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Eingeladener Vortrag
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The aim of this work was the preparation of a novel stationary monolithic phase for affinity chromatography and HPLC-applications. Therefore, we have chosen porous glass filters that are available with different pore sizes as raw materials to prepare monolithic columns. We purchased VitraPOR 4 (10-16 μm pore size) and VitraPOR 5 (1.0-1.6 μm pore size) monolithic glass filters. The physical properties of these glass filters were characterized. The surface area, pore size distribution and the porosity were determined using mercury intrusion porosimetry and BET. These glass filters only exhibit flow through pores and therefore show no bimodal pore size distribution in the mercury intrusion curves. Due to their low permeability, the applied filters that exhibit an inner diameter of 8.0 mm and a length of 15.0±0.1 mm could be operated at flow rates more than 10 ml/min. High flow rates are favorable for fast separation experiments.
A combined experimental and numerical approach is applied for a numerical analysis of the non-uniform martensitic transformation kinetic on welding residual stresses and distortion of a single pass weld. The (γ → α)-transformation kinetic within the weld pool region is governed by a non-uniform distribution of the elements chromium and nickel. The single-pass weld was performed by use of the low-alloyed high-strength steel S960QL with the high-alloyed high-strength filler wire CN 13/4-IG®. A thermo-mechanical FE model of the welding process was experimentally validated against temperature field, solid phase distribution, transformation behaviour, X-Ray stress measurements and transient optical distortion measurements.
The experimentally determined and calculated weld residual stresses and transient distortion are in good agreement. It can be shown that the change on the (γ → α)-transformation kinetic driven by the inhomogeneous distribution of the chemical contents causes a strong influence on the weld residual stresses within the volume of the weld pool, which could promote crack propagation within the solidified weld pool by use of high-alloyed filler materials. Furthermore, a significant influence on the development of the transient welding distortion is visible. This influence should be respected during numerically calculation of welding distortion in case of multi-pass welding using interpass temperatures and high-alloyed filler materials.
A long list of criteria determining the hot cracking susceptibility already exists. A main influence on solidification cracking can result from the design of the welded construction, i.e. from the influence of external loads. Using the Controlled Tensile Weldability (CTW) test, an external load hot cracking test, the influence of constant pre-load and different extension rates on the solidification cracking behavior of GTA (Gas Tungsten Arc) welds in an austenitic (AISI 309) and a ferritic (AISI 441) steel were investigated. Compared to specimens welded allowing free shrinkage and welded with an applied constant tensile pre-load, the specimens welded during the application of increasing tensile load show solidification cracks. In the weld seams, a characteristic angle α between the predominantly columnar grains and the fusion line can be observed. Specimens showing solidification cracks show a significantly larger angle α compared to the crack-free specimens. Based on these observations, the characteristic angle α is proposed as a new hot cracking criterion.
We present special applications of electron backscatter diffraction (EBSD) which aim to overcome some of the limitations of this technique as it is currently applied in the scanning electron microscope. We stress that the raw EBSD signal carries additional information which is useful beyond the conventional orientation determination. The background signal underlying the backscattered Kikuchi diffraction (BKD) patterns reflects the chemical composition and surface topography but also contains channeling-in information which is used for qualitative real-time orientation imaging using various backscattered electron signals. A significantly improved orientation precision can be achieved when dynamically simulated pattern are matched to the experimental BKD patterns. The breaking of Friedel’s rule makes it possible to obtain orientation mappings with respect to the point-group symmetries. Finally, we discuss the
determination of lattice parameters from individual BKD
patterns. Subgrain structure in a single quartz grain. The increased noise level in the left map reflects the lower precision of a standard orientation determination using band detection by the Hough transform. The right map results from the same experimental raw data after orientation refinement using a pattern matching approach. The colors correspond an adapted inverse pole figure color key with a maximum angular deviation of about 2° from the mean orientation.
Nanocomposites of Ag-ZnFe2O4@reduced graphene oxide (rGO) were synthesized using a one-pot microwave-assisted self-assembly method. The morphology and structure of the Ag-ZnFe2O4@rGO nanocomposites were characterized. The nanocomposites formed with 15.2 wt% rGO showed excellent adsorption properties and high photocatalytic activity for the degradation of methylene blue (MB), rhodamine B (RhB), and methyl orange (MO). The synergistic interactions between Ag, ZnFe2O4, and rGO decreased the aggregation of the nanoparticles (NPs) and increased the surface area, resulting in better absorption in both UV and visible light. Such a structure was helpful for separating the photoexcited electron-hole pairs and accelerating electron transfer. Electrochemical impedance spectroscopy (EIS) revealed a smaller resistance in the solid-state interface layer and charge transfer on the composite surface than that of the bare ZnFe2O4 NPs and ZnFe2O4@rGO nanocomposite. The Ag-ZnFe2O4@rGO nanocomposite could be recovered easily by a magnet and reused five times with no significant decrease in photocatalytic activity. The as-prepared Ag-ZnFe2O4@rGO nanocomposite catalyst could be applied to the removal of hard-to-degrade waste materials owing to its high efficiency in both UV and visible light and its excellent reusability.
During the processing of superconducting Nb3Sn wire, several intermediate intermetallic phases including a previously encountered Cu-Nb-Sn phase show up. The yet unknown crystal structure of this phase is now identified by a combination of different experimental techniques and database search to be of the hexagonal NiMg2 type with a proposed composition of about (Nb0.75Cu0.25)Sn2. The structure determination started from an evaluation of the lattice parameters from EBSD Kikuchi patterns from quenched material suggesting hexagonal or orthorhombic symmetry. A database search then led to the hexagonal NiMg2 type structure, the presence of which was confirmed by a Rietveld analysis on the basis of high energy synchrotron X-ray powder diffraction data. Assuming a partial substitution of Nb in orthorhombic NbSn2 by Cu, the change of the valence electron concentration provokes a structural transformation from the CuMg2 type for NbSn2 to the NiMg2 type for (Nb0.75Cu0.25)Sn2. In the previous literature the (Nb0.75Cu0.25)Sn2 phase described here has occasionally been referred to as Nausite.
