 150°C, indicating that the chemical degradation does not significantly affect the functionality of the coating. This clearly shows the durability of PANI/SiO2 coating in the geothermal condition, suggesting that this coating can be used for such geothermal application. However, further testing of this coating should be conducted in a real geothermal environment on-site to ensure safety and viability.
Recent studies have confirmed the widening of the weld pool interface, known as a bulge effect, during deep penetration high power laser beam welding. The link between such geometric particularities of the weld pool shape and the hot cracking phenomena is significant. The present work seeks to extend the level of understanding by investigating their relationship. A coupled multiphysics, multiscale numerical framework is developed, comprising a series of subsequent analyses. The study examines the influences of the bulge on the three most dominant effects causing hot cracking, namely the thermal cycles, the mechanical loading, and the local microstructure. The bulge in the weld pool shape forms approximately in the middle of the plate, thus correlating with the location of hot cracking. It increases the hot cracking susceptibility by enhancing the three dominant effects. The numerical results are backed up by experimental data.
Recent studies have confirmed the widening of the weld pool interface, known as a bulge effect, during deep penetration high power laser beam welding. The link between such geometric particularities of the weld pool shape and the hot cracking phenomena is significant. The present work seeks to extend the level of understanding by investigating their relationship. A coupled multiphysics, multiscale numerical framework is developed, comprising a series of subsequent analyses. The study examines the influences of the bulge on the three most dominant effects causing hot cracking, namely the thermal cycles, the mechanical loading, and the local microstructure. The bulge in the weld pool shape forms approximately in the middle of the plate, thus correlating with the location of hot cracking. It increases the hot cracking susceptibility by enhancing the three dominant effects. The numerical results are backed up by experimental data.
CHG is very different compared to other graphite degenerations or defects;
Filigree, multi-branched string-like, 3d interconnected structure;
Morphology and volumetric amount of CHG cannot be accessed by stereological interpretation of 2d section data;
Field-tested, technically established method to quantify CHG in components not available;
Fatigue: CHG causes substantial reduction in fatigue limit and significant increase in crack growth rate;
Therefore: Avoid or exclude CHG!
Using a novel optical measurement technique together with the OF algorithm, a two-dimensional deformation analysis during welding was conducted.
The OF technique was the first of its kind to provide a measurement of the full strain field locally in the immediate vicinity of the solidification front. The local critical strain and strain rate in vicinity of the solidification front has observed 1.57%, 28 %/s, respectively.
A self-restraint hot cracking test (free edge test) was used in combination with a novel optical measurement technique to determine the critical straining conditions for solidification cracking for the stainless steel grade 1.4828 (AISI 309). The Lucas-Kanade algorithm for the optical flow (OF) calculation was implemented to obtain the full-field displacement and then the full-field strain.
The use of external laser illumination with appropriate filters allows to obtain good image quality with good contrast. The critical straining conditions required for solidification cracking can be obtained by means the proposed technique in the immediate vicinity of the solidification front. A very good repeatability was demonstrated for the used measurement technique. The critical straining conditions for solidification cracking for the tested steel und under this welding conditions has been detected
This poster presents the focused ion beam preparation methodologies developed within the framework of the EU funded EURAMET project ADVENT (Advanced Energy-Saving Technology).
It summarises the key breakthroughs achieved for various in situ investigation techniques, e.g. in situ experiments at the Synchrotron facility BESSY II (IR-SNOM and XRS), TEM and SMM instrumentation.
The created experimental devices from diverse thin-film semiconductor materials paved the way to dynamic structural studies bearing the potential to determine nanoscale correlations between strain and electric fields and, moreover, for the fundamental development of new in situ capabilities.
