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Thermal spraying provides a rapid method for additive deposition of various ceramics as electrical insulation in applications where polymers are not suitable. New applications in complex shaped additive manufactured metal parts are emerging for example in large scale electrical devices. Microstructural and dielectric evaluation of coatings is crucial to the employment of such free-form processes. The properties and microstructure of the plasma sprayed alumina coatings are compared with dense reference samples of the same powder produced by spark plasma sintering (SPS). To obtain dense bulk samples from the coarse alumina powder for spray coating, SPS is used.
Samples are fabricated by atmospheric plasma spraying (APS) of commercially available alumina powder (d50 = 33 µm) on copper substrates and by SPS of the same powder. Microstructure and porosity were analyzed by optical microscopy and scanning electron microscopy (SEM). Phase compositions were determined by X-ray diffraction (XRD). Dielectric properties such as DC resistance, dielectric strength, dielectric loss, and relative permittivity were determined according to the standards. The microstructure and dielectric properties of the coating and bulk material are compared to assess whether the coating is suitable for use in electrical insulation application.
Nanoforms with at least one dimension below 100 nm have an important part to play in more and more areas of our daily life. Therefore, risk assessment of these materials is becoming increasingly important. In this context, the European Chemical Agency (ECHA) considered eleven physico-chemical properties as relevant, of which the following six are essential for the registration: chemical composition, crystallinity, particle size, particle shape, surface chemistry and specific surface area. Four of these priority properties can be obtained with electron microscopy and surface analytics like XPS and ToF-SIMS. The reliability of this data must be ensured, especially for their use for grouping and read across approaches. On the other hand, the “reproducibility” crisis has revealed major shortcomings in the reliability of published data.
In a case study, we show how the quality of the data can be ensured by using existing standards and protocols of each step in the workflow of sample characterization. As exemplary samples, two Al-coated TiO2 samples as nanopowders were selected from the JRC repository, capped either with a hydrophilic or a hydrophobic organic ultrathin shell. SEM results provided the size and shape of the nanoparticles, a first overview about the composition was obtained with EDS. XPS and ToF-SIMS supplied the surface chemistry, especially information about the shell and the coating of the particles. Standards and protocols of all steps of the analytical workflow including preparation and data reduction are discussed regarding reliable and reproducible data. Additionally, uncertainties for the different steps are specified.
Only such a detailed description of all these factors allows a comprehensive physico-chemical characterization of the nanoparticles with understanding of their potential risk assessment.
The novel lab-based HAXPES spectrometer (ULVAC-PHI Quantes) gives us the possibility to measure XPS at 1486.6 eV (monochromatic Al Kα source) and HAXPES at 5414.9 eV (monochromatic Cr Kα source) on a sample at the same position. The surface analysis with this spectrometer leads to an information depth of about 10 nm for XPS and in comparison, to an analysis of deeper regions of about 30 nm for HAXPES measurements. This method provides a nondestructive way to distinguish between the near-surface region of the nanoparticles and the whole nanoparticle. Additionally, HAXPES gives access to deeper core levels at higher energy.
An application of this technique is presented using nanoparticles. The results shown were obtained with nanoparticles, that were treated differently by means of sterilization for nanosafety (i.e., before studying their toxicity it is important to establish whether nanomaterials are sterile and, if not, to be treated either via microwave or autoclave sterilisation). As a complementary method, the data is compared with SEM and EDX measurements. All methods demonstrate the influence of sterilization. More specifically, these results show that the sterilization step must be considered in the physical-chemical description of the particles for establishing reliable (quantitative structure-activity) relationships.
Iron-based catalysts are employed in CO2-FTS due to their ability to convert CO2 into CO in a first step and their selectivity towards higher hydrocarbons in a second CO hydrogenation step. According to the literature, iron carbides represent the active phase for hydrocarbon formation and are claimed to emerge in the presence of CO. We propose nanostructured FeOx films as model systems to assess information about the complex phase transformations during CO2-FTS. Mesoporous hematite, ferrihydrite, maghemite, maghemite/magnetite films were exposed to CO2-FTS atmospheres at 20 bar and 300°C. Up to three distinct phases were observed depending on the timeon-stream (TOS): a sintered maghemite/magnetite phase, a carbidic core-shell structure, and a low-crystalline, needle-type oxide phase. Our findings indicate that the formation of an intermediary maghemite/magnetite phase, predominant after short TOS (30 h), precedes the evolution of the carbide phase.
Yet, even after prolonged TOS (185 h), no full conversion into a bulk carbide is observed.
Laser Powder Bed Fusion (L-PBF) allow the fabrication of lightweight near net shape AlSi10Mg components attractive to the aerospace, automotive, biomedical and military industries. During the build-up process, high cooling rates occur. Thus, L-PBF AlSi10Mg alloys exhibit a Si-nanostructure in the as-built condition, which leads to superior mechanical properties compared to conventional cast materials. At the same time, such high thermal gradients generally involve a deleterious residual stress (RS) state that needs to be assessed during the design process, before placing a component in service. To this purpose post-process heat treatments are commonly performed to relieve detrimental RS. In this contribution two low-temperature stress-relief heat treatments (SRHT) are studied and compared with the as-built state: a SRHT at 265°C for 1 hour and a SRHT at 300°C for 2 hours. At these temperatures microstructural changes occur. In the as-built state, Si atoms are supersaturated in the α-aluminium matrix, which is enveloped by a eutectic Si-network. At 265°C the Si precipitation from the matrix to the pre-existing network is triggered. Thereafter, above 295°C the fragmentation and spheroidization of the Si branches takes place, presumably by Al–Si interdiffusion. After 2 hours the original eutectic network is completely replaced by uniformly distributed blocky particles. The effect of the heat and the microstructure modification on the RS state and the fatigue properties is investigated. Energy dispersive x-ray and neutron diffraction are combined to investigate the near-surface and bulk RS state of a L-PBF AlSi10Mg material. Differences in the endurance limit are evaluated experimentally by high cycle fatigue (HCF) tests and cyclic R-curve determination.
In a laboratory test, transparent high‐density polyethylene (HDPE) jerrycans have been exposed to both UV radiation and 55 wt‐% nitric acid solution at (41 ± 2)°C, for up to 20 days. For comparison, UV radiant exposure (21 days) and nitric acid exposure (up to 6 weeks) were performed separately, at nearly equal temperatures. The damages are compared with FTIR spectroscopy in ATR and HT‐gel permeation chromatography(GPC) on a molecular level and with hydraulic internal pressure testing as a component test. For the used jerrycans, relevant oxidation can only be found after the combined exposure. This is caused by the decomposition of nitric acid into nitrous gases by UV radiation, which is also observed at lower concentrations (28 wt‐%). After 6 days of laboratory exposure, this is rated as critical, which corresponds to about 1/10 year in Central Europe, according to the UV radiant exposure. The gradual increase in oxidative damage shows the reproducibility of the test.
Flexible organic crystals (elastic and plastic) are important materials for optical waveguides, tunable optoelectronic devices, and photonic integrated circuits. Here, we present highly elastic organic crystals of a Schiff base, 1-((E)-(2,5-dichlorophenylimino)methyl)naphthalen-2-ol (1), and an azine molecule, 2,4-dibromo-6-((E)-((E)-(2,6-dichlorobenzylidene)hydrazono)methyl)phenol (2). These microcrystals are highly flexible under external mechanical force, both in the macroscopic and the microscopic regimes. The mechanical flexibility of these crystals arises as a result of weak and dispersive C−H⋅⋅⋅Cl, Cl⋅⋅⋅Cl, Br⋅⋅⋅Br, and π⋅⋅⋅π stacking interactions. Singly and doubly-bent geometries were achieved from their straight shape by a micromechanical approach using the AFM cantilever tip. Crystals of molecules 1 and 2 display a bright-green and red fluorescence (FL), respectively, and selective reabsorption of a part of their FL band. Crystals 1 and 2 exhibit optical-path-dependent low loss emissions at the termini of crystal in their straight and even in extremely bent geometries. Interestingly, the excitation position-dependent optical modes appear in both linear and bent waveguides of crystals 1 and 2, confirming their light-trapping ability.
The overview of the activity of group 8.5 Micro-NDT (BAM, Belin, Germany) in the field of additively manufacturing material characterization will be presented. The research of our group is focused on the 3D imaging of AM materials by means of X-ray Computed Tomography at the lab and at synchrotron, and the residual stress characterization by diffraction (nondestructive technique).
Additiv gefertigte (AM) dreifach periodische metallische minimale Oberflächenstrukturen (TPMSS, aus dem Englischen Triply Periodic Minimum Surface Structures) erfüllen mehrere Anforderungen sowohl im biomedizinischen als auch im technischen Bereich: Abstimmbare mechanische Eigenschaften, geringe Empfindlichkeit gegenüber Herstellungsfehlern, mechanische Stabilität und hohe Energieabsorption. Allerdings stellen sie auch einige Herausforderungen in Bezug auf die Qualitätskontrolle dar, die ihre erfolgreiche Anwendung verhindern können. Tatsächlich ist die Optimierung des AM-Prozesses ohne die Berücksichtigung struktureller Merkmale wie Fertigungsgenauigkeit, interne Defekte sowie Oberflächentopographie und -rauheit unmöglich. In dieser Studie wurde die quantitative zerstörungsfreie Analyse von Ti-6Al-4V-Legierung TPMSS mit Hilfe der Röntgen-Computertomographie (XCT) durchgeführt. Es werden mehrere neue Bildanalyse-Workflows vorgestellt, um die Auswirkungen der Aufbaurichtung auf die Wanddickenverteilung, die Wanddegradation und die Verringerung der Oberflächenrauheit aufgrund des chemischen Ätzens von TPMSS zu bewerten. Es wird gezeigt, dass die Herstellungsgenauigkeit für die Strukturelemente, die parallel und orthogonal zu den hergestellten Schichten gedruckt werden, unterschiedlich ist. Verschiedene Strategien für das chemische Ätzen zeigten unterschiedliche Pulverabtragsfähigkeiten und damit ein Gradient der Wanddicke. Dies wirkte sich auf die mechanische Leistung unter Druck durch die Verringerung der Streckspannung aus. Eine positive Auswirkung des chemischen Ätzens ist die Verringerung der Oberflächenrauhigkeit, die möglicherweise die Ermüdungseigenschaften der Bauteile verbessern kann. Schließlich wurde XCT eingesetzt, um die Menge des zurückgehaltenen Pulvers mit der Porengröße des TPMSS zu korrelieren, wodurch der Herstellungsprozess weiter verbessert werden kann.