Micrometric surface topologies are required for a wide range of technical applications. While lowered surface features have been used for many years to improve the tribological behavior of contacting surfaces, there are also other fields of application, where the potential of elevated surface features is known, e. g. for metal forming tools. However, the demand for a high wear resistance of these structures often inhibits an industrial application. A solution is offered by structuring techniques that use additional material. A promising approach is the localized dispersing of hard ceramic particles by pulsed laser radiation, the so-called laser implantation. This paper describes the potential to adjust the geometry as well as the mechanical properties of laser implanted surfaces by means of microstructural and topological investigations. Afterwards, results of a wear test are given and different applications for this structuring technique are discussed. It can be shown that dome-shaped or ring-shaped structures on a micrometric scale can be produced with high hardness and wear resistance.
Force-distance curves have been acquired with an atomic force microscope on perfluorpolyether films. It is shown that curves acquired on films of different thickness, at different rates and with different dwell times can be overlapped by rescaling the time or distance axis.When the time or distance axis is rescaled,the force depends only on the surface tension of perfluorpolyether and on geometrical properties of thetip (aperture and perimeter of the tip at a given distance from the apex). Hence, curves acquired with thesame tip overlap.
By comparing curves acquired at different rates the dynamics of tip-wetting can be investigated. Fur-thermore, rescaled force-distance curves have been matched with the perimeter of cross sections ofthe tip, i.e. with the perimeter of the three-phase contact line. Such measurements pave the way for anon-destructive investigation of the tip shape.
The residual stress distribution of tungsten inert gas welded S235JRC+C plates was determined by means of neutron diffraction(ND). Large longitudinal residual stresses with maxima around 600 MPa were found. With these results as reference, the evaluation of residual stress with high spatial resolution GMR (giant magneto resistance) sensors was discussed. The experiments performed indicate a correlation between changes in residual stresses (ND) and the normal component of local residual magnetic stray fields (GMR). Spatial variations in the magnetic field strength perpendicular to the welds are in the order of the magnetic field of the earth.
Laser-induced periodic surface structures (LIPSS, ripples) are a universal phenomenon and can be generated on almost any material upon irradiation with linearly polarized radiation. With the availability of ultrashort laser pulses, LIPSS have gained an increasing attraction during the past decade, since these structures can be generated in a simple single-step process, which allows a surface nanostructuring for tailoring optical, mechanical, and chemical surface properties. In this study, the current state in the field of LIPSS is reviewed. Their formation mechanisms are analyzed in ultrafast time-resolved scattering, diffraction, and polarization constrained double-pulse experiments. These experiments allow us to address the question whether the LIPSS are seeded via ultrafast energy deposition mechanisms acting during the absorption of optical radiation or via self-organization after the irradiation process. Relevant control parameters of LIPSS are identified, and technological applications featuring surface functionalization in the fields of optics, fluidics, medicine, and tribology are discussed.
Semicrystalline polymers have to be described by a three phase model consisting of a mobile amorphous (MAF), a crystalline (CF), and a rigid amorphous fraction (RAF). For nanocomposites based on a semicrystalline polymer the RAF is due to both the crystallites (RAFcrystal) and the filler (RAFfiller). Polymer nanocomposite based on poly(L-lactide) and MgAl layered double hydroxide nanofiller were prepared.
Due to the low crystallization rate of PLA ist crystallization can be suppressed by a high enough cooling rate, and the RAF is due only to the nanofiller. The MAF, CF, and RAF were estimated by Temperature Modulated DSC. For the first time CF, MAF, RAFcrystal, and RAFfiller could be estimated. It was found, that RAFfiller increases linearly with the concentration of the nanofiller for this system. Furthermore, RAFcrystal is only slightly influenced by the presence of the nanofiller.
Interlaboratory comparison: optical property classification of carbon-based films by ellipsometry
(2017)
The paper addresses the “INTERLABORATORY COMPARISON: OPTICAL PROPERTY CLASSIFICATION OF CARBON-BASED FILMS BY ELLIPSOMETRY” and the following points are discussed in more detail: Established classification for mechanical properties, Complementary classification for optical properties, Ellipsometry for determination of optical constants n-k plane as material fingerprint, Samples, participants & set-ups (samples: Japan, participants: Japan, Germany, France, set-ups: Japan, Germany, USA) and Results of interlaboratory comparison: thickness, n & k.
Easy to handle and stretchable polymer optical fibres for sensor applications
Basic idea of stimulated Brillouin scattering
Brillouin threshold for PMMA-POF and PFGI-POF in comparison
Sensorial behavior of Brillouin scattering in PFGI-POF and silica SMF
Basics and classification of distributed Brillouin sensing methods
Basic idea of dynamic Brillouin sensing
Present trends to lightweight design lead to an expanding relevance of high-strength fine-grained structural steels especially in mobile crane constructions. With growing material strength, the challenge for welding fabrication increases, since high loading capacities and safety requirements have to be accomplished. The utilisation of the high strength potential often requires complex constructions associated with high restraint conditions while welding. Increased residual stresses may occur due to superimposing reaction and restraint stresses, which have to be quantified and evaluated to ensure the safety and integrity of high-strength steel constructions. Particularly, the scope of residual stresses has to be taken into account for different effects in the HAZ, notches, weld and base metal. Commonly, conservative assumptions of residual stresses lead to distinct underestimations of the load bearing capacity particularly for welded high-strength steel constructions. This study concludes results of recent works of the researchers regarding the complex interaction among heat control, material and restraint intensity on the residual stress state in welded components. These analyses are extended by further experiments. Based on the obtained major effects, an approach for a welding residual stress assessment regarding component design according to prevailing standards for crane construction, an important application for high-strength steels, is presented.
The main aim of the research was the development of a first valid database for material parameters of earth block masonry (EBM) with particular regard to statistical characteristics. A solid database is needed for the determination of the materials partial safety factor. Therefore, compressive strength tests were carried out with two types of earth blocks and two types of prefabricated earth mortar.