Sufficient adhesion/tensile strength are basic requirements for any coating/composite material. For coatings, adhesive strength in N/mm2 is of Major interest for various applications such as decorative and water-repellent coatings on wood (paints and varnishes), optical coatings on glass and polymers (reflectors and filters), electrical coatings on semiconductors, glass and polymers (conducting and bondable layers), mechanical coatings on metals and polymers (wear-reduction, scratch-resistance) and adhesion-promoting layers. For composite materials, tensile strength in N/mm2 is also a key quantity for carbon fiber reinforced composites (CFC), laminates and adhesive-bonded joints. Centrifugal adhesion testing (CAT) transfers the single-sample tensile test from a tensile or universal testing machine into an analytical centrifuge as multiple-sample test of up to eight test pieces. The one-sided sample support instead of a two-sided sample clamping and the absence of mounting- and testing-correlated shear forces provides fast and reliable results both for adhesive strength and bonding strength by means of bonded test stamps. For bonding strength, the evaluation of failure pattern from microscopic inspection is required in order to determine the failure pattern according to ISO 10365 such as adhesive failure (AF), delamination failure (DF) and cohesive failure (CF). Hence, one test run by CAT-technology provides either statistics or ranking of up to eight samples at once. For adhesive strength of coatings, a variety of examples is discussed such as ALD-Al203 layers as adhesion promoters, evaporated Ag-layers on N-BK7 glass, sputtered Cr- and Al-layers on Borofloat 33 glass, evaporated Au-films on N-BK7 glass and sputtered SiO2 -layers on CR39 Polymer. Provided adhesive or bonding strength are high enough, the substrate or the joining part may also fail.
THz and mid IR spectroscopy of high-molecular PE (HMW) and ultra high-molecular PE (UHMW) reveals modifications of the molecular structure. Characteristic absorption bands are changed if the two materials are exposed by γ-Co60 radiation up to 600 kGy and subsequently stored at an annealing temperature of 398 K until for 729 days. UHMW-PE and HMW-PE behave differently during the ageing process because of their molecular weight and inherent structure distinctions. The spectroscopic data offer characteristic absorption bands, which have been used to describe the complete ageing process in more detail. For instance, the integral absorption in the B1u THz-region can be used to describe quantitatively the reduction of crystallinity. The formation of trans vinylene unsaturation and the decay of vinyl during ageing can be observed in detail in the mid IR range.
Novel Technique for On-Line Monitoring of the Curing Process of Fiber Reinforced Polymer Composites
(2020)
A specially designed experimental set up has been integrated into a commercially available FT IR Spectrometer for ATR experiments on Epoxy Systems. Representative data of far infrared spectra measured during the curing process at different temperatures of an epoxy system will be presented in dependency of the curing situation. The experiments and the selected set up are discussed to demonstrate its potential for future monitoring and ageing control applications during a manufacturing process of polymer composites.
Nanoparticle suspensions were microprinted onto TEM grids for subsequent analysis by SEM/TSEM and evaluation of particle numbers using Image J software. Various nanoparticle types, concentrations and printing conditions (temperature, rel. humidity) were evaluated in order to determine the optimal conditions for producing a uniform distribution of particles on the substrate and eliminating the coffee ring effect.
A series of different nanoparticle suspensions (Gold, Latex, and SiO2 in varying concentrations) were microprinted onto TEM grids in a 4 x 4 array in the concentration range 7x10^8 to 1x10^11 NP/mL and imaged with SEM and TSEM. Concentrations and printing conditions (temperature, relative humidity) were varied in order to minimize the coffee ring effect.
The fatigue design of metallic components is usually based on two different approaches, namely total life and damage tolerance. The former takes into account both the initiation and propagation stages. The latter is based on fracture mechanics and needs an initial defect, which propagates until the critical size under cyclic loading, provided it is large enough. In this case, a residual life rather than a total life is obtained. The overall lifetime of a cyclically loaded structure involves four consecutive stages: a) crack initiation; b) propagation of microstructurally short cracks; c) propagation of physically/mechanically short cracks; d) propagation of long cracks. Considering the propagation from the short crack regime, the damage tolerance approach can be extended to adequately calculate the total life of a component.
The fatigue strength of metallic materials containing defects depends on the non-propagation condition of small cracks emanating from these defects. In this work, the presence of mechanically short cracks from the beginning of the component's life is considered. Consequently, the methodology of analysis must be able to treat adequately local ligament yielding effects typical for short cracks and must include the thorough description of the crack closure effect up to the long-crack regime. In the analysis based on long cracks, the linear-elastic condition is mostly satisfied which allows the use of the linear elastic parameter ΔK for describing the crack driving force. On the contrary, this assumption is not adequate for mechanically short cracks because the crack depth is in the order of the plastic zone. Instead, an elastic-plastic driving force should be considered. Furthermore, the gradual build-up of the plasticity-induced crack closure effect must be considered, which implies a transition from the intrinsic (effective) threshold value, ΔKth,eff, to the long-crack threshold, ΔKth,LC.
