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Eingeladener Vortrag
- nein (1)
Additive manufacturing (AM) opens the route to a range of novel applications.However, the complexity of the manufacturing process poses a challenge for the production of defect-free parts with a high reliability. Since process dynamics and resulting microstructures of AM parts are strongly influenced by the involved temperature fields, thermography is a valuable tool for process surveillance. The high process temperatures in metal AM processes allow one to use cameras usually operating in the visible spectral range to detect the thermally emitted radiation from the process. In our work, we compare the results of first measurements during the manufacturing processes of a commercial laser metal deposition (LMD) setup and a laser beam melting (LBM) setup using a MWIR camera with those from a VIS high-speed camera with band pass filter in the NIR range.
Two metal matrix composites, both consisting of a near-eutectic cast AlSi12CuMgNi alloy, one reinforced with 15%vol. Al2O3 short fibers and the other with 7%vol. Al2O3 short fibers + 15%vol. SiC particles were studied. Distribution, orientation, and volume fraction of the different phases was determined by means of synchrotron computed tomography. The load partitioning between phases was investigated by in-situ neutron diffraction compression tests. The internal damage of the eutectic Si phase and Al2O3 fibers after ex-situ compression tests was directly observed in CT reconstructed volumes. Significant debonding between Al-matrix and SiC particles was found. Those observations allowed rationalizing the load transfer among the constituent phases of two different composites. Finally, based on the Maxwell scheme, a micro-mechanical model was utilized for the composite with one and two ceramic reinforcements. The model rationalizes the experimental data, and predicts the evolution of principal stresses in each phase.
Der Einfluss der Maschinennachgiebigkeit einschließlich der elastischen Verformung des Indenters ist bei der Bestimmung der entsprechenden Werkstoffcharakteristiken insbesondere beim Einsatz von sphärischen Indentern unter höheren Prüfkräften von Bedeutung.
Mit zunehmender Prüfkraft wird die Maschinennachgiebigkeit kraftabhängig und kann im idealen Fall als Funktion von Prüfkraft und gemessener Eindringtiefe für vorgegebene Indenterradien dargestellt werden.
Angegeben ist ein vereinfachtes Verfahren zur Bestimmung der Maschinennachgiebigkeit.
P92 is one of the important steels for super heater tubes used in combustion plants. However, in fossil fuel fired environments the formation of oxides and sulfides are challenging the material. To understand early corrosion mechanisms, which are important for process prediction, high temperature in-situ ageing experiments of Fe-Cr-Mn alloys in SO2 and SO2+H2O atmosphere were performed, applying energy dispersive X-ray diffraction (EDXRD) analysis.
One of the biggest problems in high-voltage silicone rubber insulation cable accessories is the damage on electrical treeing, initiated by partial discharges. The electrical treeing starts at unavoidable imperfections inside the material or at interfaces. The damage is usually irreversible and leads around the starting points to a partial destruction of the material. To prolong the lifetime and thereby to increase the assurance of the structural component commonly, for mechanical improvement constituted filler is modified to obtain a self-healing silicone rubber. Damage mechanism is analysed to address the filler to the damage mode.
Bei der Bewertung der Verlässlichkeit der im Labor gewonnenen Prüfergebnisse spielen Ringversuche eine entscheidende Rolle. Die Bundesanstalt für Materialforschung und –prüfung (BAM) unterstützt deshalb den weiteren Ausbau des Ringversuchsprogramms des im Jahr 2007 gegründeten Kompetenzzentrums zur Qualitätssicherung für Prüfungen von Gefahrgütern und Gefahrstoffen auf physikalische Gefahren (Centre for quality assurance for testing of dangerous goods and hazardous substances, CEQAT-DGHS).
Bei allen bisher untersuchten Prüfmethoden besteht ein Verbesserungsbedarf. Die RV müssen daher zunächst auf die Methodenentwicklung, -verbesserung und -validierung und auf die Bestimmung der Messunsicherheit der jeweiligen Prüfmethode abzielen und nicht auf Leistungstests.
The interphase between the inorganic filler and the polymer matrix is considered as one of the most important characteristics of inorganic/polymer nanocomposites. The segmental dynamics of this interphase is expected to be altered as compared to the pure matrix, which might percolate into the entire system. For instance, it was found that a so-called Rigid Amorphous Phase (RAF) is formed by adsorption of segments onto the nanoparticles yielding to its immobilization. The RAF is available from the decrease of the specific heat capacity Δcp in the glass transition region of the nanocomposites. Here, precise Temperature Modulated DSC (TMDSC) was employed to study Δcp of epoxy/Boehmite nanocomposites with different nanofiller concentrations. Surprisingly, the investigated system showed an increase of Δcp with increasing filler concentration up to 10 wt%. This implies an increased fraction of mobile segments, and is in accordance with the found decreased value of the glass transition temperature Tg. Although for higher filler contents Tg further slightly decreases, Δcp decreases in contrary, indicating a formation of RAF. This behavior was discussed as a competition of mobilization effects, due to an incomplete crosslinking reaction, and the formation of RAF.
Microbiologically influenced corrosion (MIC) of iron is usually attributed to sulfate-reducing microorganisms, either chemically (formation of hydrogen sulfide) or electrically (direct electron uptake). Methanogenetic Archaea are also known to be involved in iron corrosion, forming a multi-species biofilm on corroding metallic structures. However, mechanistic details and kinetics of the overall process in methanogen-induced MIC are poorly understood.
Thin mesoporous metal oxide films are versatile and attractive candidates for several energy applications like photovoltaics, electrolysis or batteries. Due to their high surface area and ordered pore structure, mesoporous metal oxides demonstrate higher activities. The performance of the porous films is affected by properties like size and shape of the mesopores as well as the crystallinity of the framework. The exact determination and metrological evaluation of the complex morphology of thin mesoporous films requires a new analytical approach employing to combined data of different analytical methods. In this contribution we present a novel evaluation procedure for spectroscopic ellipsometry (SE) to analyse thin mesoporous iridium oxide films.