The evaluation has shown that the mean variation of the compressive strength was remarkably less than expected, which indicates high quality standards of the components earth block and mortar with regard to industrial production. Using the reliability method, a partial safety factor for EBM subjected to compression was determined on the basis of these test results. The findings have shown that a common calculation method for EBM based on partial safety factors following the valid masonry construction standard is feasible.
Mn0.75Ga0.25As crystallites, partially embedded on and fully embedded within a single crystalline matrix of GaAs formed during metal organic vapor phase epitaxy (MOVPE) of Mn-rich (Mn,Ga)As on (001) oriented GaAs wafers. Phase and orientation analysis of these crystallites were performed with scanning nano beam electron diffraction (SNBED). The investigation of plan-view specimens using a liquid nitrogen cooling stage enabled the phase and orientation analysis of partially embedded ferromagnetic a-phase particles. In all specimens the following two orientation relationships (O) between the a-phase particles and the GaAs matrix were determined:
O1:
[1-2.0] Mn0.75Ga0.25As || [110] GaAs and
[10.2] Mn0.75Ga0.25As || [-110] GaAs
O2:
[10.2] Mn0.75Ga0.25As || [110] GaAs and
[1-2.0] Mn0.75Ga0.25As || [-110] GaAs.
The study of cross-sectional specimens enabled the analysis of fully embedded crystallites. It could be unambiguously detected that a fully embedded crystallite has the structure of the atomically ordered monoclinic β' phase. The β' phase crystallite consists of two domains which are related in twin positions to each other. The orientation relations of the different particles are illustrated by color coded stereographic projections.
Welding is the most important joining technology. In the steel construction
industry, e.g. production of windmill sections, welding accounts for a
main part of the manufacturing costs and resource consumption. Moreover, social
issues attached to welding involve working in dangerous environments. This aspect
has unfortunately been neglected so far, in light of a predominant focus on economics
combined with a lack of suitable assessment methods. In this chapter,
exemplary welding processes are presented that reduce the environmental and
social impacts of thick metal plate welding. Social and environmental Life Cycle
Assessments for a thick metal plate joint are conducted for the purpose of
expressing and analysing the social and environmental impacts of welding.
Furthermore, it is shown that state-of-the-art technologies like Gas Metal Arc
Welding with modified spray arcs and Laser Arc-Hybrid Welding serve to increase
social and environmental performance in contrast to common technologies, and
therefore offer great potential for sustainable manufacturing.
Active antibacterial and antifouling surface coating via a facile one-step enzymatic cross-linking
(2017)
Prevention of microbial contamination of surfaces is one of the biggest challenges for biomedical applications. Establishing a stable, easily produced, highly antibacterial surface coating offers an efficient solution but remains a technical difficulty. Here, we report on a new approach to create an in situ hydrogel film-coating on glass surfaces made by enzymatic cross-linking under physiological conditions. The cross-linking is catalyzed by horseradish peroxidase (HRP)/glucose oxidase (GOD)-coupled cascade reactions in the presence of glucose and results in 3D dendritic polyglycerol (dPG) scaffolds bound to the surface of glass.
These scaffolds continuously release H2O2 as long as glucose is present in the system. The resultant polymeric coating is highly stable, bacterial-repellent, and functions under physiological conditions. Challenged with high loads of bacteria (OD540 = 1.0), this novel hydrogel and glucose-amended coating reduced the cell viability of Pseudomonas putida (Gram-negative) by 100% and Staphylococcus aureus (Gram-positive) by ≥40%, respectively. Moreover, glucose-stimulated production of H2O2 by the coating system was sufficient to kill both test bacteria (at low titers) with >99.99% Efficiency within 24 h. In the presence of glucose, this platform produces a coating with high effectiveness against bacterial adhesion and survival that can be envisioned for the applications in the glucose-associated medical/oral devices.
Effect of different sulphur-based crosslink networks on the nitrile rubber resistance to biodiesel
(2017)
Biodiesel possesses some comparable physical properties to petroleum diesel in addition to its improved environmental benefits. Nonetheless, both fuels differ greatly with respect to their chemical compositions.
Therefore, the compatibility of the materials, which are commonly employed in contact with diesel, must also be assured for biodiesel. This paper assessed the influence of sulphur-based curing systems on the resistance of nitrile rubber to soybean biodiesel. Formulations were prepared using highacrylonitrile-content nitrile rubber by employing a two-level experimental design. The amounts of two different accelerators and sulphur were varied to achieve different types of vulcanisation systems.
Thermal analyses, mechanical tests and microscopy analyses were conducted to evaluate the behaviour of the material after contact with biodiesel. The results showed that the choice of the accelerator played an important role on the resistance of the rubber to the biofuel, and crosslink density was not a key factor with respect to the resistance.
Neutron Bragg-edge imaging was applied for the visualization of a γ-Austenite to α'-martensite phase transformation. In the present study, a super martensitic
stainless steel sample was heated until complete austenitization and was subsequently cooled down to room temperature. The martensitic phase Transformation started at Ms = 190 °C. Using a monochromatic neutron beam with λ = 0.390 nm, the transmitted intensity was significantly reduced during cooling below Ms, since the emerging martensitic phase has a higher attenuation coefficient than the austenitic phase at this wavelength. The phase Transformation process was visualized by filming the transmission images from a scintillator screen with a CCD camera with a temporal resolution of 30 s and a spatial
resolution of 100 µm.