Unter Passivität versteht man den Korrosionsschutz durch dünne, festhaftende Schichten aus Korrosionsprodukten. Für den schadensfreien Einsatz nichtrostender Stähle ergeben sich daraus zwei grundsätzliche Anforderungen.
Erstens muss sich die Passivschicht vollständig ausbilden können. Dabei sind die Oberflächenausführung, die mechanische Bearbeitung, die Elementverteilung, Ausscheidungen, die Wärmeeinbringung z.B. bei der schweißtechnischen Verarbeitung, Anlauffarben, sowie die chemische Nachbehandlung bzw. Konditionierung der Oberflächen von großer Bedeutung. Zweitens muss die Repassivierung von Defektstellen unter den Einsatzbedingungen möglich sein. Für das Repassivierungsvermögen sind die Legierungszusammensetzung, mögliche kritische Betriebszustände, prozessbedingte Besonderheiten, wie etwa Stagnationsbedingungen und Reinigungsprozesse von Bedeutung.
Even though we often do not knowingly recognize them, nanoparticles are present these days in most areas of our daily life, including food and its packaging, medicine, pharmaceuticals, cosmetics, pigments as well as electronic products, such as computer screens. The majority of these particles exhibits a core-shell morphology either intendedly or unintendedly. For the purpose of practicability, this core-shell nanoparticle (CSNP) morphology is often assumed to be ideal, namely a spherical core fully encapsulated by a shell of homogeneous thickness with a sharp interface between core and shell material. It is furthermore widely presumed that all nanoparticles in the sample possess the same shell thickness. As a matter of fact, most real CSNPs deviate in several ways from this ideal model with quite often severe impact on how efficiently they perform in a specific application.
The topic of this cumulative PhD thesis is the accurate characterization of the actual morphology of CSNPs by advanced X-ray analytical techniques, namely X-ray photoelectron spectroscopy (XPS) and scanning transmission X-ray microscopy (STXM). A special focus is on CSNPs which deviate from an ideal core-shell morphology. In the paper from 2019 nanoparticle shell thicknesses are extracted from the elastic-peak intensities in an XPS spectrum based on an ideal particle morphology. This happens for a series of CSNP samples comprising a poly(tetrafluoroethylene) (PTFE) core and either a poly(methyl methacrylate) (PMMA) or polystyrene (PS) shell. The same paper as well as the paper from 2020 demonstrate for the first time, that the analysis of the inelastic background in an XPS spectrum of CSNPs can identify and quantify the heterogeneity of the shell and the incomplete encapsulation of the core.
The result from an XPS experiment is always an average across a large nanoparticle ensemble. Deviations from an ideal morphology within a single particle of the sample cannot be assessed separately. As opposed to that, a spatial resolution of 35 nm enables STXM to visualize the interior of single CSNPs which exhibit a sufficient X-ray absorption contrast between core and shell material. In the paper from 2018 a STXM analysis is demonstrated based on the example of the PTFE-PS CSNP samples already mentioned in the previous paragraph.
In the publication from 2021 (Ca/Sr)F₂ core-shell like nanoparticle ensembles for the practical use in, among others, antireflective coatings are investigated. These nanoparticles do not possess a sharp interface between core and shell material, which is why a shell thickness determination as described in the second paragraph is inappropriate. Instead, in-depth profiles of the chemical composition are obtained by XPS experiments based on synchrotron radiation with variable X-ray photon energy to elucidate the internal morphology of the particles. Additionally, theoretical in-depth profiles of Ca and Sr XPS peak intensities are simulated, in order to facilitate the interpretation of the experiments. Thus, an enrichment of CaF₂ at the particle surface was determined, which could hardly have been assessed by any other analytical technique. Because this kind of non-destructive depth profiling by XPS is very demanding, more than usual effort is spent on gapless documentation of the experiments to ensure full reproducibility.
Due to the vast diversity of nanoparticles differing in material, composition and shape, a measurement procedure cannot unalteredly be transferred from one sample to another. Nevertheless, because the papers in this thesis present a greater depth of reporting on the experiments than comparable publications, they constitute an important guidance for other scientists on how to obtain meaningful information about CSNPs from surface analysis.
The fabrication of laser-generated surface structures on titanium and titanium alloys has recently gained remarkable interests, being technologically relevant for applications in optics, medicine, fluid transport, tribology, and wetting of surfaces. The morphology of these structures, and so their chemistry, is influenced by the different laser processing parameters such as the laser fluence, wavelength, pulse repetition rate, the effective number of laser pulses per beam spot area, etc. A simple way to characterize laser-generated surface structures is by means of optical microscopy (OM) or white light interference microscopy (WLIM). The latter can address the surface topography, while having a lateral resolution limit of ~(lambda)/2 (lambda = illumination wavelength). To resolve morphologies with spatial periods significantly smaller than (lambda)/2, scanning electron microscopy (SEM) is often used, taking benefit of the reduced de Broglie wavelength associated to the electrons of several keV energy. However, all the above-mentioned techniques lack the necessary depth-resolution to reveal and quantify sub-surface material modifications of these laser-generated structures. Time-of-Flight secondary ion mass spectrometry (ToF-SIMS) represents a promising surface analytical technique for studying laser-induced chemical surface alterations since the method combines a high surface sensitivity with the capability to perform a depth-profiling of the laser-affected surface zone. In this study we combine WLIM and high-resolution SEM with ToF-SIMS to fully characterize the evolution of various types of laser-generated micro- and nanostructures formed on Ti-6Al-4V alloys upon irradiation by near infrared ultrashort laser pulses (1030 nm, 925 fs) at different laser fluence levels, effective number of pulses, and at different pulse repetition rates (1 – 400 kHz). We show how this combined surface analytical approach allows to evaluate alterations in the surface chemistry and topography of the laser-generated surface structures depending on the laser processing parameters
We demonstrate here using a disulfide system the first example of reversible, selective, and quantitative transformation between three crystalline polymorphs by ball mill grinding. This includes the discovery of a previously unknown polymorph. Each polymorph is reproducibly obtained under well-defined neat or liquid-assisted grinding conditions, revealing subtle control over the apparent thermodynamic stability. We discovered that the presence of a contaminant as low as 1.5% mol mol−1 acting as a template is required to enable all these three polymorph transformations. The relative stabilities of the polymorphs are determined by the sizes of the nanocrystals produced under different conditions and by surface interactions with small amounts of added solvent. For the first time, we show evidence that each of the three polymorphs is obtained with a unique and reproducible crystalline size. This mechanochemical approach gives access to bulk quantities of metastable polymorphs that are inaccessible through recrystallisation.
The overview of the activity of group 8.5 Micro-NDT (BAM, Belin, Germany) in the field of additively manufacturing material characterization will be presented. The challenges in the residual stress analysis of AM components are discussed on the basis on the show studies performed in BAM. Also, the synchrotron X-ray refraction technique, available in BAM, is presented, showing example of in-situ heating test of Al10SiMg AM material.
We report a new sequence selective terpolymerisation in which three monomers (butylene oxide (BO) A, PhNCS B and phtalic thioanhydride (PTA) C) are selectively enchained into an (ABA′C)n sequence. PTA/PhNCS/BO ring-opening terpolymerisation ROTERP can be coupled with CS2 ROTERP to generate tetrapolymers and with εDL ROP in switchable catalysis for blockpolymer synthesis.
Till now application of printed magnetoelectronics is hindered by lack of large area exchange coupled metallic multilayers required to produce printable magneto-sensory inks. Large-scale roll-to-roll (R2R) fabrication process is an attractive approach owing to its capabilities for high volume, high throughput, and large area manufacturing. Precise and high performance R2R sputtering technology is developed to fabricate large area giant magnetoresistive (GMR) thin-films stacks that contain 30 metallic bilayers prepared by continuous R2R sputtering of Co and Cu sequential on a hundred meters long polyethylene terephthalate (PET) web. The R2R sputtered Co/Cu multilayer on a 0.2 × 100 m2 PET web exhibits a GMR ratio of ≈40% achieving the largest area exchange coupled room temperature magneto-sensitive system demonstrated to date. The prepared GMR thin-film is converted to magnetosensitive ink that enables printing of magnetic sensors with high performance in a cost-efficient way, which promotes integration with printed electronics. An average GMR ratio of ≈18% is obtained for 370 printed magnetic sensors. The realized precise R2R sputtering approach can also be extended to a wide range of hybrid thin-film material systems opening up a path for new functional inks applied with printing technologies.
n this work, three classes of fatigue models are reviewed according to the fatigue regimes commonly considered in the current components design. Particular attention is devoted to the so-called Class III fatigue models, covering the three fatigue regimes, namely, LCF, HCF and VHCF. The applicability and limitations of the pro-posed analytical sigmoidal solutions are discussed from the viewpoint of practical design. The compatible Weibull S-N model by Castillo and Canteli is revisited and improved by considering a new reference parameter GP = E⋅σM ⋅(dε/dσ)|M as the driving force alternative to the conventional stress range. In this way, the requirement, σM ≤ σu, according to the real experimental conditions, is fulfilled and the parametric limit number of cycles, N0, recovers its meaning. The probabilistic definition of the model on the HCF and VHCF regimes is maintained and extended to the LCF regime. The strain gradients may be calculated from the monotonic or cyclic stress–strain curve of the material although a direct derivation from the hysteresis loop is recommended. Some Class III fatigue models from the literature and another one improved by the authors are applied to the assessment of one experimental campaign under different stress ratios conditions and the results compared accordingly. Finally, the new probabilistic GP-N field is evaluated. The results confirm the practical confluence of the stress- and the strain-based approaches into a single and advantageous unified methodology.