Mesoporous iridium oxide films were prepared via dip-coating of a solution containing a triblock-copolymer as structure directing agent and an iridium precursor in ethanol. Deposited films were calcined in air at temperatures between 300 and 600 °C. Their morphology was studied with SEM and an electron probe microanalysis (EPMA)and correlated via SE with a Bruggeman effective medium approximation (BEMA). The developed SE model described the film thickness as well as the porosity.
Figure 1a shows a top-view SEM image of mesoporous IrO2 film calcined at 375 °C. The image reveals that the films exhibit a well-ordered mesopore structure with an average pore diameter of 16 nm and a periodic distance between pore centres of 24 nm (FFT inset). Figure 1b is a parity plot of film thicknesses determined by cross-section SEM versus SE of IrO2 film samples prepared at different calcination temperatures. The porosity from the SE model is in good agreement to the porosity values obtained by EPMA.
The contribution will assess in detail the novel approach to analyse the morphology and porosity of thin metal oxide films with spectroscopic ellipsometry. Moreover, the advantages of the new developed approach will be discussed as well as combination of datasets from multiple measurements to development new methods for innovative energy technologies.
The EC’s recommendation for a definition of nanomaterial (2011/696/EU) should allow the identification of a particulate nanomaterial based on the number-based metric criterion according to which at least 50% of the constituent particles have the smallest dimension between 1 and 100 nm. However, it has been recently demonstrated that the implementation of this definition for regulatory purposes is conditioned by the large deviations between the results obtained by different sizing methods or due to practical reasons such as high costs and time-consuming (SEM, TEM).
Within the European project NanoDefine (www.nanodefine.eu) a two-tier approach has been developed, whereby firstly a screening method is applied for the rough classification as a nano-/non-nanomaterial, and for borderline cases a confirmatory method (imaging methods or field flow fractionation) must be considered.
One of the measurement methods well suited to particulate powder is the determination of volume-specific surface area (VSSA) by means of gas adsorption as well as skeletal density. The value of 60 m2/cm3 corresponding to spherical, monodisperse particles with a diameter of 100 nm constitutes the threshold for decisioning if the material is a nano- or non-nanomaterial. The correct identification of a nanomaterial by VSSA method is accepted by the EU recommendation.
However, the application of the VSSA method is associated also by some limitations. The threshold of 60 m2/cm3 is dependent on the particle shape, so that it changes considerably with the number of nano-dimensions of the particles. For particles containing micro-pores or having a microporous coating false positive results will be produced. Furthermore, broad particle size distributions make necessary to adjust the threshold. Based on examples of commercially available ceramic powders, the applicability of the VSSA approach will be tested (in relation with SEM and TEM measurements) in order to expand the actual knowledge and to improve this good available and agglomeration tolerant method.
The EU recommendation for a definition of nanomaterial (2011/696/EU) should allow the identification of a particulate nanomaterial based on the number-based metric criterion according to which at least 50% of the constituent particles have the smallest dimension between 1 and 100 nm. Within the European Project NanoDefine (www.nanodefine.eu) a two-tier approach has been developed, whereby firstly a screening method is applied for the rough classification as a nanomaterial or non-nanomaterial, and for borderline cases a confirmatory method (imaging methods or field flow fractionation) must be considered.
One of the measurement methods well suited to particulate powder is the determination of volume-specific surface area (VSSA) by means of gas adsorption as well as skeletal density. The value of 60 m2/cm3 corresponding to spherical, monodisperse particles with a diameter of 100 nm constitutes the threshold for decisioning if the material is a nanomaterial or non-nanomaterial. The correct identification of a nanomaterial by VSSA method (positive test) is accepted by the EU recommendation.
However, the application of the VSSA method is associated also by some limitations. The threshold of 60 m2/cm3 is dependent on the particle shape. For particles containing micro-pores or having a microporous coating, false positive results will be produced.
Furthermore, broad particle size distributions – as typically for ceramic materials – as well as multi-modal size distributions make necessary to adjust the threshold.
Based on examples of commercially available ceramic powders, the applicability of the VSSA approach will be tested (in relation with SEM and TEM measurements) in order to expand the actual knowledge and
improve the method.
The reduction of harmful emissions to the environment is one of the most urgent challenges of our time. To achieve this goal, it is inevitable to shift from using fossil fuels to renewable energy sources. Within this transition, hydrogen can play a key role serving as fuel in transportation and as means for energy storage.
The storage and transport of hydrogen using austenitic stainless steels as the infrastructure, as well as the use of these grades in hydrogen containing aggressive environments, remains problematic. The degradation of the mechanical properties and the possibility of phase transformation by ingress and accumulation of hydrogen are the main drawbacks. Advanced studies of the behaviour of hydrogen in austenite is necessary to fully understand the occurring damage processes. This knowledge is crucial for the safe use of components in industry and transportation facilities of hydrogen.
A powerful tool for depicting the distribution of hydrogen in steels, with high accuracy and resolution, is time-of-flight secondary ion mass spectrometry (ToF-SIMS). We here present a comprehensive research on the hydrogen degradation processes in AISI 304L based on electrochemical charging and subsequent ToF-SIMS experiments. To obtain furthermore information about the structural composition and cracking behaviour, electron-backscattered diffraction (EBSD) and scanning electron microscopy (SEM) were performed afterwards. All the gathered data was treated employing data fusion, thus creating a thorough portrait of hydrogen diffusion and its damaging effects in AISI 304L.
Specimens were charged with deuterium instead of hydrogen. This necessity stems from the difficulty to separate between artificially charged hydrogen and traces existing in the material or adsorbed from the rest gas in the analysis chamber. Similar diffusion and permeation behaviour, as well as solubility, allow nonetheless to draw onclusions from the experiments.