Welding is the most important joining technique and offers the advantage of customizable plate thicknesses. On the other hand, welding causes residual stresses and deformations influencing the load carrying capacity. Their consideration in the design requires simple and fast models. Though welding simulation has contributed to accurately access to these values nowadays, their application to large components remains still in a less practicable range. Nevertheless, many studies emphasized the need to make corrections in recently available simplified models. Especially the influence of residual stresses seems somewhat overestimated in many cases if comparing conventional structural steel S355 and high-strength steel S690. In the age of computer-aided design, an improved procedure to implement weld-inducted imperfections appears overdue. This will be presented in two parts. The first part illustrates the potential influence of post-welding imperfections exemplified for weak axis buckling in comparison with the general method in accordance with Eurocode 3. Residual stresses and initial crookedness were varied systematically in order to produce a scatter band of capacities. An approach to characterize the borders of these imperfections was untertaken before that. The excessive scattering of reduction factors for the load bearing capacity demonstrates the importance of these variables. Results were finally evaluated against advanced simulation models which will be further detailed in part two of this contribution.
Micrometric surface topologies are required for a wide range of technical applications.
While lowered surface features have been used for many years to improve the tribological behavior of contacting surfaces, there are also other fields of application, where the potential of elevated surface features is known, e. g. for metal forming tools. However, the demand for a high wear resistance of these structures often inhibits an industrial application. A solution is offered by structuring techniques that use additional material. A promising approach is the localized dispersing of hard ceramic particles by pulsed laser radiation, the so-called laser implantation. This paper describes the potential to adjust the geometry as well as the mechanical properties of laser implanted surfaces by means of microstructural and topological investigations. Afterwards, results of a wear test are given and different applications for this structuring technique are discussed. It can be shown that dome-shaped or ring-shaped structures on a micrometric scale can be produced with high hardness and wear resistance.
This paper describes austenitic-ferritic duplex stainless steels, SAF 2205, in the presence of hydrogen. The duplex stainless steels (DSS) properties include excellent resistance to stress corrosion cracking, high strength and good weldability. Those steels are preferably used in industries combining hydrogen and loads. Hydrogen location in addition to hydrogen binding energy with the steel's defects are of great importance for the analysis of hydrogen embrittlement model in that steel. It is known from previously published works that the susceptibility to hydrogen embrittlement will depend on the competition between reversible and irreversible traps; meaning a direct relation to the hydrogen's state and position in the steel. In this work, we examine the local hydrogen concentration, trapping and distribution by two modern and advanced techniques: thermal desorption spectrometry (TDS) and we support it by time of flight-secondary ion mass spectrometer (ToF-SIMS). In this paper, we support and give for the first time new insights and better understanding to the hydrogen embrittlement mechanism in SAF 2205. The trapping energies levels were calculated using TDS and Lee and Lee's model. This model revealed reversible in addition to irreversible trapping sites. Also the trapping controlling mechanism was found to be a combination of detrapping controlled mechanism and diffusion controlled mechanism. The use of ToF-SIMS for local imaging the distribution of hydrogen species supports the discussion of the different hydrogen traps in this type of steel. The hydrogen embrittlemet phenomenon in SAF 2205 will be discussed in details in that paper.
Residual stresses and distortions in welded I-girders for steel construction are relevant when evaluating the stability of steel beams and column members. The application of high strength steels allows smaller wall thicknesses compared to conventional steels. Therefore, the risk of buckling has to be considered carefully. Due to the lack of knowledge concerning the residual stresses present after welding in high strength steel components conservative assumptions of their level and distribution is typically applied. In this study I-girders made of steels showing strengths of 355 MPa and 690 MPa were welded with varying heat input. Due to the dimension of the I-girders and the complex geometry the accessibility for residual stress measurement using X-ray diffraction was limited. Therefore, saw cutting accompanied by strain gauge measurement has been used to produce smaller sections appropriate to apply X-ray diffraction. The stress relaxation measured by strain gauges has been added to residual stresses determined by X-ray diffraction to obtain the original stress level and distribution before sectioning. The combination of both techniques can produce robust residual stress values. From practical point of view afford for strain gauge application can be limited to a number of measuring positions solely to record the global amount of stress relaxation. X-ray diffraction can be applied after sectioning to determine the residual stresses with sufficient spatial resolution.
Estimation of heat flux parameters during static gas tungsten arc welding spot under argon shielding
(2017)
A multi-physics modelling of a static Gas Tungsten Arc Welding (GTAW) operation has been established in order to estimate the heat flux exchanged between the arc plasma and the work-piece. The heat flux was described with a Gaussian function where two parameters required to be estimated: process efficiency and radial distribution. An inverse heat transfer problem (ihtp) has been developed in the aim to estimate these parameters from experimental data. Levenberg-Marquardt algorithm was used as the regularization method in addition to an iterative process. The experiment consisted in a static spot weld with GTAW process. The weld spot was on for 5 s under Argon shielding gas, 2.4 mm pure tungsten electrode on a SS304L disc. Temperatures were measured with thermocouples and weld pool growth monitored with a high speed camera. The experimental data were used to solve the ihtp what led to values such as 0.7 for process efficiency and average radial distribution of 1.8 mm.
Polar semiconductor materials enable a variety of classic and quantum-light sources, which are optimized continuously. However, one key problem—the inherent electric crystal polarization of such materials—remains unsolved and deteriorates the radiative exciton decay rate. We suggest a sequence of reverse interfaces to compensate these polarization effects, while the polar, natural crystal growth direction is maintained. Former research approaches, like growth on less-polar crystal planes or even the stabilization of unnatural phases, never reached industrial maturity. In contrast, our concept provides a way for the development of ultrafast devices based on established growth processes for polar materials, while the electric potential landscape becomes adjustable.
Circumventing boundary effects while characterizing epoxy/copper interphases using nanoindentation
(2017)
Characterization of the size and mechanical properties of interphases is essential when designing multicomponent materials. When nanoindentation is used to investigate the size and mechanical properties of an interphase, a common challenge is that the indenter or the stress zone formed around it are often restricted by the reinforcement, making it difficult to distinguish the mechanical property variations caused by the interphase itself from those caused by the boundary effect. In this work, a testing system was developed that allows determining the indent affected zone and accounting for it in the interphase measurements of an epoxy/Cu system. Using finite element analysis, we confirmed the validity of the proposed system. Nanoindentation was used to investigate the Interphase between copper and two different epoxy systems; amine-cured and anhydride-cured. Nanoindentation results showed that a copper layer that is only 10 nm thick still exhibits a constriction effect on the indentations in its vicinity. The amine-cured epoxy did not show any sign of interphase existence using the introduced method. However,
a soft interphase with a thickness of ~1.7 μm was measured on theanhydride-cured epoxy. Furthermore, we show that the proposed system can be used to determine the interphase thickness as well as its relative mechanical properties regardless of the indentation depth.