Statement of problem
The design of the implant-abutment connection has been widely researched, but the impact of different crown-abutment geometries remains unclear.
Purpose
The purpose of this in vitro study was to evaluate the effect of different crown-abutment margin geometries on the mechanical behavior and fit of screw-retained implant-supported single-crown restorations by using mechanical static and fatigue tests and mastication simulation.
Material and methods
A total of 45 cobalt-chromium premolar-shaped metal frameworks were fabricated for single-unit implant-supported screw-retained restorations on stock abutments and internal hexagon Ø4.25×11-mm cylindrical implants. They were divided into 3 groups according to margin geometry: S, shoulder; C, chamfer; and F, feather-edge. Three static load until fracture and 24 dynamic load tests were performed by using the International Organization for Standardization 14801:2016 standard (ISO 14801:2016) (number of cycles limit: 5×106 cycles, frequency: 6 Hz). The ProFatigue software program was used to optimize the procedure (S, n=12 specimens; C, n=7 specimens; and F, n=5 specimens). Six additional specimens from each group were subjected to a mastication simulation (limit number of cycles: 1×106 cycles, cyclic loading from Pmin=30 N to Pmax=300 N, frequency: 6 Hz). Results from the fatigue tests were reported descriptively, and the Fisher exact test was used to analyze the difference in failure modes. Data from maximum misfit were evaluated by photogrammetry and statistically analyzed with the Anderson-Darling test and the Kruskal-Wallis and Dunn multiple comparison tests (α=.05).
Results
The fatigue limit was 456 N for group S, 512 N for group C, and 514 N for group F. The mean ±standard deviation misfit was 2.6 ±0.1 μm for group S, 3.8 ±1.1 μm for group C, and 3.6 ±0.8 μm for group F. Differences in misfit between groups S and C and between groups S and F were statistically significant (P<.05).
Conclusions
Crown-abutment connections with chamfer and feather-edge margins showed better mechanical behavior, while shoulder margin exhibited better fit. However, high levels of fit were achieved for all the evaluated geometries.
Design methodology of vessel produced by L PBF stainless steel using representative specimens
(2022)
This work presents the preliminary results of an ongoing project with a double objective: on the one hand, the characterisation of the mechanical properties against fatigue damage of an additively manufactured 316 stainless steel produced by laser powder bed-based (L-PBF) technology; on the other hand, the implementation of numerical simulation techniques able to predict the mechanical behaviour of the material in order to optimise and reduce the design costs of vessels used in the chemical sector. The current state of the work developed in this research framework allows showing the first batch of experimental results of crack propagation rate (FCGR) and high cycle fatigue (HCF) tests. The geometry of the vessels studied presents three clearly differentiated regions, either in terms of thickness (11-15 mm) or concerning the inclination of the walls to the direction of manufacturing (0º - 45º). The experimental campaign carried out so far allows identifying the differences in behaviour when comparing different extraction locations around the vessel. This is due to the variations in thermal cycles that the deposited material undergoes during the manufacturing process. Therefore, this causes variations in the microstructure which lead to changes in the response of the material. In this work, these differences are analysed qualitatively and quantitatively from the results of FCGR and HCF, thus allowing to locate the regions with the highest risk in terms of structural integrity against fatigue. This preliminary phase together with the numerical simulation of the additive manufacturing process are key to achieving a reliable description and modelling of the material. The latter will make it possible to address the priority aim of this project, involving the manufacture of independent samples whose properties are representative of the original material extracted from the reference vessels. It is, therefore, a comprehensive methodology for the design of additively manufactured components based on the localised fatigue mechanical properties of representative specimens.
La tecnología de fabricación aditiva (AM) continúan progresando y permitiendo alcanzar diseños cada vez más complejos y optimizados. La industria química es uno de los sectores donde componentes AM han adquirido un gran interés. La falta hasta la fecha de una directiva europea que regule la inspección, certificación y aceptación de equipos sometidos a presión hace necesario progresar en esta línea. El objetivo que se persigue en este trabajo es el de desarrollar una metodología de diseño sobre componentes fabricados aditivamente basada en la estimación de vida a fatiga de las zonas más susceptibles de sufrir dicho tipo de fallo. El estudio comprende diversas facetas de análisis, simulaciones numéricas, análisis de la microestructura del material y una extensa campaña experimental. La evaluación de la integridad estructural se realiza aplicando mecánica de fractura. La historia térmica a lo largo del proceso de fabricación determina la microestructura del componente en cada región y, por ende, influye en las propiedades mecánicas en cada una. Se presentan los resultados preliminares de un proyecto de investigación en curso dirigido a la caracterización de propiedades mecánicas en recipientes de presión producidos por fusión láser en lecho de polvo (L-PBF, por sus siglas en inglés) de acero inoxidable 316L. Se detallan los resultados preliminares en términos de velocidad de crecimiento de grietas por fatiga (FCGR), y se comparan los resultados de probetas extraídas de diferentes regiones de los depósitos.
L-lactide (LA) was polymerized in toluene by means of neat tin(II) 2-ethylhexanoate (SnOct2). Concentration, time and temperature were varied. The isothermally crystallized polyLAs (PLA) were characterized in the virgin state with regard to topology, molar mass, melting temperature (Tm), crystal modification, high or low Tm morphology, crystallinity and crystal thickness. Even a small amount of solvent favored cyclization relative to polymerization in bulk, so that cyclic polylactides were obtained at 115 ◦C and even at 95 ◦C. At all temperatures the α-modification of PLA was obtained along with crystallinities up to 90%. With 6 M solution the high Tm morphology with Tm’s > 190 ◦C was obtained at 115 ◦C. The crystal thickness of crystallites grown from solution at 115 ◦C was on the average 10–20% higher than that of PLA polymerized in bulk. At a polymerization temperature of 75 ◦C cyclization was incomplete and fewer perfect crystallites were formed. A new hypothesis for the crystal growth of cyclic polyLAs is proposed.
Trash to treasure: recovery of transition metal phosphates for (electro-)catalytical applications
(2022)
Wastewaters containing high concentrations of NH4+, PO43- and transition metals are environmentally harmful and toxic pollutants. At the same time phosphorous and transition metals constitute valuable resources. Here, we report the synthesis routes for Co- and Ni-struvites (NH4MPO4∙6H2O, M = Ni2+, Co2+) out of aqueous solutions resembling synthetic/industrial waste water compositions, and allowing for P, ammonia and metal co-precipitation. Furthermore, the as-obtained struvites were further up-cycled. When heated, these transition metal phosphates (TMPs) demonstrate significant changes in the degree of crystallinity/coordination environment involving a high amount of amorphous phases and importantly develop mesoporosity (Figure 1). In this regard, amorphous and mesoporous TMPs are known to be highly promising (electro-)catalysts.
Amorphous phases do not represent a simple “disordered” crystal but more a complex system with a broad range of compositions and physicochemical properties, which remain mostly unknown. Consequently, we investigated the recrystallization and amorphization process during thermal treatment and a resolved the complex amorphous/crystalline structures (Figure 2). As a proof-of-principle for their applicational use, the as-obtained TMPs demonstrate significant proton conductivity properties similar to apatite-like structures from room to high temperatures (>800°C).
Hence, we have developed a promising recycling route in which environmental harmful contaminants like PO43-, NH4+ and 3d metals would be extracted out of waste waters in the form of precursor raw materials. These raw materials can be then further up-cycled through a simple thermal treatment for their specific application in electrocatalysis.
Industrial and agricultural waste streams (waste water, sludges, tailings, etc.) which contain high concentrations of NH4+, PO43–, and transition metals are environmentally harmful and toxic pollutants. At the same time, phosphorous and transition metals constitute highly valuable resources. Typically, separate pathways have been considered to extract hazardous transition metals or phosphate independently from each other. Investigations on the simultaneous removal of multiple components have been carried out only to a limited extent. Here, we report the synthesis routes for Ni- and Co-struvites (NH4MPO4·6H2O, M = Ni2+ and Co2+), which allow for P, ammonia, and metal co-precipitation. By evaluating different reaction parameters, the phase and stability of transition metal struvites as well as their crystal morphologies and sizes could be optimized. Ni-struvite is stable in a wide reactant concentration range and at different metal/phosphorus (M/P) ratios, whereas Co-struvite only forms at low M/P ratios. Detailed investigations of the precipitation process using ex situ and in situ techniques provided insights into the crystallization mechanisms/crystal engineering of these materials. M-struvites crystallize via intermediate colloidal amorphous nanophases, which subsequently aggregate and condense to final crystals after extended reaction times. However, the exact reaction kinetics of the formation of a final crystalline product varies significantly depending on the involved metal cation in the precipitation process: several seconds (Mg) to minutes (Ni) to hours (Co). The achieved level of control over the morphology and size makes precipitation of transition metal struvites a promising method for direct metal recovery and binding them in the form of valuable phosphate raw materials. Under this paradigm, the crystals can be potentially up-cycled as precursor powders for electrochemical or (electro)catalytic applications, which require transition metal phosphates.