The effective component is a material parameter which is dependent on the elastic properties and crystal lattice. The gradual build-up of crack-closure is described by ΔKth,op which is a function of the plastic properties, grain-size, environment conditions, load ratio and crack-depth. The crack closure can be characterized experimentally by the so-called cyclic R-curve. Some other crack closure effects, such as roughness or oxide-debris induced, might be incorporated as well.
The knowledge of the cyclic R-curve can be useful to determine the largest non-propagating crack size at the material fatigue limit. This is realised by means of the so-called cyclic R-curve analysis: The tangent criterion between the driving force and the cyclic R-curve define the transition between crack arrest and propagation. In this regard, a0 is defined as that crack depth which will only grow into a non-propagating crack due to the development of crack closure.
The procedure outlined briefly here has been successfully applied to the determination of the fatigue limits of steel weldments. Considering the stochastic distribution of the weld geometric parameters (namely, weld toe radius, the flank angle, and the excess weld metal) it is possible to perform a full probabilistic cyclic R-curve analysis and determine this way the statistical distribution of the initial crack size at the weld toe at the fatigue limit.
Laser material processing is an emerging technology that generates surface functionalities on the basis of optical, mechanical, or chemical properties. In the form of laser surface texturing (LST), it has attracted a remarkable amount of research to tailor surface properties towards various tribological applications. The main advantages of this single-step, laser-based technology are the contactless machining, featuring a high flexibility, efficiency, and speed, along with the excellent quality of the processed products. LST can be applied precisely localized to sub-micrometric areas, but, via laser beam scanning, it is also feasible for structuring large surface areas at the square meter size.
This Special Issue focuses on the latest developments concerning the tribological performance of laser-generated periodic surface nano- and microstructures and their applications. This includes the laser-based processing of different surface patterns, such as “self-organized” laser-induced periodic surface structures (LIPSS, ripples), grooves, micro-spikes, hierarchical hybrid nano-/micro-structures, microfeatures generated by direct laser interference patterning (DLIP), or even dimples or other topographic geometries shaped by direct laser modification or ablation. The applications of these periodically nano- and micro-patterned surfaces may improve the lubricated or non-lubricated tribological performance of surfaces in conformal and even non-conformal contact through a reduction of wear, a variation of the coefficient of friction, altered load carrying capacity, etc., resulting in energy saving, improved reliability, increased lifetimes as well as durability, leading in turn to extended maintenance intervals/reduced down-time. This can be beneficial in terms of bearings, gears, engines, seals, cutting tools, or other tribological components. Fundamental aspects addressed may involve the investigation of the relevant physical and chemical effects accompanying the laser-generated nano- and microscale topographies, such as alterations of the material structures, the hardness, superficial oxidation, the role of additives contained in lubricants, surface wettability, micro-hydrodynamic effects, etc.
For this Special Issue we aim to attract both academic and industrial researchers and would like to provide a bridge between research in the fields of tribology and laser material processing in order to foster the current knowledge and present new ideas for future applications and new technologies.
The intention of the presentation is to inspire a discussion on the needs and challenges for the digitalisation of SOPs. SOPs are available for the disciplines of physical-chemical characterisation, for toxicology, for environmental applications and for exposure applications. Furthermore the SOPs need to be integrated in the regulatory framework and need to be detailed enough for the digital processing. This is highlighted in this presentation.
Reaction sintering and sintering additives for cost-effective production of thermoelectric oxides
(2020)
Thermoelectric oxides attract much interest recently. Although their thermoelectric properties are inferior to non-oxides, they exhibit distinct advantages. Thermoelectric oxides are stable in air at higher temperatures, their raw materials are less toxic, and more abundant. To enhance attractivity of these materials for industrial applications, production costs need to be reduced.