High-strength low-alloyed (HSLA) steels with yield strength ≥ 690 MPa have increasing im-portance in steel construction and civil engineering. However, weld processing of those steels is a major challenge. The susceptibility for degradation of mechanical properties of weld joints sig-nificantly increases in presence of hydrogen and can result in hydrogen assisted cracking (HAC). Generally, risk for HAC increases with increasing yield strength of HSLA steels. To min-imize the incidence of HAC, it is essential to gain knowledge about both the (1) absorbed hydro-gen amount and its distribution in the weld seam and (2) options to lower the amount of intro-duced hydrogen. Existing standards recommend heat treatment procedures (interpass tempera-ture or post weld heat treatment) to reduce the diffusible hydrogen concentration in weldments. In this context, different weld seam geometries should be considered. For HSLA steel fabrication weld processing with seam opening angles of 45° to 60° is typical. Modern weld technologies allow welding with seam opening angles of 30° - reduced welding time and costs. In the present study, the hydrogen distribution in multi-layer welds of a 960 MPa HSLA steel was analysed. Influence of different seam opening angles as well as heat input, interpass temperature and post weld heat treatments were investigated. The welded samples were quenched in ice water imme-diately after welding and subsequently stored in liquid nitrogen. After defined warming up, small specimens were machined from the weld seam by water jet cutting. The diffusible hydrogen concentration was measured by carrier gas hot extraction with coupled mass spectrometer. The results showed, that low heat input and post weld heat treatment procedures can lower hydrogen concentrations in welds. Furthermore, a gradient of the hydrogen concentration was identified with increasing weld pool depth. By varying the seam opening angles different hydrogen concen-trations were measured.
Ferritic alloys containing Cr form Cr5S6 precipitates along grain boundaries in hot SO2 environment. Grain boundary precipitates may influence the steel’s mechanical behavior. Cr5S6 precipitates were reconstructed three-dimensionally using FIB tomography analysis to determine the volume, number, and penetration depth. The volume growth of Cr5S6 precipitates increased only for the initial aging time of 3 h but became constant after 6 h. The number of precipitates increased linearly.
Phage display is used to find specific target binding peptides for polypropylene (PP) surfaces. PP is one of the most commonly used plastics in the world. Millions of tons are produced every year. PP binders are of particular interest because so far gluing or printing on PP is challenging due to its low surface energy. A phage display protocol for PP was developed followed by Next Generation DNA Sequencing of the whole phage library. Data analysis of millions of sequences yields promising peptide candidates which were synthesized as PEG conjugates. Fluorescence-based adsorption-elution-experiments show high adsorption on PP for several sequences.
Initial situation:
Aluminum is an often-used building material in modern architecture, not only for construction but as well for facades and decorative elements. In the 1950th and 1960th, after World War II, many buildings in Germany were constructed with aluminum or contain elements of colored anodized aluminum. In the last years a larger number of these buildings are increasingly in the sight of conservation works including the aluminum parts such as window frames or facade coverings.
Damaged Aluminum Surfaces:
Common damages are a change of color or gloss changes through weathering processes, drill holes or marks due to later modifications, scratches in the anodized layer due to extensive wear e.g. at handrails or door handles.
To repair damaged aluminum surfaces, there are usually two options: smaller damaged areas are repaired by using a touch-up pen. In case of larger damages, the complete re-anodization is necessary. This includes to de-anodize the surface with cleaning and grinding the whole aluminum object. Both possibilities are disadvantageous for the objects. The touch-up pen often does not match the color of the original surface together with an insufficient corrosion protection for outdoors. While the newly anodized surface differs in color and gloss from the originally applied color.
Research Approach:
The whole procedure contrasts with the principal approach in conservation which aims to intervene as less as possible, in case of the conservation of an object. To fulfill this approach in a more appropriate way the research project focuses on a mobile and partial application for colored, anodized aluminum parts.
To anodize aluminum the application of an electrolyte onto the surface together with sufficient voltage and current is necessary. Generally diluted sulfuric acid is used as electrolyte. Different possibilities are examined to enable the mobile application of the electrolyte, e. g. the application by producing a gel matrix or like in electroplating by pen or brush wrapped with a fleece fabric.
Experimental part:
First experiments are conducted to examine the structure of the anodized layer in relation with proper cleaning, anodization time with applied voltage and current and the coloring process. The aim was to reduce the preparation procedure and the anodization time as much as possible to facilitate the mobile application.
Examinations with Keyence microscope, Eddy current testing and REM are performed to characterize the layers. The results are shown in table 1. A clear connection between proper cleaning, anodization time, voltage and amperage and the achieved thickness of the anodized layer is significant. Cracks in the layer show that raising the voltage and amperage results in thicker layers but as well in a crumbled and less stable anodized surface.
Gel preparation:
In addition to the anodization process with a liquid e.g. sulfuric acid a gel application is tested to prevent the electrolyte from rinsing down during the mobile application. For this purpose, several gel-forming agents are tested together with their stability in acid systems. It was observed, that the consistency of the gels varies dependent of the time.
Conductivity:
The conductivity of sulfuric acid combined with different gel-systems was measured and compared in order to predict the possible growth of layers during anodic oxidation process.
Further steps:
Determination and optimization of application parameters like voltage, amperage and anodization-time to build up a preferably stable and sufficient thick anodized layer. Examination of gel preparation to guarantee a stable product, enforcing with textile tape for easy application.
Electrochemical study of polyaniline/silicon dioxide containing coatings in geothermal solution
(2018)
Polyaniline/Silicon Dioxide containing coatings were electrochemically investigated in a saline geothermal solution.
With the increase of exposure time, impedance values of coated specimens decreased at low frequency, which could be caused by the decrease of pore resistance due to electrolyte or water uptake.
Coating system needs further optimization work.
In-situ SAXS techniques
(2018)
This project studies the orientation of nanoparticles under the influence of external stimuli such as electric fields, magnetic fields and ultra-sonic vibrations. A set of functional sample holders that fit inside the sample chamber of a state-of-the-art Small Angle X-ray Scattering (SAXS) machine, called the “Multi-scale Analyzer for Ultrafine Structures” (MAUS).