In the present work, electron backscatter diffraction was used to determine the microscopic dislocation structures generated during creep (with tests interrupted at the steady state) in pure 99.8% aluminium. This material was investigated at two different stress levels, corresponding to the power-law and power-law breakdown regimes. The results show that the formation of subgrain cellular structures occurs independently of the crystallographic orientation. However, the density of these cellular structures strongly depends on the grain crystallographic orientation with respect to the tensile axis direction, with <111> grains exhibiting the highest densities at both stress levels. It is proposed that this behaviour is due to the influence of intergranular stresses, which is different in <111> and <001> grains.
It is already known that the laser beam welding (LBW) or hybrid laser-arc welding (HLAW) processes are sensitive to manufacturing tolerances such as gaps and misalignment of the edges, especially at welding of thick-walled steels due to its narrow beam diameter. Therefore, the joining parts preferably have to be milled. The study deals with the influence of the edge quality, the gap and the misalignment of edges on the weld seam quality of hybrid laser-arc welded 20-mm-thick structural steel plates which were prepared by laser and plasma cutting. Single-pass welds were conducted in butt joint configuration. An AC magnet was used as a contactless backing. It was positioned under the workpiece during the welding process to prevent sagging. The profile of the edges and the gap between the workpieces were measured before welding by a profile scanner or a digital camera, respectively. With a laser beam power of just 13.7 kW, the single-pass welds could
be performed. A gap bridgeability up to 1 mm at laser-cut and 2 mm at plasma-cut samples could be reached respectively.
Furthermore, a misalignment of the edges up to 2 mm could be welded in a single pass. The new findings may eliminate the need for cost and time-consuming preparation of the edges.
The incorporation of nanoscale particles into elastomers enable a boost in performance and/or a distinct reduction of conventional filler loadings due to their high surface to volume ratio. 2D layered nanoparticles like graphene and graphene-related materials provide a great potential as effective fillers in rubber, especially by enhancing mechanical and barrier properties. The type and properties of the nanoparticles, their interface and the elastomeric matrix materials influence the technical behavior, and therefore the potential application fields of such rubber nanocomposites. Especially crucial for the efficiency of the nanofiller, however, is its best possible incorporation into the elastomer. The dispersing of nanoparticles without agglomerates usually constitutes a challenge when using conventional two-roll milling or internal mixing. Academic approaches for highly dispersed nanocomposites solve this problem but are often energy and time consuming with no feasible scale up possibility. Therefore, an ultrasonic assisted NR latex premixing process was established to produce highly filled masterbatches, enabling the main processing with conventional rubber processing techniques.
Two carbon-based nanoparticles with similar specific surface areas were investigated and incorporated in natural rubber as nanocomposites: A commercially available multilayer graphene (MLG) and a nanoscale carbon black (nCB). The mentioned premixed masterbatches were further processed to nanocomposites by the addition of matrix NR, two-roll milling, and hot pressing (vulcanization). By this procedure an increase in Young’s modulus of 157% (MLG) and 71% (nCB) could be obtained at a concentration level of 3 phr. As anisotropic material behavior was observable for the nanocomposites containing MLG, different measurement methods were investigated to quantify the orientation of the nanoparticles in the nanocomposites: Sorption measurements (swelling in 2 dimensions), hardness and dynamical mechanical analysis (in-plane vs. cross-plane), X-Ray diffraction and transmission and scanning electron microscopy.
Quantification of the Total and Accessible Number of Functional Groups and Ligands on Nanomaterials
(2022)
Surface-functionalized organic and inorganic nanoparticles (NP) are of great interest in the life and material sciences, as they can be used e.g. as drug carriers, fluorescent sensors, and multimodal labels in bioanalytical assays and imaging applications. NP performance in such applications depends not only on particle size, size distribution, and morphology, but also on surface chemistry, i.e. the total number of surface functional groups (FG) and the number of FG accessible for subsequent functionalization with ligands or biomolecules, which in turn determines surface charge, colloidal stability, biocompatibility, and toxicity. Methods for FG quantification should be simple, robust, reliable, fast, and inexpensive, and allow for the characteriza-tion of a broad variety of nanomaterials differing in size, chemical composition, and optical properties.
Aiming at the development of simple, versatile, and multimodal tools for the quantification of many bioanalytically relevant FG such as amine, carboxy, thiol and aldehyde functionalities, we investigated and compared various analytical methods commonly used for functional group quantification. This includes electrochemical titration methods, dye-based optical assays, and other instrumental analytical techniques such as nuclear magnetic resonance, mass spectrometry, and thermal analysis methods.
The robust determination of the threshold against fatigue crack propagation DKth is of paramount importance in fracture mechanics based fatigue assessment procedures. The standards ASTM E647 and ISO 12108 introduce operational definitions of DKth based on the crack propagation rate da/dN and suggest linear fits of logarithmic DK– da/dN test data to calculate DKth. Since these fits typically suffer from a poor representation of the actual curvature of the crack propagation curve, a method for evaluating DKth using a nonlinear function is proposed. It is shown that the proposed method reduces the artificial conservativeness induced by the evaluation method as well as the susceptibility to scatter in test data and the influence of test data density.
The large surface-to-volume ratio of nanoparticles is understood to be the source of many interesting phenomena. The melting temperature of nanoparticles is shown to dramatically reduce compared to bulk material. Yet, at temperatures below this reduced melting point, a liquid-like atomic arrangement on the surface of nanoparticles is still anticipated to influence its properties. To understand such surface effects, here, we study the coalescence of Au nanoparticles of various sizes using molecular dynamics simulations. Analysis of the potential energy and Lindemann index distribution across the nanoparticles reveals that high-energy, high-mobility surface atoms can enable the coalescence of nanoparticles at temperatures much lower than their corresponding melting point. The smaller the nanoparticles, the larger the difference between their melting and coalescence temperatures. For small enough particles and/or elevated enough temperatures, we found that the coalescence leads to a melting transition of the two nominally solid nanoparticles, here discussed in relation to the heat released due to the surface reduction upon the coalescence and the size dependence of latent heat. Such discontinuous melting transitions can lead to abrupt changes in the properties of nanoparticles, important for their applications at intermediate temperatures.
Genormte künstliche Bewitterungstests sind häufig nicht spezifisch für die Anwendungssituation oder das Material. Das macht die Entwicklung spezifischer Tests erforderlich. Für deren Entwicklung müssen Maximalparameter der Anwendungssituation bekannt sein, womit dann der künstliche Test formuliert wird und dessen Bedingungen werden dann solange optimiert, bis die Korrelation der Effekte von natürlichem und künstlichem Test ausreichend ist.
Für Untersuchungen der Freisetzung kann der verbleibende Rest in der Probe und/oder die freigesetzte Menge in Luft, Boden, Wasser bestimmt werden.
Im ersten Beispiel der Witterungswirkung wurde die Freisetzung von Kohlenstoff-Nanoröhrchen (CNT) aus Polymer-Kompositen untersucht (unter Verwendung von empfindlich-nachweisbarer radioaktiver 14C-Markierung für einzelne CNT-Partikel), in einem zweiten die Freisetzung von anorganischen und organischen Bestandteilen aus elastomeren Bestandteilen von Sportböden (Bahnen und Kunstrasen) in Wasser.
Molecularly imprinted polymers (MIPs) against sialic acid (SA) have been developed as a detection tool to target cancer cells. Before proceeding to in vivo studies, a better knowledge of the overall effects of MIPs on the innate immune system is needed. The aim of this study thus was to exemplarily assess whether SA-MIPs lead to inflammatory and/or cytotoxic responses when administered to phagocytosing cells in the innate immune system. The response of monocytic/macrophage cell lines to two different reference particles, Alhydrogel and PLGA, was compared to their response to SA-MIPs. In vitro culture showed a cellular association of SA-MIPs and Alhydrogel, as analyzed by flow cytometry. The reference particle Alhydrogel induced secretion of IL-1b from the monocytic cell line THP-1, whereas almost no secretion was provoked for SA-MIPs. A reduced number of both THP-1 and RAW 264.7 cells were observed after incubation with SA-MIPs and this was not caused by cytotoxicity. Digital holographic cytometry showed that SA-MIP treatment affected cell division, with
much fewer cells dividing. Thus, the reduced number of cells after SA-MIP treatment was not linked to SA-MIPs cytotoxicity. In conclusion, SA-MIPs have a low degree of inflammatory properties, are not cytotoxic, and can be applicable for future in vivo studies.
Most of the Al alloys used in additive manufacturing (AM), in particular Laser Powder Bed Fusion (LPBF), do not exceed a strength of 200 MPa, whereas conventionally high-performance alloys exhibit strengths exceeding 400 MPa. The availability of such Al alloys in AM is limited due to difficulties in printability, requiring synergetic material and AM process development to satisfy harsh processing conditions during LPBF [1]. One approach is the addition of reinforcement to the based powder, allowing tailoring composition and properties of a Metal Matrix Composite (MMC) by AM. Still, the effect of the reinforcement on the resulting mechanical properties must be studied to understand the performance and limits of the newly developed material. The goal of this work was to investigate the failure mechanism of LPBF Al-based MMC material using in-situ Synchrotron X-ray Computed Tomography (SXCT) during mechanical testing.