Conventionally, the legs of thermoelectric generators are sintered from green bodies of previously synthesized powder. Reaction-sintering is a fabrication method without a powder synthesis step, as the final phase is formed during the sintering from a raw material mixture. Moreover, the reduction of chemical potential during reaction-sintering is effective as an additional driving force for sintering. We show that reaction-sintering increases the densification of CaMnO3 (n-type, Sm doped). Consequently, the electrical conductivities improved by about 100 % leading to superior power factors (PF = 230 µW/mK² for CaMnO3).
Another approach to reduce the production costs is to lower the sintering temperature by adding sinter additives. The addition of 4 wt% CuO to CaMnO3 lowers the sinter temperature from 1250 °C to 1050 °C. The achieved power factor PF = 264 µW/mK is more than two times higher as reported in literature for the same dopant.
Thermoelectric materials can convert waste heat directly into electrical power by utilizing the Seebeck effect. Calcium cobaltite (Ca3Co4O9, p-type) and calcium manganate (CaMnO3, n-type) are two of the most promising oxide thermoelectric materials. The performance of these materials is evaluated by the power factor PF = S²∙σ and the figure of merit ZT = (PF ∙ T) / κ, demanding high Seebeck coefficient S, high electrical conductivity σ and low thermal conductivity κ. The latter two are increasing with increasing relative sinter density. According to theory, the relative density of ceramics can be improved by increasing the driving force for sintering. This study investigates different approaches to increase the driving force for sintering of Ca3Co4O9 and CaMnO3 to improve densities and thermoelectric properties.
The following approaches were applied: minimizing the energy input during powder synthesis by calcination, fine milling of the powder, using reaction-sintering without a powder synthesis step, and adding a transient liquid phase by sinter additives.
All different approaches led to an increased densification and thus higher electrical conductivity and higher PF. Thermal conductivity increased as well but not to the same extent. E.g. reaction-sintering increased the densification of Ca3Co4O9 (p-type) and CaMnO3 (n-type). Consequently, the electrical conductivities improved by about 100 % for both oxides leading to superior power factors (PF = 230 µW/mK² for CaMnO3). Although the thermal conductivity increased as well by 8 %, the figures of merit (ZT) were significantly higher compared to conventionally sintered bars. The addition of 4 wt% CuO as a sinter additive to CaMnO3 lowers the sinter temperature from above 1250 °C to below 1100 °C and increases the relative density. Due to the increased density, both electrical conductivity and PF increased by more than 200 % even though the sintering temperature was 150 K lower.
Porous ceramic diesel particulate filters (DPFs) are extruded products that possess macroscopic anisotropic mechanical and thermal properties. This anisotropy is caused by both morphologic features (mostly the orientation of porosity) and crystallographic texture. We systematically studied those two aspects in a cordierite and two aluminum titanate (AT) ceramic materials of different porosity using mercury porosimetry, gas adsorption, electron microscopy, X-ray diffraction, and X-ray refraction radiography. We found that a lower porosity in AT content implies a larger isotropy of both the crystal texture and the porous space orientation. We also found that, analogous to cordierite, AT crystallites do align with their axis of negative thermal expansion along the extrusion direction. However, unlike what found for cordierite, the aluminium titanate crystallite form is such that a more pronounced (0 0 2) texture along the extrusion direction implies porosity aligned perpendicular to it.
As opposed to reviewing results on experimental determination of residual stress by diffraction, this paper discusses the open issues when dealing with residual stress determination in additive manufactured parts, in particular those manufactured with laser powder bed fusion techniques. Three points are addressed in detail: (a) the proper determination of the strain-free reference d0, (b) the problem of the determination of the principal axes, and (c) the use of the correct diffraction elastic constants. It is shown that all methods to determine the strain-free reference d0 suffer from caveats, and care must be taken in evaluating the most suitable for the problem being tackled. In addition, it is shown that, in some systems, the principal axes do correspond to the geometrical axes of the specimen, but this needs to be systematically checked, especially in the case of uni- or bidirectional hatching strategies. Finally, the need to experimentally determine the proper diffraction elastic constants is underlined, especially in the case of strongly textured specimens, which again depends on the deposition strategy.