This system can be further used for investigating other polymer/metal interphases to better understand the factors influencing them, thus helping engineer the interphase size and properties to enhance composite performance.
The reinforcement of concrete with polymer fibers provides resistance to crack formation. The orientation distribution of these fibers has a significant influence on the mechanical behavior of the material. To optimize material performance, micromechanical models that are capable of making accurate predictions of the mechanical behavior of composite materials are needed. These models must be calibrated using experimental results from microstructural characterization. For the fiber orientation distribution analysis in the present study, computed tomography (CT) data were used to evaluate the properties of a fiber-reinforced cement mortar. The results have indicated that the fibers in this material have highly anisotropic orientation characteristics and that there is a clear tendency for the polymer fibers to agglomerate during mixing and casting. The incorporation of this experimental data into micromechanical models will increase the accuracy of those models for material simulation and optimization.
The effectiveness of distinct fillers, from micro to nano-size scaled, on the fire behaviour of an epoxy resin and its carbon fibre reinforced composites was assessed by cone calorimetry. The performance was compared not only regarding the reaction to fire performance, but also in terms of thermal stability, glass transition temperature and microstructure. Regarding the fire reaction behaviour of nanofilled epoxy resin, anionic nanoclays and thermally oxidized carbon nanotubes showed the best results, in agreement with more compact chars formed on the surface of the burning polymer. For carbon fibre reinforced composite plates, the cone calorimeter results of modified resin samples did not show significant improvements on the heat release rate curves. Poorly dispersed fillers in the resin additionally caused reductions on the glass transition temperature of the composite materials.
3D imaging techniques are very fashionable nowadays, and allow enormous progress in understanding ceramic microstructure, its evolution, and its link to mechanical, thermal, and transport properties. In this feature article, we report the use of a powerful, yet not so wide-spread, set of X-ray techniques based on refraction effects. X-ray refraction allows determining internal specific surface (surface per unit volume) in a non-destructive fashion, position and orientation sensitive, and with a nanometric detectability. While the techniques are limited by the X-ray absorption of the material under investigation, we demonstrate showcases of ceramics and composite materials, where understanding of process parameter influence or simply of microstructural parameters could be achieved in a way unrivalled even by high-resolution techniques such as electron microscopy or computed tomography.
High-strength steels are favoured materials in the industry for production of safe and sustainable structures. The main technology used for joining the components of such steel is fusion welding.
Steel alloy design concepts combined with advanced processing technologies have been extensively investigated during the development of High-Strength Low-Alloy (HSLA) steels. However, very few studies have addressed the issue of how various alloy designs, even with limited microalloy addition, can influence the properties of high-strength steel welds. In high-strength steel welding practices, the challenges regarding microstructure evolution and the resulting mechanical properties variation, are of great interest. The main focus is the debate regarding the role of microalloy elements on phase transformation and weld performance. Limited Heat Affected Zone (HAZ) softening and limited austenite grain coarsening are significant design essentials, but the primary goal is to ensure excellent toughness and tensile properties in the steel weld. To achieve this purpose, microalloy elements such as Ti, Nb, or V were intentionally added to modern high-strength steels. The focus of this work was to understand the mechanical properties of HSLA steels resulting from differences in alloy design after joining by modern welding processes.
To begin, three microalloyed S690QL steels (Nb, Ti, and Ti+V addition) were investigated. Optical microscopy confirmed that similar mixtures of tempered bainite and martensite predominated the parent microstructure in the three steels, different types of coarse microalloy precipitates were also visible. These precipitates were analysed by using a thermodynamic-based software and then identified by Transmission Electron Microscopy (TEM). Results of mechanical testing revealed that all three steels performed above the standard toughness and tensile strength values, but with varied yielding phenomena. During the welding operation, each of the three steels was joined by using the same filler material. The fused weld metal was influenced by the high dilution of microalloyed elements in the base metal, this was significantly pronounced during the modified spray arc welding technique. As a result, the Nb-containing steel exhibited sufficient amounts of alloy pick-up to transition the microstructure in the weld metal from acicular ferrite to bainite as cooling rate was increased, leading to reduced toughness. This was not observed with the other two steels.
A second focus was made on the microstructure Evolution and toughness properties of the coarse and fine grained HAZ as welding parameters changed. In order to characterise the microstructure and austenite grain growth behaviour, physical simulations were conducted. The microalloy precipitates were found to be a dominant factor restricting the austenite grain coarsening. The extent of Austenite coarsening in the HAZ is closely related to the type and volume fraction of each microalloy precipitate.
Among the three steels, the Ti-containing HAZ exhibited the smallest extent of grain growth due to the sufficient amount of stable Ti-rich precipitates. Microalloy Addition also markedly influenced the subsequent phase transformation in the HAZ. The formation of intragranular acicular ferrite was promoted by Ti-rich precipitate, acting as favourable nucleation sites of ferrite. This structure enhanced the HAZ toughness owing to fine, high-angle boundaries of ferrite plates. The synergistic effect of Nb and Mo elements was beneficial to improve the HAZ toughness at fast cooling rates by promoting fine lower bainite formation. At high heat input, large upper bainite was formed which caused reduced toughness.
The final set of experimental work was concentrated on understanding the HAZ softening mechanisms that influenced variations in the tensile properties of the welded joints. The tensile failure in the softened HAZ or base material depended on the welding parameters and the type of steel being joined. In Ti-containing steel, increased heat Input extended the softened zone width, which caused a significant decrease in hardness and then resulted in failure in this area. Therefore, limited heat Input was used to shift failure position to base material. But this was not observed in the other two steels.