The MAUS has been custom engineered to serve as a miniaturized Synchrotron, thus enabling standard material to be characterized to a high standard. Our work is needed to detail the fine characterization of reference nano-particles, not only on the nano-scale, but also coupled with external agents.
A second aim of this project is to verify a few proof-of-concept designs for the alignment of nano-particles. Where the alignment of nano-particles In-Situ is intended to further develop 3D printing technologies, and SAXS is an ideal choice to study the alignment of an oriented ensemble.
For more information about the MAUS;
https://www.bam.de/Content/DE/Pressemitteilungen/2018/AnalyticalSciences/2018-01-31-mit-maus-an-die-spitze-der-nano-forschung.html
The utilization of silver nanoparticles in consumer related products has significantly increased over the last decade, especially due to their antimicrobial properties. Today they are used in a high variety of products ranging from food containers over children toys and textiles. Therefore, research on the toxicological potential of silver nanoparticles becomes increasingly important for a high amount of studies. Unfortunately, the results of these studies are extremely diverse and do not lead to a consistent evaluation. The central problem lies in the use of a wide range of silver nanoparticles, which show a broad size distribution. To overcome this problem we report on the synthesis and application of small silver nanoparticles with a narrow size distribution (R = 3.1 nm, σ = 0.6 nm). The poly(acrylic acid) stabilized particles are thoroughly characterized by small-angle X-ray scattering, dynamic light scattering and UV/Vis spectroscopy. The particles are highly stable and show no aggregation for more than six months. It is foreseen to use these thoroughly characterized nanoparticles as reference material to compare the catalytic and biological properties of functionalized silver nanoparticles. As a first step the particles are used in the first world-wide inter-laboratory comparison of SAXS. Furthermore, the stabilizing ligand PAA can be easily exchanged by biomolecules to modify the surface functionality. Replacements of PAA with glutathione (GSH) and bovine serum albumin (BSA) have been performed as examples. With this flexible system first applications regarding biological application in an artificial digestion procedure have been performed. Thereby the changes in size distribution and aggregation state were monitored by SAXS. Additionally these particles show a high catalytic activity of (436 ± 24) L g-1 s-1 in the reduction of 4- nitrophenol to 4-aminophenol. This activity is two orders of magnitude higher than for other silver particles in the literature.
Ever since increasing a reaction’s yield while shortening the reaction time is the main objective in synthesis optimization. Microwave reactors meet these demands. In literature however their usage is under discussion due to claims of the existence of non-thermal effects resulting from the microwave radiation. Especially for nano-reference-material syntheses it is of crucial importance to be aware of influences on the reaction pathway. Therefore, we compare ultra-small silver nanoparticles with mean radii of 3 nm, synthesized via conventional and microwave heating.
We employed a versatile one-pot polyol synthesis of poly(acrylic acid) (PAA) stabilized silver nanoparticles, which display superior catalytic properties. No microwave specific effects in terms of particle size distribution characteristics, as derived by small-angle X-ray scattering (SAXS) and dynamic light scattering (DLS), are revealed. Due to the microwave reactor’s characteristics of a closed system, syntheses can be carried out at temperatures beyond the solvent’s boiling point. Particle formation was accelerated by a factor of 30 by increasing the reaction temperature from 200 °C to 250 °C. The particle growth process follows a cluster coalescence mechanism.
A post-synthetic incubation step at 250 °C induces a further growth of the particles while the size distribution broadens. Thus, utilization of microwave reactors enables an enormous decrease of the reaction time as well as the opportunity of tuning the particles’ size. Possibly, decomposition of the stabilizing ligand at elevated temperatures results in reduced yields. A temperature of 250 °C and a corresponding reaction time of 30 s represent a compromise between short reaction times and high yields.
Safety experts, carriers or traders must be able to rely on the validity of the method and on correct results of safety tests and assessments in the laboratory.
Bundesanstalt für Materialforschung und –prüfung (BAM), Berlin and Physikalisch-Technischen Bundesanstalt (PTB), Braunschweig have extensive experience in the field of testing and assessment of physical hazards of chemicals.
Interlaboratory tests on different test methods have been performed by BAM and PTB during the last 10 years. Significant differences between the results of the participating laboratories were observed in all interlaboratory test. The deviations of the test results were not caused only by laboratory faults but also by deficiencies of the test method; i.e. many of the method descriptions are too ambiguous and allow divergences for interpretation.
Therefore, it is necessary to know exactly how good the method is that is used to classify dangerous goods or hazardous substances or to determine safety-relevant parameters. A key criterion is the measurement uncertainty.
One can choose simple methods with large error limits, but the measurement uncertainties should be known and always communicated together with the test results. This would allow safety specialists to be able to assess test results correctly and make well-founded decisions, e.g. for adequate protective measures.
Interlaboratory tests play a decisive role in assessing the reliability of test results. Participation in interlaboratory tests is not only a crucial element of the quality assurance of laboratories; as such it is explicitly recommended in DIN EN ISO/IEC 17025. In addition, interlaboratory tests are also used to develop and validate test methods and can be used for the determination of the measurement uncertainty.
Therefore, the BAM and PTB continue to support the further development of the interlaboratory test programme of CEQAT-DGHS (Centre for quality assurance for testing of dangerous goods and hazardous substances, www.ceqat-dghs.bam.de), established in 2007. This programme is run by BAM in collaboration with the PTB and the QuoData Gesellschaft für Qualitätsmanagement und Statistik mbH, Dresden.
A new interlaboratory test for methods validation on the test method UN Test N.5 "Test method for substances which in contact with water emit flammable gases” is currently being prepared and will be carried out in 2018. Laboratories that specialise in this test are invited to participate in the interlaboratory test. Interested laboratories can check the details and register to participate in the interlaboratory test at the CEQAT-DGHS website.