A new approach towards performance-related design and scientific evaluation of joint sealing systems
(2020)
While there is a permanent improvement of concrete pavement mixtures and pavement construction types over the last decades, the state-of-the-art joint sealing materials and joint constructions seem to stagnate on an antiquated empirical level. This status has been reaffirmed in the latest European standard.
The consequences in the motorway network due to unsatisfying capability and durability of joint sealing systems are unacceptable. In addition, inadequate traffic performance (noise emissions, roll-over comfort) and traffic safety losses in the joint area of concrete pavements are existing challenges. These deficits and weaknesses reflect a demand for joint sealing materials and constructions whose approval requirements take functional aspects into account. Furthermore a sufficient analysis of decisive loads and a practice-oriented method to evaluate the requirements towards performance and durability is still missed.
In this contribution decisive loads to German highways are analyzed. The design of test specimen for representative functional testing of joint sealing systems is discussed. The focus is on the geometry of the test specimens and the used concrete mixture. Finally, a new approach for a function-orientated test concept that considers representative load functions is presented. The potential of this approach to validate the durability and capability of various joint sealing systems is also presented using an example.
While there is a permanent improvement of concrete pavement mixtures and pavement construction types over the last decades, the state-of-the-art joint sealing materials and joint constructions seem to stagnate on an antiquated empirical level. This status has been reaffirmed in the latest European standard. The consequences in the motorway network due to unsatisfying capability and durabilty of joint sealing systems are unacceptable. In addition, inadequate traffic performance (noise emissions, roll-over comfort) and traffic safety losses in the joint area of concrete pavements are existing challenges. These deficits and weaknesses reflect a demand for joint sealing materials and constructions whose approval requirements take functional aspects into account. Furthermore a sufficient analysis of decisive loads and a practice-oriented method to evaluate the requirements towards performance and durability is still missed. In this contribution decisive loads to German highways are analyzed. The design of test specimen for representative functional testing of joint sealing systems is discussed. The focus is on the geometry of the test specimens and the used concrete mixture. Finally, a new approach for a function-orientated test concept that considers representative load functions is presented. The potential of this approach to validate the durability and capability of various joint sealing systems is also presented using an example.
This book introduces to aspects to be considered when dealing with coatings and linings. Philip A. Schweitzer covers and compares a variety of specific coatings and their applications. In 18 chapters he divided the content into two main parts: linings and coatings.
All professionals involved in design and maintenance processes get by this book a compact survey of necessary considerations which needs to be done when applying surface protection measures. The literature references at the end of some chapters support the readers finding additional information about the special topic, mainly written by the author himself. Since this newly issued paperback edition is a 1:1 re‐print of the 2001 hardcover version, neither current publications are referenced, nor revisions were made.
The first edition of this book, published within the series “Materials Science – Metals and Alloys”, provides broad knowledge of this interesting and widely applied metal from manufacturing and production to finishing and application in 13 chapters, written by 29 contributors. Each chapter is separately concluded and ends with references used.
This book fulfills its intention of conveying comprehensive and cutting‐edge knowledge of magnesium alloys. It is useful for practicing engineers, researchers and students searching for an instructional and reference source.
his fully updated examination of sustainable processes for gaseous and liquid biofuels production, published for the second time within the series “Biomass, Biofuels, Biochemicals”, provides 33 contributions made by 120 authors. They present a holistic view of biofuels in research, operation, scale‐up and application. Comparing to the first edition, all chapters have been updated and new chapters covering topics of current interest, including sustainability and biohydrogen have been added.
By its wide overview on existing technologies, this book provides state‐of‐the‐art information and knowledge to the desired readership, like post‐graduates, researchers in the area of biofuels, wastewater treatment, alternate energy sources, renewable energy from biomass, chemical and biochemical engineers, microbiologists, biotechnologists working in academic and research institutes as well as in industry and governmental agencies.
Since geothermal wells are a feasible energy source to replace fossil fuel supply, many technologies have been developed to take advantage of geothermal energy. Nevertheless, service conditions in geothermal facilities are in many cases extreme in terms of corrosion due to the chemical composition of hydrothermal fluids and temperatures. Therefore, materials selection based on preliminary material qualification is essential to guarantee a secure and reliable operation of the facilities. During operation of a geothermal research facility in Groß Schönebeck copper and lead effects have been found downhole. Occurring mechanisms and measures to prevent precipitation or scaling needed to be investigated as well as potential influences of such precipitates on corrosion resistance of metallic materials used for equipment.