Hence, small differences in microalloy addition exhibited large variation in tensile properties. Among the three steels, Ti-containing welds were found to have the most pronounced softening, followed by Ti+V-containing welds and finally Nb-containing welds. This varied softening phenomenon was related to two significant processes supported by the results of additional dilatometry simulation: phase transformation and tempering behaviour. In the Ti-containing steel, the phase Transformation product ferrite was large-sized, as a consequence of initial large austenite grains. This led to the decreased corresponding hardness of the Ti-containing steel. Furthermore, lower tempering resistance in Ti-containing steel as compared to Nb-containing steel, resulted in additional softening effect in the softened HAZ. Therefore, steel alloy identification and heat Input during welding were critical, proven by the experimentation within the same S690QL steel grade.
This work emphasised the influence of microalloy elements on weld microstructure and mechanical properties in welded joints. Knowledge of this delicate balance between steel alloy design and appropriate welding parameters is critical for the end product. Thus, this work provides specific recommendations and results to ensure proper welding practice and steel design of microalloyed high-strength steels.
The kinetics of the anodic dissolution of brass (CuZn42 and CuZn21Si3P) in synthetic tap water were investigated by atomic emission spectroelectrochemistry. Elemental Cu and Zn dissolution rates were measured in situ and in real time during galvanostatic dissolution. A complete mass/charge balance for the system yielded, as a function of applied current and a function of time, the quantity of Cu in the dezincification layer and the quantity of Cu and Zn in the oxide layer. In this way, a complete kinetic characterization of the fundamental chemical processes occurring during dezincification was realized for the first time. The oxide layer was composed primarily of Cu2O as indicated by grazing incidence XRD and Raman analysis. The soluble Cu oxidation product was determined to be Cu(II) by a mass/charge balance. Zn was oxidized to soluble Zn(II) leaving behind a trivial amount of solid Zn corrosion product on the surface. The kinetic analysis depicts a two-stage dissolution process of dezincification: a first stage of a rapid growth of the dezincified layer and a second stage where the growth of dezincified layer was much slower. The Cu2O layer grows continually during the exposure.
Silica nanowires spanning 10 μm-deep trenches are fabricated from different types of silsesquioxane-based precursors by direct e-beam patterning on silicon followed by release through deep reactive ion etching. Nanowire aspect ratios as large as 150 are achieved with a critical dimension of about 50 nm and nearly rectangular cross-sections. In situ bending tests are carried out inside a scanning electron microscope, where the etch depth of 10 mm provides sufficient space for deformation. Silica NWs are indeed observed to exhibit superplastic behavior without fracture with deflections reaching the full etch depth, about two orders of magnitude larger than the nanowire thickness. A large-deformation elastic bending model is utilized for predicting the deviation from the elastic behavior. The results of forty different tests indicate a critical stress level of 0.1–0.4 GPa for the onset of plasticity. The study hints at the possibility of fabricating silica nanowires in a monolithic Fashion through direct e-beam patterning of silsesquioxane-based resins. The fabrication technology is compatible with semiconductor manufacturing and provides silica nanowires with a very good structural integrity.
Shock tube systems are non-electric explosive fuses employed in blasting and demolition applications to trigger the detonation of explosive charges. Their working principle is based on the explosive reaction of a fine powder on the tubing´s inner surface, generating a percussive wave travelling at a velocity of 2,100 m/s along the length of the tube, without destroying it. One of the key aspects of the manufacturing process of these shock tubes is the size and morphology of the explosive powder grains and their distribution on the inner wall of the tube, in order to propagate the shockwave efficiently and reliably. For the first time, synchrotron X-ray computed tomography has been used to characterize non-destructively the explosive powder grains, typically Al/HMX between 10 and 20 μm in size, in terms of morphology and 3D distribution but also to characterise the presence and location of defects within the shock tube walls.
Polymers with intrinsic microporosity (PIMs) are of great interest in the field of gas separation membranes. Already the first synthesized PIM-1 shows extraordinary permeability and selectivity. Unfortunately, PIM-1 is susceptible to physical aging and thus gradually loses its outstanding properties. In this study a polyhedral oligomeric silsesquioxane with phenethyl substituents (PhenethylPOSS) was used as a nanofiller (0–40 wt%) in the PIM-1 matrix to potentially improve the gas transport properties and prevent physical aging. The molecular mobility of the solution-cast nanocomposite films was analyzed by Broadband Dielectric Spectroscopy (BDS). Furthermore, gas permeability was determined with the time lag method (0–20 bar upstream pressure) at 35 °C for N2, O2, CH4 and CO2.
Non-isothermal heating rate kinetics was applied to two epoxy resin systems. In situ near-infrared (NIR) measurements were taken with a heatable NIR cell which allowed the cure to be monitored by characteristic absorption bands. An autocatalyzed reaction of the nth order was shown to describe the epoxy conversion curves. Differential Scanning Calorimetry (DSC) was used as a complementary method. The kinetic models developed by both NIR and DSC are in good accordance with experimental epoxy conversion in the in situ NIR setup for single and multiple cure temperature ramps.
A linear calibration curve of the characteristic absorption bands of epoxy normalized to aromatic vibrations was introduced. The curing degree of structural epoxies that were cured according to an industrial temperature cure profile was determined by NIR using the calibration curve. The epoxy conversions of the structural components showed good agreement with the experimental in situ NIR. Several degrees of cure for structural specimens were evaluated by NIR and residual reaction enthalpy by DSC. We present the non-destructive NIR spectroscopy as an alternative to determine fast and non-destructive epoxy conversion, particularly suitable for high degrees of cure on structural components.