UCST-type thermoresponsive polymers (i.e. that phase separate from solution upon cooling) present a tremendous potential not only in aqueous media with applications in the field of drug delivery, diagnostic and microfluidic applications, but also in water/alcohol mixtures, where they can be used for instance in sensing systems for alcohol-soluble drugs. However, only a few thermoresponsive polymers have been reported that present an UCST in a relevant temperature range and “green” solvents such as water or ethanol.
In this context, acrylamide-based monomers can be very useful building blocks for designing novel non-ionic UCST-type polymers because of their hydrophilic nature (with the appropriate side chain) and propensity to form hydrogen bonds. We will present our latest results on the UCST-type thermoresponsive behaviour of acrylamide- and/or 2,6-diaminopyridine-based homopolymers and copolymers in water or water/alcohol mixtures, and give some insights about the rational design of UCST polymers relying on H-bonding.
Les aubes de turbines à gaz utilisées en particulier pour les turboréacteurs de l’aéronautique sont élaborées par fonderie en superalliage monocristallin à base de nickel. Le procédé de fonderie, ainsi que les traitements thermique d’homogénéisation réalisés à très haute température, induisent la présence de pores au sein des pièces qui affectent les propriétés mécaniques et la durée de vie des aubes. Afin de réduire cette porosité les motoristes effectuent un traitement de compression isostatique à chaud (CIC) au cours duquel la porosité diminue par fermeture des pores. Afin de mieux comprendre les mécanismes impliqués au cours du traitement de CIC, nous avons lancé un programme de recherche dans le cadre du projet ERA-Net MICROPORE. La modélisation par champ de phase des mécanismes en jeu est présentée au cours de ce colloque. Nous présentons dans cette affiche un des volets de la caractérisation expérimentale du projet.
Des échantillons de superalliage CMSX4 sont observés après traitement de mise en solution et CIC sous 103 MPa à 1288°C pour différentes durées. Les pores présents sont caractérisés par microscopie électronique à balayage (MEB) afin de suivre l’évolution du taux de porosité au cours du traitement. Une caractérisation plus détaillée de pores partiellement refermés est menée par MEB et grâce à la diffraction des électrons rétrodiffusés (EBSD). Une vision tridimensionnelle de ces défauts est obtenue par des coupes métallographiques effectuées par découpe ionique (FIB).
Le projet ERA – Net MICROPORE est financé en Allemagne par la DFG (projects EP 136/1-1 and FE933/2-1) et en France par l’ANR (projects ANR15-MERA-000-03 and ANR15-MERA-0003-04).
Colloidal semiconductor nanoparticles with a spherical core and an elongated shell form bright emitters with a high absorption cross section. They show great potential for a multitude of optoelectronic applications such as LEDs or photovoltaic cells and can be used as gain material or as markers for bio imaging. For most of these applications high fluorescence quantum yields are a figure of merit for the emitter quality. In this work we investigate how the ensemble quantum yield is affected by the properties of the individual particles. In particular, we prove the role of non-emitting particles as well as the role of blinking. Using a combination of AFM and spatially resolved photoluminescence spectroscopy we measured hundreds of individual CdSe/CdS dot/rod particles of different shell lengths exciting with two different excitation wavelengths for shell or core excitation, respectively.
Ferritic-martensitic high temperature alloys are widely used as boiler tube and heat exchanger materials in combustion based power plants. All technologies have in common that the applied materials are exposed to different temperatures, process pressures and reactive atmospheres which lead to a change of the material properties and a further degradation of the material.
To date corrosion analytics mainly proceeds via the use of various microscopic techniques and the analysis of the corrosion products after the reaction is completed. Comprehensive efforts have been made to study high temperature corrosion by the use of environmental SEM’s or in-situ TEM technologies. The here presented work will show a different approach to study high temperature gas corrosion in a multiple gas atmosphere by energy dispersive X-ray diffraction (EDXRD). For this technique high energetic white X-ray radiation (10-100 keV) was used as radiation source instead of conventional monochromatic radiation. It enables us to study crystallization procedures on short and medium time scales (1 min < t < 24 h) and the collection of Bragg-Signals of the phases of interest as a function of process time. Their occurrence can directly be correlated with thermodynamic and kinetic parameters. A special designed corrosion reactor was used to combine high temperature gas corrosion experiments with the collection of diffraction patter. The crystallization and reaction paths for oxide and sulfide formation was followed in-situ on Fe-Cr and Fe-Cr-Mn model alloys in a hot SO2 containing (T=650 °C) atmosphere.
Influence of deposition hatch length on residual stress in selective laser melted Inconel 718
(2018)
The present study aims to evaluate the bulk residual stresses in SLM parts by using neutron diffraction measurements performed at E3 line -BER II neutron reactor- of Helmholtz-Zentrum für Materialien und Energie (HZB) Berlin. Together with microstructure characterization and distortion measurements, it is possible to describe the stress state throughout the whole sample. The sample was measured in as-build condition (on a build plate) and after releasing from the build plate. The used material is the nickel based superalloy 718. This alloy is widely used in aerospace and chemical industries due to its superior corrosion and heat resistant properties.
Obtained results indicated different residual stress states for each of the transversal, longitudinal and normal component. The normal and transversal component exhibits a rather compressive behavior while the longitudinal was tensile in the center part of the sample and became compressive towards the tip. As expected, the absolute values of all stress components decreased after releasing the sample from the building plate. A surface scan utilizing a coordinate-measuring machine (CMM) allowed us to present top surface distortion before and after releasing. The top surface showed a distortion around ±80µm after releasing. Microstructure evolution in the scanning-building cross-section is largely dominated by columnar grains. In addition, many small random orientated grains are prominent in the regions of a laser overlap during SLM.
In summary, for the sample of superalloy 718 manufactured by SLM, a small distortion occurred when removing the sample from the build plate whereby the residual stress state decreases. Moreover, the observed columnar grains in the building direction could give a reason for the lowest stress values in that normal direction. However, the most important parameter controlling the residual stresses is the temperature gradient. Hence, future investigations are planned for a different scan strategy to distribute the laser impact in a more homogenous manner.