Additively manufactured (AM) metallic sheet-based Triply Periodic Minimal Surface Structures (TPMSS) meet several requirements in both bio-medical and engineering fields: Tunable mechanical properties, low sensitivity to manufacturing defects, mechanical stability, and high energy absorption. However, they also present some challenges related to quality control. In fact, the optimization of both the AM process and the properties of TPMSS is impossible without considering structural characteristics as manufacturing accuracy, internal defects, and as well as surface topography and roughness. In this study, the quantitative non-destructive analysis of TPMSS manufactured from Ti-6Al-4V alloy by electron beam melting was performed by means of laboratory X-ray computed tomography (XCT).
Toughening mechanisms and enhanced damage tolerant fatigue behaviour in laminated metal composites
(2022)
In the present study, fatigue crack growth (FCG) in a laminated metal composite (LMC) consisting of Al-based constituents with dissimilar strength was studied. Additionally, the FCG in both monolithic constituent materials was determined and a linear elastic rule of mixture (ROM) concept was calculated as a reference for the FCG of the laminated composite. Crack networks in the laminates were analyzed post-mortem by means of light microscopy and synchrotron X-Ray tomography (SXCT). Significantly reduced FCG rates for the LMC were found at elevated stress intensity ranges compared to both the monolithic constituents as well as the ROM concept. This is the result of the formation of a complex 3D crack network in the laminated architecture caused by the appearance of the two different toughening mechanisms a) crack deflection and b) crack bifurcation at the vicinity of the interfaces.
Sintering, crystallization, and foaming of 44.8SiO2–2.5P2O3–36.5CaO–6.6Na2O–6.6K2O–3.0CaF2 (F3) and 54.6SiO2–1.7P2O3–22.1CaO–6.0Na2O–7.9K2O–7.7MgO (13–93) bioactive glass powders milled in isopropanol and CO2 were studied via heating microscopy, differential thermal analysis, vacuum hot extraction (VHE), Infrared spectroscopy, and time-of-flight secondary ion mass spectrometry. Full densification was reached in any case and followed by significant foaming.
VHE studies show that foaming is driven by carbon gases and carbonates were detected by Infrared spectroscopy to provide the major foaming source. Carbonates could be detected even after heating to 750◦C, which hints on a thermally very stable species or mechanical trapping. Otherwise, dark gray compact colors for milling in isopropanol indicate the presence of residual carbon as well. Its significant contribution to foaming, however, could not be proved and might be
limited by the diffusivity of oxygen needed for carbon oxidation to carbon gas.
To assess the ability of cracks to grow, a robust determination of the threshold against fatigue crack propagation ∆Kth is of paramount importance. The standards ASTM E647 and ISO 12108 introduce operational definitions of ∆Kth based on the crack propagation rate da/dN. For evaluating ∆Kth, both suggest fitting a linear function to a defined subset of the logarithmic ∆K – da/dN test data, where ∆Kth follows by evaluating the linear function at da/dN = 10-7 mm/cycle and da/dN = 10-8 mm/cycle, respectively.
In general, this kind of fit suffers from a bad representation of the actual curvature of the crack propagation curve. Therefore, we propose a robust method for evaluating ∆Kth using a non-linear function that reduces the artificial conservativeness induced by the evaluation method as well as the susceptibility to scatter in test data and the influence of test data density. The method is calibrated against a large set of S690QL crack growth data obtained from a total of 48 specimens, and validated against a set of S355NL and S960QL data (3 specimens each), obtained as a part the IBESS (integral fracture mechanics determination of the fatigue strength of welds) project.
Concrete has a long history in the construction industry and is currently one of the most widely used building materials. Especially precast concrete elements are frequently utilized in construction projects for standardized applications, increasing the quality of the composite material, as well as reducing the required building time. Despite the accumulated knowledge, continuous research and development in this field is essential due to the complexity of the composite combined with the ever-growing number of applications and requirements. Especially in view of global climate change, design aspects as CO2 emissions and resource efficiency require new mix designs and optimization strategies. A result of the material’s high complexity and heterogeneity on multiple scales is that utilizing the full potential with changing demands is highly challenging, even for the established industry. We propose a framework based on an ontology, which automatically combines experimental data with numerical simulations. This not only simplifies experimental knowledge transfer, but allows the model calibration and the resulting simulation predictions to be reproducible and interpretable. This research shows a way towards a more performance oriented material design. Within this talk we present our workflow for an automated simulation of a precast element, demonstrating the interaction of the ontology and the finite element simulation. We show the automatic calibration of our early-age concrete model [1, 2], to improve the prediction of the optimal time for the removal of the form work.
Here, we present a study on agarose thin-film samples that represent a model system for the exopolysaccharide matrix of biofilms. Povidone-iodide (PVP-I) was selected as an antibacterial agent to evaluate our x-ray photoelectron spectroscopy (XPS)-based methodology to trace specific marker elements, here iodine, commonly found in organic matrices of antibiotics. The in-depth distribution of iodine was determined by XPS analyses with variable excitation energies and in combination with argon gas cluster ion beam sputter cycles. On mixed agarose/PVP-I nanometer-thin films, both methods were found to solve the analytical task and deliver independently comparable results. In the mixed agarose/PVP-I thin film, we found the outermost surface layer depleted in iodine, whereas the iodine is homogeneously distributed in the depth region between this outermost surface layer and the interface between the thin film and the substrate. Depletion of iodine from the uppermost surface in the thin-film samples is assumed to be caused by ultrahigh vacuum exposure resulting in a loss of molecular iodine (I2) as reported earlier for other iodine-doped polymers.
Morpho-Chemical Characterisation of Me-TiO2 Nanoparticles for Enhanced Photocatalytical Activity
(2022)
The conversion of solar energy into electricity and solar fuels is of crucial importance for a green and sustainable future. Water splitting using semiconductor photo-catalysts is considered a sustainable method to produce clean hydrogen (H2) fuel. Nevertheless, H2 photo-production efficiency remains still low, although extensive research works to understand better the mechanisms of the Hydrogen Evolution Reaction (HER) and the Oxygen Evolution Reaction (OER) are being carried out. In this respect, TiO2 is a key photoactive material, usually employed with a co-catalyst deposited onto the surface to enhance charge carriers’ separation and catalyze surface charge transfer reactions. The deposition of a co-catalyst on the TiO2 nanoparticle surface represents one successful way to enhance the activity of the photocatalyst through a modification of its surface and redox properties. In this context, high-resolution scanning electron microscopy coupled with elemental analysis by energy-dispersive X-ray spectroscopy (EDS) is fundamental for studying and understanding the effect of the nanoparticle morphology on the functional properties of shape-controlled TiO2 crystals (bipyramides, platelets, and elongated particles). Different types of metal-semiconductor combinations, TiO2 shapes and dopant metals (Ag, Pt, etc) and metal concentrations will be discussed.
For the development of selective and sensitive chemical sensors, we have developed a new family of poly(etherphosphoramide) polymers. These polymers were obtained with satisfactory yields by nucleophilic aromatic polycondensation using isosorbide as green resources, and bisphenol A with two novel difluoro phosphinothioic amide monomers. Unprecedented, the thiophosphorylated aminoheterocycles monomers, functionalized with two heterocyclic amine, N-methylpiperazine and morpholine were successfully obtained by nucleophilic substitution reaction of P(S)–Cl compound. The resulting polymers were characterized by different analytical techniques (NMR, MALDI–ToF MS, GPC, DSC, and ATG). The resulting partially green polymers, having tertiary phosphine sulfide with P–N side chain functionalities along the main chain of polymers are the sensitive film at the surface of a gold electrode for the impedimetric detection of Cd, Ni, Pb and Hg. The bio-based poly(etherphosphoramide) functionalized with N-methylpiperazine modified sensor showed better analytical performance
than petrochemical based polymers for the detection of Ni2+. A detection limit of 50 pM was obtained which is very low compared to the previously published electrochemical sensors for nickel detection.
Recently, additive manufacturing of ceramics has achieved the maturity to be transferred from scientific laboratories to industrial applications. At the same time, research is progressing to expand the boundaries of this field into the territory of novel materials and applications. This feature issue addresses current progress in all aspects of additive manufacturing of ceramics, from parts design to feedstock selection, from technological development to characterization of printed components.
Nach einer kurzen Einführung in die Schallemissionsprüfung und -Analyse wird ein Versuchsstand vorgestellt, der im Rahmen des Themenfeldprojektes Seal Waste Safe installiert wurde. Schwerpunkt des Vortrages sind die Schallemissionsmessungen an einem 150 l Demonstrator aus Salzbeton und einem weiteren aus alkali-aktiviertem Material. Neben der konventionellen Schallemissionsanaylse mit Aktivitäts- und Intensitätsparametern der Zeitsignale, werden auch frequenzbasierte Parameter zur Analyse andiskutiert.
This 6 minute long MP4-video presents some key results of the European research project "BioCombs4Nanofibers" to the broader public. Inspired by nature, some concepts of certain types of spiders are transferred to technology in order to develop bacteria-repellent surfaces through laser surface nanostructuring.
Funding notice: This study was funded by the European Union's research and innovation program under the FET Open grant agreement No. 862016 (BioCombs4Nanofibers, http://biocombs4nanofibers.eu).