Photoluminescence techniques are amongst the most widely used tools in the life sciences, with new and exciting applications in medical diagnostics and molecular imaging continuously emerging. Advantages include their comparative ease of use, unique sensitivity, non-invasive character, and potential for multiplexing, remote sensing, and miniaturization. General drawbacks are, however, signals, that contain unwanted wavelength- and polarization contributions from instrument-dependent effects, which are also time-dependent due to aging of instrument-components, and difficulties to measure absolute fluorescence intensities. Moreover, scattering systems require special measurement geometries and the interest in new optical reporters with emission > 1000 nm strategies for reliable measurements in the second diagnostic for the comparison of material performance and the rational design of new fluorophores with improved properties.
Here, we present strategies to versatile method-adaptable liquid and solid fluorescence standards for different fluorescence parameters including traceable instrument calibration procedures and the design of integrating sphere setups for the absolute measurement of emission spectra and quantum yields in the wavelength region of 350 to 1600 nm. Examples are multi-emitter glasses, spectral fluorescence standards, and quantum yield standards for the UV/vis/NIR
Lanthanide-doped up-converting nanoparticles (UCNPs) are promising reporters for medical diagnostics and bioimaging, which are excited in the near infrared (NIR) by multiphoton absorption processes, and show multiple narrow emission bands in the visible (vis) and NIR, long luminescence lifetimes in the μs range, and excellent photostability. Current limitations present their relative low absorption cross sections and low fluorescence efficiencies, with the latter being affected by particle size, surface chemistry, and microenvironment, particularly water.
Here, we present results from systematic studies of the excitation power density dependent upconversion luminescence spectra, intensities/intensity ratios of the individual emission bands, slope factors, and quantum yields of UCNPs of varying size, dopant concentration, and surface chemistry in different microenvironments as well as the up- and downconversion luminescence decay kinetics of the different emission bands. Moreover, first studies of the energy transfer from UCNPs to surface-bound organic dyes acting as fluorescence acceptors are shown. Based upon these measurements, fluorescence deactivation channels are identified and spectroscopic parameters for the screening of material performance are derived.
Lanthanide-doped up-converting nanoparticles (UCNPs) are promising reporters for medical diagnostics and bioimaging. Current limitations present their relative low absorption cross sections and low fluorescence efficiencies, with the latter being affected by particle size, surface chemistry, and microenvironment, particularly water.
Here, we present results from systematic studies of the excitation power density dependent upconversion luminescence spectra, intensities/intensity ratios of the individual emission bands, slope factors, and quantum yields of UCNPs of varying size, dopant concentration, and surface chemistry in different microenvironments as well as the up- and downconversion luminescence decay kinetics of the different emission bands. Moreover, first studies of the energy transfer from UCNPs to surface-bound organic dyes acting as fluorescence acceptors are shown. Based upon these measurements, fluorescence deactivation channels are identified and spectroscopic parameters for the screening of material performance are derived.
In order to study the temporally distributed energy deposition in the formation of laser-induced periodic surface structures (LIPSS) on single-crystalline zinc oxide (ZnO), two-colour double-fs-pulse experiments were performed. Parallel or cross-polarised double-pulse sequences at 400 and 800 nm wavelength were generated by a Mach–Zehnder interferometer, exhibiting inter-pulse delays up to a few picoseconds between the sub-ablation 50-fs-pulses. Twenty two-colour double-pulse sequences were collinearly focused by a spherical mirror to the sample surface. The resulting LIPSS periods and areas were analysed by scanning electron microscopy. The delay-dependence of these LIPSS characteristics shows a dissimilar behaviour when compared to the semiconductor silicon, the dielectric fused silica, or the metal titanium. A wavelength-dependent plasmonic mechanism is proposed to explain the delay-dependence of the LIPSS on ZnO when considering multi-photon excitation processes. Our results support the involvement of nonlinear processes for temporally overlapping pulses. These experiments extend previous two-colour studies on the indirect semiconductor silicon towards the direct wide band-gap semiconductor ZnO and further manifest the relevance of the ultrafast energy deposition for LIPSS formation.
Kikuchi diffraction patterns can provide fundamental information about the lattice metric of a crystalline phase. In order to improve the possible precision and accuracy of lattice parameter determination from the features observed in Kikuchi patterns, some useful fundamental relationships of geometric crystal-lography are reviewed, which hold true independently of the actual crystal symmetry. The Kikuchi band positions and intersections and the Kikuchi band widths are highly interrelated, which is illustrated by the fact that all lattice plane trace positions of the crystal are predetermined by the definition of only four traces. If, additionally, the projection centre of the gnomonic projection is known, the lattice parameter ratios and the angles between the basis vectors are fixed. A further definition of one specific Kikuchi band width is sufficient to set the absolute sizes of all lattice parameters and to predict the widths of all Kikuchi bands. The mathematical properties of the gnomonic projection turn out to be central to an improved interpretation of Kikuchi pattern data, emphasizing the importance of the exact knowledge of the projection centre.
The use of renewable energy technologies, such as photovoltaics (PV) should be sustainable and environmentally compatible and therefore protect the environment from risks and damaging impacts. Regarding the growing number of installed photovoltaic systems, the end-of-life management of the pv-modules will become increasingly important. Thin film panels contain hazardous substances that may harm the environment if they are not recycled or disposed properly after reaching the end of their service life. Heavy metals, for example, can be toxic as well as carcinogenic or teratogenic. Processing methods for the recycling of PV thin film modules have to take these facts into account. Currently the available recycling techniques usually utilise chemicals such as acids for a wet-chemical treatment of end-of-life modules. The aim of RESOLVED was to identify and test alternative methods for a wet-mechanical treatment in order to reduce the consumption of chemicals in the recycling of thin film modules. Furthermore, the recovered Cadmium-Telluride (CdTe) and Copper-Indium-Diselenide/Disulfide (CIS) should be helping to save scare resources especially for limited elements such as tellurium and indium. The project RESOLVED investigated the recovery of semiconductors material as secondary raw material and the decontamination of the residues of the PV thin film modules. These goals were achieved by testing and optimising existing technologies for the recycling process as well as for the enrichment of the semiconductor materials. The target is to re-use the enriched recovered material in the production of new PV modules. Special efforts were made to look into life cycle analysis, process sustainability, economical aspects, and resource availability.