Ellipsometry is well known as a highly sensitive and reproducible surface analysis technique. However, in a context of metrological applications, the most important property of a measurement process is accuracy, relying on statistical precision, (reproducibility) and trueness (in an absolute sense versus a given standard). The latter is much more difficult to achieve. In this presentation, we discuss the possibility of establishing ellipsometry in a diverse metrological landscape by means of defining standard procedures and best practice methodologies for the measurement and for calibration purposes. The most important task of this approach is to determine the model-inherent uncertainty, originating from parameter coupling. We achieve this by means of sensitivity analysis of the parameters resulting from the fit process. We discuss the definition of reference materials by which accuracy can be made available for ellipsometry, passed along between ellipsometry laboratories and for other measurement techniques. The determination of uncertainty is presented in this work for a number of examples involving difficult analysis models employed for samples from different production environments. We present a standardization initiative with the goal to disseminate this work into an international standard alongside an inter-laboratory study comparing the results for complex samples gained by laboratories with different instrumentation. We also present the results gained within EURAMET projects focused on the metrology of materials with strong non-idealities used in photovoltaics and other energy technology.
Die Probenpräparation ist ein Teil im Prozess der Baustoffuntersuchung und muss dementsprechend sorgfältig geplant werden. Die Probenpräparation ist letztendlich der Grundstein für alle folgenden Untersuchungen, somit wirken sich alle hier getroffenen Entscheidungen direkt auf die Qualität der Ergebnisse aus.
Im Gegensatz zur Druckfestigkeit weisen zementgebundene Werkstoffe i. a. nur geringe Zugfestigkeiten auf. Ein Weg, Zugfestigkeiten zementgebundener Werkstoffe zu erhöhen und Rissbildung aufgrund von Zugspannungen zu verringern, besteht in der Einarbeitung von Fasern, die diese Spannungen aufnehmen. Häufig eingesetzt werden Stahlfasern, obwohl synthetische Polymerfasern leichter und meist beständiger gegenüber chemischen Angriffen und Korrosion sind. Die Polymerfasern zeigen allerdings meist einen deutlich schwächeren Haftverbund, was an der hydrophoben Faseroberfläche liegt. Um nun eine Anbindung der Fasern an die mineralische Matrix zu erreichen, müssen die Faseroberflächen modifiziert werden, ohne dass die mechanischen Eigenschaften negativ beeinflusst werden. Eine Herausforderung besteht somit in einer Oberflächenmodifikation durch eine schonende Behandlung der Fasern zur Erzeugung von anbindungsfähigen Gruppen.
Durch eine Behandlung von modifizierten Fasern mit geeigneten Polymerlösungen werden die Oberflächeneigenschaften verändert und erlauben eine Anbindung an die Zementsteinmatrix. Der Einsatz von Tensiden als grenzflächenaktive Verbindungen ermöglicht in diesem Zusammenhang eine Vermittlung zwischen Polymeroberflächen und mineralischen Werkstoffen.
As the well-known damage mechanisms slow crack growth (SCG) and environmental stress cracking (ESC) are the major causes for possible failure of polyolefin-based materials, especially for PE-HD, they are highly relevant and need to be considered thoroughly. Furthermore, due to slight but perceptible differences in damaging effect, a differentiation between SCG and ESC is expedient. SCG appears in “inert” or “neutral” media without a decisive influence of the surrounding medium whereas ESC occurs in “active” media, which influence the failure behavior and time to failure crucially.
To characterize the inherent resistance of the material against those damage mechanisms, the well-established Full-Notch Creep Test (FNCT) is used. In this study, the FNCT – usually applied according to ISO 16770 [3] using a few universal model liquid media and mainly for pipe materials – is extended by investigations with appropriate parameters of selected relevant PE-HD container materials also in real media, such as the topical fuels diesel and biodiesel. The investigations were performed using a novel FNCT-device with 12 individual sub-stations, each equipped with individual electronic stress and temperature control and continuous online monitoring of the specimen elongation.
Especially, mechanical stress and temperature were varied systematically during FNCT and time to failure values, time-dependent elongation data as well as detailed fracture surface analysis by laser scanning microscopy (LSM) were combined for the first time (Fig. 1). Particularly, the fracture surface analysis provides a sound basis to characterize failure behavior, mainly regarding the balance between brittle crack propagation and ductile deformation. Therefore, fracture surface analysis is an essential tool for a decent assessment of SCG and ESC by FNCT measurements.
The copper alloyed stainless steel 1.4542 (X5CrNiCuNb16-4) is used in different areas due to its good mechanical properties and corrosion resistance. Strength and corrosion resistance can be adjusted by the heat treatment, which is of importance for the application of this alloy. The mechanical properties (strength and hardness) are attributed to the dispersive precipitation of the copper rich ε–Phase. The additional precipitation of chromi-um carbides can reduce the corrosion resistance. Different ageing states were produced to investigate the precipitation behaviour with various methods. Furthermore, the influence of cold-rolling on the precipitation behaviour was studied in comparison to a solution annealed state without deformation. The microstructure was studied by SEM and the variations of hardness and magnetic proportion were characterised. The electrochemical potentiodynamic reactivation (EPR) was used to determine the corrosion resistance and detect chromium depletion in all heat-treated states. The results show that a work hard-ening accelerates the precipitation rate, while ageing at 600 °C reduces the corrosion resistance due to chromium depletion.