The detection of internal irregularities is crucial for quality assessment in metal-based additive manufacturing (AM) technologies such as laser powder bed fusion (L-PBF). The utilization of in-process thermography as an in situ monitoring tool in combination with post-process X-ray micro computed tomography (XCT) as a reference technique has shown great potential for this aim. Due to the small irregularity dimensions, a precise registration of the datasets is necessary as a
requirement for correlation. In this study, the registration of thermography and XCT reference datasets of a cylindric specimen containing keyhole pores is carried out for the development of a porosity prediction model. The considered datasets show variations in shape, data type and dimensionality, especially due to shrinkage and material elevation effects present in the manufactured part. Since the resulting deformations are challenging for registration, a novel preprocessing methodology is introduced that involves an adaptive volume adjustment algorithm which is based on the porosity distribution in the specimen. Thus, the implementation of a simple three-dimensional image-to-image registration is enabled. The results demonstrate the influence of the part deformation on the resulting porosity location and the importance of registration in terms of irregularity prediction.
Das Grundproblem der heute verfügbaren und normativ geregelten Prüfverfahren für Zinküberzüge besteht neben den realitätsfernen Prüfbedingungen vor allem in der subjektiv geprägten Auswertung der Prüfergebnisse. Die systematische Betrachtung der Entwicklungen der letzten Jahre zeigt, dass die üblichen Verfahren den aktuellen Anforderungen damit schon vom Ansatz her nicht gerecht werden können und auch die bisher betriebene, fortlaufende Variation und Anpassung von Prüfbedingungen keinen grundlegend neuen Lösungsansatz bieten können. Ein solcher ergibt sich nur, wenn die Zinküberzüge hinsichtlich der kinetischen Eigenschaften der Deckschichtbildung und -auflösung umfassend beschrieben werden können, was nur durch den Einsatz elektrochemischer Untersuchungsmethoden mittels Gelelektrolyten möglich ist.
Aus diesem Grund wurde im Verbundforschungsvorhaben GELELEK auf der Basis elektrochemischer Methoden unter Verwendung eines Gelelektrolyten ein Normenvorschlag für eine Prüfnorm erarbeitet und zur Normungsreife geführt, welcher den Anforderungen an ein Messsystem für Feldanwendungen entspricht.
Im Verbundforschungsvorhaben GELELEK wurde eine gezielte Kombination von Laboruntersuchungen mit Untersuchungen im Feld und Bauteilen unter realen Einsatzbedingungen angestrebt. Randbedingungen für eine gesicherte Messung von atmosphärisch bewitterten Zinküberzügen unter Einsatz von Gelelektrolyten wurden erarbeitet und im Normenvorschlag festgeschrieben. Darüber hinaus wurde ein mobiles Messgerät für Messungen mit Gelelektrolyten an realen Bauteilen entwickelt. Nach Abschluss des Forschungsvorhabens steht Industrievertretern und Prüfinstituten ein wissenschaftlich gesichertes Messverfahren basierend auf Kennwerten zur Verfügung, um Zinküberzüge und deren momentane Schutzwirkung unter praxisrelevanten Bedingungen einschätzen und normativ geregelt prüfen zu können.
Der vorliegende Forschungsbericht gibt einen Überblick über die Motivation zur Durchführung des Forschungsvorhabens, wichtige Arbeitsschritte, Details zur entwickelten Prüfmethode sowie Einsatzmöglichkeiten für Prüfinstitute und Unternehmen.
Aim of this study is to provide information about moisture dependent material behaviour of unstabilised loadbearing earth blocks and mortars. Compressive strength and Young’s modulus were investigated after conditioning in varying relative humidity reaching from 40 % up to 95 %. The material composition and physical properties were investigated to understand the influence of relative humidity onto the mechanical properties. A normalisation of strength and stiffness by the values obtained at 23 ◦C and 50 % relative humidity reveals a linear dependence of compressive strength and Young’s modulus that is regardless of the material composition.
Thus, it is possible to describe the influence of relative humidity onto the load-bearing behaviour of unstabilised earth masonry materials in a generally valid formulation.
Alkali-silica reaction (ASR) is a chemical reaction within concrete which can lead over time to cracking and spalling. Due to the complexity of the problem, it still causes damage to concrete constructions worldwide.
The publication aims to illustrate the interdisciplinary research of the German Federal Institute for Materials Research and Testing (BAM) within the last 20 years, considering all aspects of ASR topics from the macro to the micro level. First, methods for characterization and assessment of ASR risks and reaction products used at BAM are explained and classified in the international context. Subsequently the added value of the research approach by combining different, preferably nondestructive, methods across all scales is explained using specific examples from a variety of research projects. Aspects covered range from the development of new test-setups to assess aggregate reactivity, to analysis of microstructure and reaction products using microscopical, spectroscopical and X-ray methods, to the development of a testing methodology for existing concrete pavements including in-depth analysis of the visual damage indicator and the de-icing salt input using innovative testing techniques. Finally, research regarding a novel avoidance strategy that makes use of internal hydrophobization of the concrete mix is presented.
Für die rechnerische Dimensionierung der Betondecken im Oberbau von Verkehrsflächen für den Neubau sowie die Erneuerung nach RDO-Beton 09 ist die statische Spaltzugfestigkeit an der unteren und oberen Bohrkernscheibe entsprechend der Vorgaben der AL Sp-Beton zu bestimmen. Aufgrund der unzureichenden Kenntnis der Präzision dieses Prüfverfahrens wurden, basierend auf dem Entwurf des FGSV-Merkblatts zur statistischen Auswertung von Prüfergebnissen, mit einem breit aufgestellten Ringversuch die statistischen Kennwerte an Labor- und Bestandsbetonen unter Vergleich- und Wiederholbedingungen ermittelt. Zur möglichst guten statistischen Absicherung nahmen an dem Ringversuch dreizehn erfahrene Prüfstellen teil, die vorab einem Audit unterzogen wurden. Zur Abdeckung des vielschichtigen Einsatzes des Prüfverfahrens erfolgte der Ringversuch an acht Prüflosen, die sowohl die Erst-/ Eignungsprüfung und Übereinstimmungskontrolle bei Neubaumaßnahmen, als auch die Restsubstanzbewertung von Betonfahrbahnplatten berücksichtigen. Zur Bewertung des Materialeinflusses wurde zusätzlich ein Prüflos mit Labormörtel untersucht.
Die Probenvorbereitung erfolgte zentral an der BAM. Zur Sicherstellung einheitlicher Prüfbedingungen bei den Prüfstellen wurde zusätzlich eine detaillierte Standardarbeitsanweisung erarbeitet, die partiell bereits Eingang in das Normenwerk gefunden hat. Bei der Plausibilitätsprüfung aller prüflosspezifischen Einzelwerte der Spaltzug- und Druckfestigkeit wurden vereinzelt sowohl Ausführungsfehler als auch Übertragungs- und Tippfehler festgestellt. Der sich anschließende Lilliefors-Test zeigt, dass die ermittelten Einzelwerte bis auf wenige Aus-nahmen normalverteilt sind und damit die Voraussetzungen für die statistische Auswertung gegeben sind.
Mittels grafischer Darstellung der Mandel’s h- und k-Werte wurden die Auffälligkeiten hinsichtlich der Mittelwerte und Varianzen prüflosspezifisch für die einzelnen Prüfstellen visualisiert und anschließend einige von ihnen mittels Grubbs- und Cochran-Test als Ausreißer identifiziert. Nach Ausreißerelimination wurde mit dem klassischen Verfahren bei der Spaltzugfestigkeit der geringste Variationskoeffizient unter Vergleich- und Wiederholbedingungen bei der Erst-/Eignungsprüfung mit 6,2 und 6,4 Prozent ermittelt. Bei einer Verminderung des Materialeinflusses durch die Verwendung eines Labormörtels verbessern sich die statistischen Kennwerte auf 4,5 und 5,3 Prozent. Mit 8,2 und 9,5 Prozent beziehungsweise 8,6 und 9,5 Prozent werden bei der Restsubstanzbewertung von Wasch- und Unterbetonen die höchsten Werte bestimmt.
Das robuste Auswerteverfahren (ohne Eliminierung der Ausreißer) nach dem Entwurf des FGSV-Merkblatts zur statistischen Auswertung von Prüfergebnissen erwies sich in der Form als ungeeignet und bedurfte einer Überarbeitung. Bezüglich der vergleichend mit klassischen und robusten Verfahren gewonnenen Kennwerte ist festzustellen, dass bei sehr homogenen Messergebnissen eines Prüfloses beide Verfahren nahezu die gleichen statistischen Kennwerte liefern. Bei der Eliminierung von Ausreißern sind die Ergebnisse des robusten Verfahrens in der Regel etwas größer als die des klassischen Verfahrens.
Die begleitenden vertiefenden Untersuchungen bei der Spaltzugprüfung mit innovativen Prüftechniken lieferten wertvolle Erkenntnisse zur Bewertung der Prüfeinflüsse.
The OECD Working Party on Manufactured Nanomaterials (WPMN) has actively worked towards understanding possible safety issues for manufactured nanomaterials and has contributed significantly to resolving these by developing Test Guidelines, Guidance Documents, Test Reports and other publications with the aim of a safe use of manufactured nanomaterials. To address the specific needs of manufactured nanomaterials, the OECD Test Guideline No. 110 “Particle Size Distribution/Fibre Length and Diameter Distributions” was identified as one of the test guidelines (TGs) to require an update. The current TG 110 (adopted in 1981) is only valid for particles and fibres with sizes above 250 nm. The WPMN prioritised to either update TG 110 to be applicable also to particles at the nanoscale or draft a new nanomaterial specific (TG).