A laser induced breakdown spectroscopy (LIBS) system was combined with the Gas Tungsten Arc (TIG) Welding process for the in situ monitoring of chemical compositions in austenitic stainless steels during welding. The purpose of this project is to develop a prototype of an online chemical composition control system for welding applications. One of the use cases of this new LIBS-based measurement system can be the controlling of potentially dangerous emissions during the welding process in order to improve the working safety conditions.
Synchrotron Radiation with its high intensity and the opportunity to tune the wavelength offers unique possibilities to investigate real catalysts, even under industry-like conditions.
A good example is a XAFS study performed at supported Ni catalysts used for the dimerization of butene at elevated temperature and pressure. Another example are investigations at titania supported Pd based catalyst elucidating the role of co-components (e.g. Sb, Co, Mn and Au) which are necessary to get the desired promising performance in the gas phase acetoxylation of toluene to benzyl acetate, an environmentally benign alternative for the conventional process using chlorine.
Furthermore, investigations about the redox properties of different Cu catalysts will be presented. It could be shown that the redox properties of Cu have a great impact on the performance of such catalysts, not only in some gas phase reactions, but also in photocatalytic applications, e.g. water splitting.
Additive Manufacturing by Selective Laser Melting (SLM) offers ample scope for producing geometrically complex parts as compared to the traditional subtractive manufacturing strategies. However, the residual stresses (RS) developed during the processing can reduce the load bearing capacity as well as induce unwanted distortion, limiting the application of SLM parts. In the present work, residual stresses in additivly manufactured IN718 part were analised by means of neutron diffraction and synchrotron X-ray diffraction.
The work aims at addressing the modelling and implementation of criteria for multiple crack propagation, including interaction and coalescence, for a more reliable fracture mechanics-based prediction of stress-life curves for weldments.
A large experimental work is presented in which micro-cracks have been made visible by heat-tinting at successive stages of fatigue life of the welded specimens. Here the correlation between the number of initiation sites and the applied stress level has been also investigated.
The criteria have been implemented in in-house software, which allows multiple fatigue crack propagation, and validated against selected experimental tests. The results have shown that the modelling of multiple crack propagation and interaction is crucial for the prediction of the fatigue strength of weldments, both in finite and infinite life regime.
The work aims at addressing the modelling and implementation of criteria for multiple crack propagation, including interaction and coalescence, for a more reliable fracture mechanics-based prediction of stress-life curves for weldments.
A large experimental work is presented in which micro-cracks have been made visible by heat-tinting at successive stages of fatigue life of the welded specimens. Here the correlation between the number of initiation sites and the applied stress level has been also investigated.
The criteria have been implemented in in-house software, which allows multiple fatigue crack propagation, and validated against selected experimental tests. The results have shown that the modelling of multiple crack propagation and interaction is crucial for the prediction of the fatigue strength of weldments, both in finite and infinite life regime.
Up to now, there exists a lack of methods for the additive manufacturing of voluminous ceramic parts with properties comparable to those of conventionally manufactured ones. A high density after sintering is needed to reach the superior properties of ceramic materials. We have developed a new additive manufacturing method, Laser-Induced Slip casting (LIS), to generate ceramic green bodies with high particle packing density and with virtually no restriction in the particle size of the feedstock, especially in terms of small particles. This is achieved by laser-induced local drying of slurries, with the process resembling many features of the well-established stereolithography, but without the excessive use of polymeric material. Thus, unlike the stereolithography process, the resulting green bodies can be processed like traditionally produced ceramic parts. This method allows large and dense additive-manufactured parts to be obtained from conventional water-based ceramic slurries. As an example, we will demonstrate the application of this novel technique with Si3N4.
An approach to develop an arc sensor for gap-width estimation during automated NG-GMAW with a weaving electrode motion is introduced by combining arc sensor readings with optical measurement of the groove shape to allow precise analyses of the process. The two test specimen welded for this study were designed to feature a variable groove geometry in order to maximize efficiency of the conducted experimental efforts, resulting in 1696 individual weaving cycle records with associated arc sensor measurements, process parameters and groove shape information. Gap width was varied from 18 to 25 mm and wire feed rates in the range of 9 to 13 m/min were used in the course of this study. Artificial neural networks were used as a modelling tool to derive an arc sensor for estimation of gap width suitable for online process control that can adapt to changes in process parameters as well as changes in the weaving motion of the electrode. Wire feed rate, weaving current, sidewall dwell currents and angles were used as inputs to calculate the gap width. Evaluation the proposed arc sensor model show very good estimation capabilities for parameters sufficiently covered during experiments.
Borosilicate glass has a wide range of technical applications due to its high chemical durability and thermal-shock resistivity. Here the effect of H2O on 16 Na2O, 10 B2O3,74 SiO2 glass is studied over a wide range of water contents from 0 to 8 wt.%. MIR spectra give evidence for the coexistence of strongly and weakly H-bonded hydrous species. Evaluation of NIR bands at 5200 cm-1 (molecular H2O), 4700 cm-1 (B-OH), and 4500 cm-1 (Si-OH) reveal that OH groups dominate up to ~6 wt.% H2O, with B-OH/Si-OH of ≈ 0.8. The incorporation of low amounts of H2O has strong impact on structure. NMR spectra of nominally dry glasses indicate a significant fraction (12 %) of 3-coordinated boron, but almost all boron is 4-coordinated after addition of 3 wt.% H2O. Raman spectra show that hydration results preferentially in transformation of Q4 to Q2 while Q3 remain unchanged, probably stabilized by bonding to BO4 tetrahedra. Viscosity measurements and differential thermal analysis give consistent results, confirming strong decrease of the glass transition temperature with addition of water from 849 K (dry) to 540 K (5 wt% H2O). An additional relaxation mechanism in hydrous glasses is inferred from dynamic mechanical analysis and is assigned to cooperative processes involving hydrous species. It is postulated that this relaxation mechanism plays an important role in crack growth kinetics.