Hyperbranched polyamine ester (HPAE)/ kaolinite nanocomposites were papered via an ex situ (solution-based) method. The kaolinite has been modified by dodecylamine (DCA). SAXS measurements revealed that the Ka interlayer space increased from 0.71 to 3.6 nm-1. A partly exfoliated structure of the HPA/Ka-DCA nanocomposites was proved by SAXS and TEM. By a combination of BDS and SHS, the relaxation properties of the nanocomposites were investigated in dependence on frequency and temperature. The activation energies of γ-relaxation for the nanocomposites were lower than the values found for the pure HPAE. The segmental dynamics (α- relaxation) was found to be screened out by the conductivity contribution. While it is retrieved by SHS employing AC-chip calorimetry. A systematic change of the dynamic glass transition estimated by AC-chip calorimetry was observed, which is in agreement with a behavior expected for a confined sample. The confinement effect of the Ka-DCA nanofillers reduces the glass transition temperature Tg and enhances, meanwhile, the electrical conductivity of the polymer. By comparing the temperature dependence of the dynamic glass transition measured with SHS and that of the dc conductivity measured by dielectric spectroscopy, a decoupling in their temperature dependencies was found.
With increasing concentration of the nanofiller, which results in a stronger glass-formation behavior, this decoupling becomes weaker.
Hybrid materials have attracted growing interest during the last decade, particularly due to their extraordinary properties. Cycloalyphatic-epoxy oligosiloxane (CEO) resin was shown to be a good candidate as a barrier material for the encapsulation purposes. Incorporation of inorganic nanoparticles such as Boehmite (BA) into polymers was observed to modify their specific characteristics, in particular, thermal, thermo-oxidative and barrier ones. In this work, novel BA-embedded organic inorganic hybrid nanocomposite material was engineered by combining the advantageous properties of hybrid polymers and nanoparticle enhancement effect. Impacts of particles on the photocuring kinetics, degree of crosslinking and the resultant changes in the thermal properties of the cured films were investigated. CEO synthesis via condensation reaction was confirmed by 1H and 29Si NMR. The particle distribution within the films was verified by SEM including transmission mode coupled with EDX elemental analysis. Photocuring kinetics and thermal properties of the films were studied by in situ FTIR spectroscopy and DSC with TGA, respectively.
The layer-by-layer Additive Manufacturing (AM) by means of Selective Laser Melting (SLM) offers many prospects regarding the design of a part used in aeroplane components and gas turbines. However, structural deviations from the nominal morphology are unavoidable. The cooling of the finished part leads to shrinkage and a high surface roughness is induced by attached powder particles affecting the part volume too.
The integrity and load-bearing capacity of a SLM produced lattice structure (see Fig.1) has been investigated by means of in-situ X-ray computed tomography during compression. The lattice structure was compressed by 10 % in height with an applied maximum force of 5 kN. Additionally, a single strut has been investigated ex-situ as a component of the lattice structure. With the higher resolution achieved on the single strut, the pore distribution (size and location) as well as the surface roughness were assessed. One of the main results coming from the in-situ analysis was that the nodes were identified as the weakest points in the lattice structure.
Collective Orientational Order and Phase Behavior of a Discotic Liquid Crystal under Confinement
(2018)
Discotic liquid crystals (DLCs) are a promising class of soft matter for electronic applications. This is due to their ability to self-organize into columns in a hexagonal columnar mesophase, driven by the overlapping of the π orbitals of their aromatic cores. This leads to a high charge-carrier mobility along the column axis. Previous studies on DLCs showed that their properties, such as phase transition temperatures and enthalpies, are susceptible to nanoconfinement. In this study, 2,3,6,7,10,11 hexakis[hexyloxy] triphenylene (HAT6) was confined into parallel aligned cylindrical nanopores of anodic aluminum oxide (AAO) membranes by melt infiltration. Furthermore, the pore surfaces of a series of membranes were chemically modified, resulting in a more hydrophobic pore surface than the unmodified ones. Collective orientational order and phase behavior of HAT6 confined into modified and unmodified nanopores of AAO were investigated by broadband dielectric spectroscopy and differential scanning calorimetry respectively.
In recent years, substantial efforts have been devoted to investigating nanoscopic confinement of polymers, and its effect on glassy dynamics. Broadband Dielectric Spectroscopy (BDS) was used to study the dynamics of ultra-thin films of PVME/PS 50/50 wt% blend, employing a novel nano-structured capacitor sample arrangement. The investigated system shows a complex dynamic behavior. First, an α-relaxation, related to a bulk-like layer was found. Second, an α’-relaxation was observed, characteristic for dynamically asymmetric blends, where the out of equilibrium dynamics is attributed to weakly-cooperative PVME segments relaxing within a frozen environment of PS segments. Thirdly, for thinnest films, an Arrhenius-like process was dominant in the dielectric spectra, indicating localized fluctuations of the segments. Relaxation rates of this process resembled that of the degenerated α-relaxation of the adsorbed layer, found for pure PVME, thus it was assigned accordingly. For thinnest films, this process undergoes a further confinement, due to the topological constraints, introduced by PS. Such multiple confinement effect has not been reported for ultra-thin films of polymer blends, before this study.
The polymer matrix region near a filler surface, termed as the interface, witnessed increasing interest, due to its possible influence on the macroscopic properties of the nanocomposite. The interphase is expecting to have different segmental dynamic, as compared to the pure matrix, which can percolate into the entire system. Here, the segmental dynamics of epoxy/Boehmite nanocomposite was studied by Broadband Dielectric Spectroscopy. It was found that an artificial relaxation process is present in the nanocomposite, on the contrary to the pure epoxy system. It was assigned to constrained fluctuations of polymer chains in the interfacial region, due to the nanofiller. However, the overall dynamic Tg of the system decreased with increasing filler concentration, indicating higher segmental mobility. This was in accordance with Temperature Modulated DSC investigations of specific heat capacity of the system, which was found to increase with increasing filler concentration, up to 10 wt%, indicating increasing mobility of the polymer matrix segments. Surprisingly, for the highest filler content, the heat capacity decreases, implying a formation of an immobilized rigid amorphous phase in the interfacial region.