This contribution deals with the evaluation of the corrosion behavior of carbon steel and corrosion resistant alloys in copper and/or lead containing artificial geothermal water, simulating the conditions in the Northern German Basin.
The behavior of these materials in an artificial geothermal water obtained by electrochemical measurements and exposure tests are presented. While carbon steel exhibits precipitation and deposition, higher alloyed material shows different response to such species and a higher resistance in saline geothermal water.
Basing on these results the suitability of the investigated corrosion resistant alloy is given for use in such conditions, whereas carbon steel creates difficulties due to its susceptibility to Cu- and Pb-precipitation.
This paperback issue of the 2007 hardcover version within the “Corrosion Engineering Handbook” series presents various materials and methods for controlling and protecting against corrosion instead of using expensive alloys to construct a tank or processing vessel.
This book is a very comprehensive collection of the current knowledge about applied linings and coatings. So, it fulfills its intension, “that regardless of what is being built, … information for … whoever is responsible for the selection of material of construction will be found in this book to enable them to avoid unnecessary loss of material through corrosion”, to a very large extent.
This book by Scrivener Publishing contains 14 chapters written by 82 leading scientists, experienced in the field of coatings. They demonstrate mechanisms, usage and manipulation of cutting‐edge coating methods. Each chapter is well structured and ends with a conclusion, highlighting the content. The book is divided into 3 parts: “Materials and Methods”, “Coating Materials Nanotechnology” and “Advanced Coating Technology and Applications”.
Finally, this book provides a comprehensive insight into innovative research in advanced coating materials and state‐of‐the‐art technologies, without being a real textbook. It fulfills its intension of being beneficial both for technicians and scientists.
Since nanoscience has a tremendous impact on the development of electrochemistry, Wiley‐VCH paid attention to that by publishing thisbook as volume 17 within the series “Advances in Electrochemical Science and Engineering”.
This collection of “nanoaspects”on electrodes provides a helpful overview on principles and current findings to readers interested in such applications. It fulfills its intention of being “a valuable resource for researchers working in such fields as electrochemistry, materials science, spectroscopy, analytical and medicinal chemistry”.
This book grew out of a course on polymer coatings held by the author at the university. It shall serve as an introduction to the wide field of polymer coatings. It is not intended to cover completely all facts on polymer coatings.
All chapters are well structured. Selected figures and formulas illustrate the content and contribute to a good understandability. At the end of each chapter some hints for further reading are provided.
Finally, the book fulfills its intention to introduce into the topic by providing basics on science and technology of polymer coatings, suitable for chemists in industry, materials scientists, polymer chemists and physical chemists.
This concise reference book,consisting of 2 volumes, provides “key scientific and technical properties and data” for “materials scientists, metallurgists, engineers,chemists, and physicists as well as academic staff, technicians, and students” dealing with such kind of materials.
Within its 3rd edition the previous work was extended by a chapter on occupational health and safety issues of materials, beside of the update of whole content. Within 22 chapters materials properties and data are summarized in many tables. Some facts are illustrated by drawings and diagrams for better understandability. Each chapter ends with a part on further reading arranged accordingly.
This edition, published as first issue within the series “Corrosion Atlas”, provides 181 corrosion case studies, collected from 29 contributors.
These Corrosion Atlas Case Studies provide a helpful tool required for engineers in their daily life to quickly determine and solve their equipment's corrosion problems by compact theoretical background and vivid examples. It fulfills the intension of the editors to be “the first centralized collection of case studies containing challenges paired directly with solutions together in one location”.
Currently, storage of electric energy is becoming more and more interesting in terms of applicability and efficiency. One way is the electrochemical storage by already well‐developed battery‐systems. This textbook provides an introduction into physical and chemical processes necessary for battery application.
This book fulfills its intension to serve graduate students of electrical engineering as an introduction into the field of batteries. Even students and interested readers of other faculties might find an introduction in physical and chemical background of batteries.