Eventually, it was decided to develop a new TG that covers the size range from 1 nm to 1000 nm, intended for particle size and particle size distribution measurements of nanomaterials. Paragraph 11 provides further justification on the need for such measurements for nanomaterials. This TG overlaps with TG 110 in the size range from 250 nm to 1000 nm. When measuring particulate or fibrous materials, the appropriate TG should be selected depending on the size range of particles tested. In line with TG 110, the new TG for nanomaterials includes separate parts for particles and fibres.
For the part of this TG which addresses particles, several methods applicable to nanomaterials were reviewed and included to take into account developments since 1981 when the TG 110 was adopted. This TG includes the following methods: Atomic Force Microscopy (AFM), Centrifugal Liquid Sedimentation (CLS)/Analytical Ultracentrifugation (AUC), Dynamic Light Scattering (DLS), Differential Mobility Analysis System (DMAS), (Nano)Particle Tracking Analysis (PTA/NTA), Small Angle X-Ray Scattering (SAXS), Scanning Electron Microscopy (SEM), and Transmission Electron Microscopy (TEM). The method Single Particle Inductively Coupled Plasma Mass Spectrometry (sp-ICP-MS) could not be sufficiently validated within the interlaboratory comparison (ILC) carried out for the different methods in this TG (see also paragraph 6 for further details on the ILC). Applicability of sp-ICP-MS is strongly limited to nanomaterials with high mass values in combination with a sufficiently high particle size. However, the general method ICP-MS is widely used and the sp-mode for the size measurement of specific nanomaterials was successfully performed in ILCs elsewhere. The method is therefore included in the Appendix Part C of this TG, which further details the limitations of sp-ICP-MS.
For measuring the diameter and length of fibres, analysing images captured with electron microscopy is currently the only method available. This TG includes Scanning Electron Microscopy (SEM) and Transmission Electron Microscopy (TEM).
To test the validity of this TG, an ILC was performed. Test materials were chosen to reflect a broad range of nanomaterial classes, e.g. metals, metal oxides, polymers and carbon materials. Where possible, well-characterised test materials were used.
Additionally, the test materials were chosen to reflect a broad range of sizes representing the size range 1 nm to 1000 nm. Specifically for fibres, a broad range of aspect ratios was included (length/diameter of 3 to > 50). Some of the test materials used are commercially available and further references are given in the validation report of the ILC. Sample preparation for physical chemical characterisation is critical for all listed methods. Due to the differences between individual nanomaterials and due to the wide range of individual material properties it is impossible to have a generic protocol to obtain the best possible sample preparation for every nanomaterial. Therefore, a generic protocol on sample preparation is not part of this TG. Information on sample preparation is given in the paragraphs 25-29, 33, 34 and 39 for particles and in paragraphs 159) for fibres. Further information on sample preparation of nanomaterials for physical chemical characterisation can be found in the OECD Guidance on Sample Preparation and Dosimetry for the Safety Testing of Manufactured Nanomaterials and elsewhere.
We study the molecular mobility and electrical conductivity of a homologous series of linear shaped columnar ionic liquid crystals ILCn, (n = 8, 10, 12, 14, 16) using broadband dielectric spectroscopy (BDS), specific heat spectroscopy (SHS), and X-ray scattering. We aim to understand how the alkyl chain length influences the dynamics and electric conductivity in this system. Two dielectrically active relaxation modes are observed, the γ and the αcore process, that correspond to the localized fluctuations of the alkyl chains and cooperative motions of the aromatic core in the columns, respectively. Both the γ relaxation and the αcore process slow down with increasing alkyl chain length. SHS reveals one relaxation process, the αalkyl process that has a similar temperature dependence as that of the αcore process for ILC12, 14, and 16 but shifts to higher temperature for ILC8 and 10. For ILC12, 14, and 16, the absolute values of DC conductivity increase by 4 orders of magnitude at the transition from the plastic crystalline to hexagonal columnar phase. For ILC8 and 10, the DC conductivity behavior is similar to ionic liquids, where the conductivity is coupled with structural relaxation. Small-angle X-ray investigations reveal that both the intercolumnar distance and the disorder coherence length increase with alkyl chain length; conversely, the DC conductivity decreases monotonically.
A few layer/multilayer graphene (MLG) with a specific surface area of BET=250 m2/g is proposed as an efficient multifunctional nanofiller for rubbers. The preparation method, i.e., ultrasonically-assisted solution mixing of master batches followed by two-roll milling, strongly influences the dispersion in the elastomeric matrix and is fundamental for the final properties. When homogenously dispersed, single stacks of only approximately 10 graphene sheets, with an aspect ratio of 34, work at low loadings, enabling the replacement of large amounts of carbon black (CB), an increase in efficiency, and a reduction in filler load. The appropriate preparation yielded nanocomposites in which just 3 phr are sufficient to significantly improve the rheological, curing, gas barrier properties, electrical and thermal conductivity, as well as mechanical properties of different rubbers, as shown for chlorine-Isobutylene-Isoprene rubber (CIIR), nitrile-butadiene rubber (NBR), natural rubber (NR), and styrene-butadiene rubber (SBR). 3 phr of MLG tripled the Young’s modulus of CIIR, an effect equivalent to 20 phr of CB. The stronger interactions between MLG and NR or SBR also resulted in a reduction in the elongation at break by 20% and 50%, respectively, while the same parameter was hardly changed for CIIR/MLG and NBR/MLG. CIIR/MLG and NBR/MLG were stiffer but just as defomable than CIIR and NBR. The strong reinforcing effect of 3 phr MLG was confirmed by the increase of greater than 10 Shore A in hardness. MLG reduces gas permeability, increases thermal and electrical conductivities, and retards flammability, the latter shown by the reduction in heat release rate in the cone calorimeter. We investigated MLG also as a synergist for reducing the aluminium trihydrate loading in flame retardant hydrogenated acrylonitrile-butadiene (HNBR), polybutadiene chloroprene (BR/CR), and chlorosulfonated polyethylene rubber(CSM). The higher the nanofiller concentration is, the greater the improvement in the properties. For instance, the permeability decreased by 30% at 3 phr of MLG, 50% at 5 phr and 60% at 10 phr, respectively. Moreover, the MLG nanocomposites improve stability of mechanical properties against the effects of weathering. In key experiments an increase in UV-absorption and a pronounced radical scavenging were proved as stabilizing mechanisms. In a nutshell, MLG is an efficient multifunctional nanofiller ready to be used for innovative rubber development.
SI Files for "Towards automation of the polyol process for the synthesis of silver nanoparticles"
(2022)
The graphml file: reaction_graph_AgNP.graphml is included. It contains topological information (Fig. 1 in the main text) about the reaction setup and metadata with reaction condtions. It used by the Python API used to control the Chemputer.
SAXS reports. The complete report sheets generated by McSAS are included. They contain extended information characterising the size distributions and the fitting parameters.
NP3_I: saxs_report_NP3_I.pdf
NP3_II: saxs_report_NP3_II.pdf
NP3_III: saxs_report_NP3_III.pdf
NP3_IV: saxs_report_NP3_IV.pdf
NP5_I: saxs_report_NP5_I.pdf
NP5_II: saxs_report_NP5_II.pdf
NP5_III: saxs_report_NP5_III.pdf
In pursuing the automated synthesis of metal nanoparticles (NPs), the capabilities of the “Chemputer” are deployed, for the first time, into the field of inorganic chemistry. Metal NPs have a substantial impact across different fields of science, such as photochemistry, energy conversion, and medicine. Among the commonly used nanoparticles, silver NPs are of special interest due to their antibacterial properties and applications in sensing and catalysis. However, many of the methods used to synthesize Ag NPs often do not result in well-defined products, the main obstacles being high polydispersity or a lack of particle size tunability.
The Chemputer is a modular, automated platform developed by the Cronin group for execution of multi-step, solution based organic synthesis. The machine has been further implemented at BAM, where we used this setup to perform automated organic syntheses, autonomously controlled by feedback derived from online NMR. In the Chemputer liquids can be transferred across a backbone, constructed from HPLC selection valves and syringe pumps. The Chemputer operates in a batch mode, common laboratory devices, such as heaters and glassware like round bottom flasks, are connected to the backbone, forming reaction modules. Solutions can be manipulated in these modules, and as all operations are controlled through a software script, reproducibility among individual syntheses is high. Likewise, any adjustments of the synthesis conditions, if required, are straightforward to implement and are documented in the reaction log file and a code versioning system.
We characterised Chemputer-synthesized nanoparticles using small-angle X-ray scattering, dynamic light scattering and further methods, showing that automated synthesis can yield colloids with reproducible and tuneable properties. The approach is an important first step towards the automation of nanoparticle syntheses in a modular, multipurpose platform. The modularity of the Chemputer opens many possibilities for the synthesis of a variety of different NP morphologies and sizes and potentially more complex structures. These advances and further work can help in the general investigations of silver nanoparticles by supplying a reliable and reproducible method of their synthesis and removing tacit knowledge by significantly reducing the experimental bias.
The complexity of any microstructural characterization significantly increases when there is a need to evaluate the icrostructural evolution as a function of temperature. To date, this characterization is primarily performed by undertaking elaborative ex-situ experiments where the material’s heating procedure is interrupted at different temperatures or times. Moreover, these studies are often limited to a region smaller than the representative elementary volume, which can lead to partial or even biased interpretations of the collected data. This limitation can be greatly overcome by using in-situ synchrotron X-ray refraction (SXRR).