In well-annealed thin polymer films, with non-repulsive polymer/substrate interactions, an irreversibly adsorbed layer is expected to form. These adsorbed layers have shown great potential for technological applications. However, their growth kinetics and molecular dynamics are still not fully understood. This is partially due to the hard accessibility of these layers in thin films. Here, the irreversibly adsorbed layers of homopolymer thin films are revealed by solvent-leaching experiments. First, the growth kinetics of these layers is investigated as a function of annealing times and original film thickness. The thickness, topography and quality of the adsorbed layer is controlled with Atomic Force Microscopy (AFM). Secondly, the molecular mobility of the adsorbed layer is investigated with Broadband Dielectric Spectroscopy (BDS). A recently developed nanostructured capacitor is employed to measure the adsorbed layers with a free surface layer. The results are quantitatively compared and discussed with respect to recently published work.
Optimization of laser treatment parameters of Inconel 686 overlay weld on carbon steel 13Mo4-5
(2017)
The work presents the effects of the change of the laser cladding parameters on microstructure, chemical composition and mechanical properties of Inconel 686 overlays (coatings). To obtain the best quality of these coatings the various parameters of laser cladding such as the power density of the laser beam, the laser beam velocity and overlapping ratio of the weld tracks were applied. The substrates were boilers plate made of the 13Mo4-5 steel. Ni - base alloys characterize by the excellent high-temperature corrosion resistance, good strength and good ability to work in aggressive environments. Applied overlays had a proper combination of the metal substrate in particular small amount of Fe. This could be achieved by the reduction of the substrate melting and its dissolution into the overlays. The microstructure, chemical composition of the obtained overlays were investigated by means of a light microscope, a scanning electron microscope (SEM) equipped with the EDS detector. The overlays had cellular-dendritic structure. The variations of the chemical composition (especially Mo, Ni and W ) in the interdendritic and dendritic regions were observed. The interdendritic regions were enriched during solidifications in Mo and W and had lower content of Ni.
Compact nuclear magnetic resonance (NMR) instruments make NMR spectroscopy and relaxometry accessible in industrial and harsh environments for reaction characterization and process control. Robust field integration of NMR systems have to face explosion protection or integration into process control systems with short set-up times. This paves the way for industrial automation in real process environments.
The design of failsafe, temperature and pressure resistant flow through cells along with their NMR-specific requirements is an essential cornerstone to enter industrial production plants and fulfill explosion safety requirements. Additionally, if fast reactions are monitored, suitable mixing devices need to be placed in close vicinity to the measuring volume to mix the reactants properly.
NMR-specific requirements aim at full quantitative pre-magnetization and acquisition with maximum sensitivity while reducing sample transfer times and dwell-times. All parameters are individually dependent on the applied NMR instrument.
Luckily, an increasing number of applications are reported together with an increasing variety of commercial equipment. However, these contributions have to be reviewed thoroughly.
The performance of sample flow cells commonly used in online analytics and especially for low-field NMR spectroscopy was experimentally and theoretically investigated by 1H-NMR experiments and numerical simulations. Especially, the applicability of 3D printed zirconium dioxide for innovative flow cell designs was of interest. Here, we demonstrate and discuss an automated test method to determine the critical parameters of flow through cells for quantitative online NMR spectroscopy. The setup is based on randomized setpoints of flow rates in order to reduce temperature related effects. Five flow cells and tubing were assessed and compared for high-field as well as low-field NMR spectrometers.
An understanding on crystallization behavior and kinetics in glasses is one of the important topics in the glass science and technology. Tsukada et al.1) found an extremely unique and curious phenomenon in the crystallization of multiferroic (ferroelectric and ferroelastic properties) ’-Gd2(MoO4)3 crystals in Gd2O3-MoO3-B2O3 glasses. That is, crystals formed in the crystallization break into small pieces with a triangle prism or pyramidal shape having a length of 50-150 um spontaneously during the crystallization in the inside of an electric furnace, not during the cooling in air after the crystallization. They proposed to call this phenomenon “self-powdering phenomenon”. To the best of our knowledge, such a self-powdering phenomenon has not been observed in the crystallization of any other glasses. To investigate this phenomenon is very important for the glass science and for the preparation of bulk crystallized glasses with ferroelastic crystals. In this work, the preparation of crystallized glasses keeping the original shape is challenged, and the mechanism of self-powdering phenomenon is proposed. Glasses with the compositions of 21Gd2O3-63MoO3-(16-x)B2O3-xTeO2 (mol%) (x=0, 2, 4, 8) such as 21Gd2O3-63MoO3-16B2O3 (GM16B) and 21Gd2O3-63MoO3-8B2O3-8TeO2 (GM8T8B) were prepared using a conventional melt quenching technique. The quenched glasses were heat-treated at some temperatures, and the crystalline phase present in the crystallized samples was identified by X-ray diffraction (XRD) analyses, and the morphology and birefringence of crystals formed were observed using a polarized optical microscope (POM). The densities of GM16B and GM8T8B glasses are 4.76 g/cm3 and 4.91 g/cam3, respectively, and these values are higher than the density of ’-Gd2(MoO4)3 crystal, 4.555 g/cm3. These differences in the density might induce the large stresses in the inside of crystals during the crystal growth. The crystallized glasses of GM16B with ’-Gd2(MoO4)3 crystals do not keep the original glass shape, showing self-powdering phenomenon (breaking into small pieces). However, the crystallized glasses of GM8T8B keep the original glass shape without indicating any self-powdering. It is proposed that the stress at the interface between the glassy phase and ’-Gd2(MoO4)3 crystalline phase might be reduced in GM8T8B glasses containing TeO2 with weak Te-O bonds.
Additive manufacturing (AM) offers an effective solution to the medical sector. It enables the production, on demand, of customised implants which match the patient’s anatomy, with grafts that promote bone growth, as well as surgical guides that help the surgeons. The objective of this project is to provide a comprehensive basis to enable the safe use of medical AM products with traceable and reliable dimensionalmeasurements. This will guarantee the reliability of medical AM products to notified bodies and facilitate acceptance of AM in the medical sector for a better quality of life.