The aim of the work presented was the evaluation of corrosion resistance
of various materials in geothermal Waters as a base to create a catalogue of suitable materials for applications in (not only) German geothermal power plants.
Users shall be enabled to have a basis for designing such facilities. High alloyed corrosion resistant alloys are suitable and do not cause copper or lead deposition. They shall be chosen for future design of the piping system, either in massive or in cladded form, if crevices formation with non-metallic materials can be prevented!
Since data processing has now also found its way into materials science, there has been a great demand from users for a corresponding textbook. This book provides a guide to the latest advances of materials informatics and data mining for materials science. 46 authors introduce readers to methods, present tools and case studies to illustrate the power of materials informatics within this new field of application.
Often 3D‐printing and additive manufacturing are mentioned as the 3rd industrial revolution. In this conjunction this book provides a brief overview on additively manufactured metal pieces.
This book fulfills its intension to serve as an educational guide, providing a holistic picture encompassing science, technology and applications for the real‐life use of Metal Additive Manufacturing.
This contribution provides current findings regarding materials susceptibility for CCUS applications. Basing on results gathered in 2 German long-term projects (COORAL and CLUSTER) suitable materials are introduced as well as dominating impurities of the CO2 stream and corrosion mechanisms. Investigations cover the whole CCUS process chain and provide the following recommendations for certain parts. Commercially available carbon steels are suitable for compression and pipelines as long as moisture content and impurities are limited (water 50 to 100 ppmv, SO2 and NO2 ca. 100 ppmv).
Corrosion rates increase with increasing water content (0.2 – 20 mm/a).
Condensation of acids and therefore droplet formation is always possible, even at low water contents.
A low SO2 content within the CO2-stream might be more important than a low water content.
Cr13-steels showed a general susceptibility to shallow pitting and pitting. So, they seem to be not suitable for CCUS applications.
Low alloyed steels showed better corrosion behavior (predictable uniform corrosion).
For direct contact with saline aquifer fluids only high alloyed steels shall be used.
The possibility of creating patient-specific individual implants makes Additive Manufacturing technologies of special interest for the medical sector. For substitution of bone defects, powder based Additive Manufacturing by Binder Jetting is a suitable method to produce complex scaffold-like structures made of bioceramics with easily adapted geometries and controlled porosity. The process inherent residual porosity in the printed part, even though desired as it supports bone ingrowth, also leads to limited mechanical strength. Currently, bioceramic scaffolds made by Binder Jetting feature suitable biocompatible and biodegradable properties, while a sufficient mechanical stability is rather challenging. The purpose of this work is to apply the gas flow assisted powder deposition introduced in 2014 by Zocca et al., to the powder bed during printing of bioceramic tablets and scaffolds using α-TCP powder as feedstock. This enables exploiting the advantages of an increased powder bed density, thereby improving the mechanical properties of the printed parts.
Data quality is a vast term, which comprises the completeness, relevance (adequacy), and reliability of data. So far, many attempts to assure data quality have been pursued, and evaluation criteria for data quality have been established. One relatively novel but already well-known aspect of data quality refers to the concept of data FAIRness, which states that data should be: findable, accessible, interoperable and re-usable. In order to find, use, and access data, a user has to be guided properly. Such guidelines already exist for regulators and the scientific community. However, a ‘simple’ non-academic user from general society is very unlikely to be able to access or understand such data. Our objective in the H2020 project NANORIGO is to help and guide all types of users (i.e., scientists, regulators, industry workers, citizens, etc.) to access and make use of high-quality data and information from available and suitable data repositories in order to increase the transparency of and trust in nanotechnology.
At the end of the sixteenth century, a number of relics and artefacts were discovered in Granada, Spain. They included what became known as the Lead Books of the Sacromonte, twenty-one written artefacts made of circular lead leaves engraved in archaic Arabic characters. The authorship was attributed to some Arab disciples of St James the Greater considered to be the first evangelisers of the Iberian Peninsula. The texts, the materiality and the circumstances of the discoveries fuelled a debate surrounding their authenticity that lasted more than two centuries, a debate so fierce and controversial that not even papal condemnation in 1682 was able to stop it. Soon after the discoveries were made public, scholars highlighted the many contradictions and errors of a historical, linguistic and theological nature present in the texts, identifying members of the local Morisco community as possible forgers. This article focuses on how the scholarly community of the sixteenth and seventeenth centuries handled these findings and looks at the methods employed by the scholars to evaluate the authenticity of the artefacts. It will also look at how the particular interests of the various authorities involved influenced the acceptance or dismissal of relevant academic results.
Development and characterization of starch film and the incorporation of silver nanoparticles
(2020)
Starch is one of the biopolymers being used for bioplastic synthesis. For production, starch can be combined with different plasticizers, starches from different plant sources and even with nanomaterials to improve or to add film properties. The challenge of adding these, e.g. in the form of silver nanoparticles (AgNp) is to determine the concentration so as to avoid impairing the properties of the film, agglomeration or altering the visual characteristics of the film. In this study, a starch film synthesis route and the incorporation of silver nanoparticles has been proposed in order not to alter the properties of the film while maintaining the transparency and a clear colour of the starch film. The results showed that the proposed synthesis route is promising, efficient, reproducible, fast and the film has good mechanical properties.
A powerful tool to understand, demonstrate and explain the limits of the pulsed technique in terms of detectability and localizability of AM keyhole pores has been assessed by comparing the active thermographic approach (both experimental and FEM simulations) to Computed Tomography results;
✓ µCT results demonstrate that the intended defect geometry is not achieved; indeed a network of voids (microdefects consisting of small sharp-edged hollows with a complicated, almost fractal, inner surface) was found;
✓ both Exp-PT and FEM results explains clearly why no indication of defect related to the thermal contrasts could be found during the investigation of an uncoated surface. However, the application of further data evaluations focusing on the thermal behavior and emissivity evaluation (PPT post data processing) enable the detection of some defects;
✓ coating facilitates a closer inspection of inner defects, but inhomogeneities of the coating could impair the spatial resolution and lead to the emergence of hotspots (the FEM simulation reached its limit with this extreme geometry where a 25 µm thin disc is considered at a 1 cm thick specimen in millisecond time resolution);
✓ both Exp-PT and FEM results allow the conclusion that very short pulses of 200 ms or shorter should be sufficient to detect these defects below, but near the surface; besides a short duration of the thermal phenomenon it should be emphasized, about 0.04 s (high frame rate camera);
A new approach for fabrication of ceramic components with inner channels is proposed, as a result of the combination of two additive and one subtractive manufacturing processes. In this project, porcelain parts are manufactured by the Layerwise Slurry Deposition (LSD) process, meanwhile end milling and Direct Ink Writing (DIW) are applied to create channels on the surface of the deposited ceramic. Unique to the LSD process is the Formation of a freestanding powder bed with a mechanical strength comparable to conventional slip casted ceramic green bodies. Combining these three processes allows the manufacturing of ceramic objects containing an internal path of ink, which in this case was a graphite-based ink that can be further eliminated by heat treatment to obtain a porcelain object embedded with channels. The results show the capabilities of this method and its potential to fabricate not only parts with inner channels, but also multi-material and multi-functional components (such as integrated electronic circuits).
This is the repository of all experimental raw data used in the Scientific Reports publication "Specific adsorption sites and conditions derived by thermal decomposition of activated carbons and adsorbed carbamazepine" by Daniel Dittmann, Paul Eisentraut, Caroline Goedecke, Yosri Wiesner, Martin Jekel, Aki Sebastian Ruhl, and Ulrike Braun.
It includes
- overview_measurements.xlsx and overview_measurements.ods containing a list of all TGA experiments (TGA, TGA-FTIR, TED-GC-MS, and ramp-kinetics)
- TED-GC-MS.zip containing gas chromatography-mass spectrometry experimtent files for the Chemstation and OpenChrom
- TGA.zip containing thermogravimetric analyses raw data on evolved gas analyses experiments (TGA-FTIR and TED-GC-MS)
- TGA_kinetics.zip containing thermogravimetric analyses raw data on decomposition kinetic experiments (ramp-kinetics)
- TGA-FTIR.zip containing Fourier-transform infrared spectroscopy series files for OMNIC
- XRF.zip containing x-ray flourescence data on elemental composition