Herein, a simple one-pot procedure is reported to obtain aqueous zinc oxide (ZnO) nanoparticle dispersions from ZnO nanoparticles dispersed in cyclohexane. In the process, polyoxyethylene (20) sorbitan monooleate (polysorbate 80, Tween 80) functions as a phase transfer agent and colloidal stabilizer. The particles grow in a defined manner during the transfer, presumably via coalescence. The final particle radii are tuneable in the range from 2.3 ± 0.1 nm to 5.7 ± 0.1 nm depending on the incubation time of the dispersion at 90 °C. Small-angle X-ray scattering is employed to determine the particle radius distributions before and after phase transfer. The larger ZnO particle radii are associated with a redshift of the optical bandgap and luminescence emission, as expected for semiconductor nanoparticles. The particles presented here exhibit a relative size distribution width of 20%, rendering them attractive for applications in, e.g., biology or catalysis. The latter application is demonstrated at the photocatalytic degradation of methylene blue dye.
The industrial use of additive manufacturing for the production of metallic parts with high geometrical complexity and lot sizes close to one is rapidly increasing as a result of mass individualisation and applied safety relevant constructions. However, due to the high complexity of the production process, it is not yet fully understood and controlled, especially for changing (lot size one) part geometries.
Due to the thermal nature of the Laser-powder bed fusion (L-PBF) process – where parts are built up layer-wise by melting metal powder via laser - the properties of the produced part are strongly governed by its thermal history. Thus, a promising route for process monitoring is the use of thermography. However, the reconstruction of temperature information from thermographic data relies on the knowledge of the surface emissivity at each position on the part. Since the emissivity is strongly changing during the process due to phase changes, great temperature gradients, possible oxidation, and other potential influencing factors, the extraction of real temperature data from thermographic images is challenging. While the temperature development in and around the melt pool, where melting and solidification occur is most important for the development of the part properties. Also, the emissivity changes are most severe in this area, rendering the temperature deduction most challenging.
A possible route to overcome the entanglement of temperature and emissivity in the thermal radiation is the use of hyperspectral imaging in combination with temperature emissivity separation (TES) algorithms. As a first step towards the combined temperature and emissivity determination in the L-PBF process, here, we use a hyperspectral line camera system operating in the short-wave infrared region (0.9 µm to 1.7 µm) to measure the spectral radiance emitted. In this setup, the melt pool of the L-PBF process migrates through the camera’s 1D field of view, so that the radiation intensities are recorded simultaneously for multiple different wavelength ranges in a spatially resolved manner. At sufficiently high acquisition frame rate, an effective melt pool image can be reconstructed. Using the grey body approximation (emissivity is independent of the wavelength), a first, simple TES is performed, and the resulting emissivity and temperature values are compared to literature values. Subsequent work will include reference measurements of the spectral emissivity in different states allowing its analytical parametrisation as well as the adaption and optimisation of the TES algorithms. An illustration of the proposed method is shown in Fig.1.
The investigated method will allow to gain a deeper understanding of the L-PBF process, e.g., by quantitative validation of simulation results. Additionally, the results will provide a data basis for the development of less complex and cheaper sensor technologies for L-PBF in-process monitoring (or for related process), e.g., by using machine learning.
Die additive Fertigung (ugs. „3D-Druck“) ist bei der Herstellung von hochkomplexen metallischen Bauteilen, bionisch inspiriertem Leichtbau oder Prototypen nicht mehr wegzudenken.
Für die konventionelle Fertigung hat sich das bestehende System der Qualitätsinfrastruktur (QI) bewährt. Die additive Fertigung vergrößert den gestalterischen Spielraum von möglichen Bauteilgeometrien und Prozessfehlern jedoch erheblich. Hier gerät die QI an ihre Grenzen, sodass die Fertigung und Zulassung sicherheitsrelevanter Bauteile sehr zeit- und kostenintensive Versuche erfordern. Eine moderne digitale QI erlaubt eine effizientere Qualitätssicherung für additiv gefertigte Bauteile. Dies erfordert eine durchgängig digitale Abbildung des physischen Materialflusses.
To enhance the biological effects of radiation damage in cancerous cells, we present an alternative approach to the use of gold nanoparticles (AuNP), focusing on the synthesis and characterization of highly monodisperse, spherical radioactive gold nanoparticles 198AuNP. The size of the AuNP size was optimized with the help of Geant4/TOPAS particle scattering simulations, and energy deposition per nm3 per decay for varying radii (2–10 nm) was evaluated. This work is the foundation for ongoing experimental work to evaluate cell death induced by 198AuNP which aims for the use of radioactive gold nanoparticles in cancer treatment.
High sensitizer and activator concentrations have been increasingly examined to improve the performance of multi-color emissive upconversion (UC) nanocrystals (UCNC) like NaYF4:Yb,Er and first strategies were reported to reduce concentration quenching in highly doped UCNC. UC luminescence (UCL) is, however, controlled not only by dopant concentration, yet by an interplay of different parameters including size, crystal and shell quality, and excitation power density (P). Thus, identifying optimum dopant concentrations requires systematic studies of UCNC designed to minimize additional quenching pathways and quantitative spectroscopy. Here, we quantify the dopant concentration dependence of the UCL quantum yield (ΦUC) of solid
NaYF4:Yb,Er/NaYF4:Lu upconversion core/shell nanocrystals of varying Yb3+ and Er3+ concentrations (Yb3+ series: 20%‒98% Yb3+; 2% Er3+; Er3+ series: 60% Yb3+; 2%‒40% Er3+). To circumvent other luminescence quenching processes, an elaborate synthesis yielding OH-free UCNC with record ΦUC of ~9% and ~25 nm core particles with a thick surface shell were used. High Yb3+ concentrations barely reduce ΦUC from ~9% (20% Yb3+) to ~7% (98% Yb3+) for an Er3+ concentration of 2%, thereby allowing to strongly increase the particle absorption cross section and UCNC brightness. Although an increased Er3+ concentration reduces ΦUC from ~7% (2% Er3+) to 1% (40%) for 60% Yb3+. Nevertheless, at very high P (> 1 MW/cm2) used for microscopic studies, highly Er3+-doped UCNC display a high brightness because of reduced saturation. These findings underline the importance of synthesis control and will pave the road to many fundamental studies of UC materials.
The talk gives an introduction into gas metal arc welding and its relation to plasma science as well as current challenges in welding research concerning research data management and the application of the FAIR principles.
The WelDX project is introduced and the main goals are discussed and contrasted with the current features of the weldx API.
Different internal and public facing use cases focusing on research data management and their implementation using weldx are presented.
The interactive part of the presentation displays some advanced multi layer use cases and data analysis using the weldx API as well as the integration of materials properties into weldx.
In typical material oriented research projects numerous types and sources of data need to get connected to form the final outcome. The data-structures have to be described in a manner semantically concise enough so that all participants share the meaning and at the same time flexible enough to allow connecting findings and facts that have not been connected before.
The present contribution describes the approach that is being taken in a public funded research project with two cooperating research institutes. The aim of the data-management solution is to describe and interlink three main entity types: material entities like a test specimen that is under observation, immaterial entities like a fatigue life model and processes that generate and transform the immaterial and material entities.
The shared understanding of what is described by the data is achieved by referring to existing linked data resources. In addition a common thesaurus that is subject to ongoing discussion is used for concepts and terms that need precision beyond publicly available concept descriptions. The data associated with the entities and processes and entities is rather small and well structured. The entities and processes covered by the vocabularies are typical to laboratories performing fatigue testing and microstructure analysis. Through the interlinking of the entities and processes it becomes possible to intuitively understand the knowledge that is accumulating in the database. For example it is easy to trace the history of a creep test specimen starting from the chemical composition that has been analyzed for the heat, continuing with the heat treatment of the material, going into the creep test itself with the associated creep data and finally finding the transmission electron microscopy images that have been taken from the crept sample.
The presented approach is prototypical way to tackle the sustainable management of structured open research data. Open questions remain for example with the management of attributions, the acceptance of an increased effort in data creation and the access control to specific regions of the data. On the other hand the approach sketches what added value can be created, if the community adopts and contributes to the linked data principles.
Automated bonding analysis software has been developed based on Crystal Orbital Hamilton Populations to facilitate high-throughput bonding analysis and machine-learning of bonding features. This work presents the software and discusses its applications to simple and complex materials such as GaN, NaCl, the oxynitrides XTaO2N (X=Ca, Ba, Sr) and Yb14Mn1Sb11.
Recent developments of X-ray photoelectron spectroscopy using excitation energies different from the usual lab-sources Mg Kα and Al Kα, thus covering larger and different kinetic energy ranges, require more flexible approaches for determining the transmission function than the well-established ones using reference spectra. Therefore, the approach using quantified peak areas (QPA) was refined allowing a more precise estimation of the transmission function. This refinement was tested by comparing the results obtained with the new version with former calculations. Furthermore, the obtained transmission function was validated by comparing the results with a transmission function using the reference spectrum of polyethylene. Additionally, an ionic liquid was used as reference for estimating the transmission function at the energy resolved HE-SGM beamline at BESSY II. Comparison between the measured and stoichiometric composition shows that a transmission function was determined, which allows a reasonable quantification.
This paper is focused on the approximation of absorbed Charpy impact energy-temperature curves (KV-T) and the management of sub-size test piece results in Charpy pendulum impact tests. Both subjects are frequently underestimated but may have a strong impact on the assessment of product quality and structural integrity. The status of related test standards, product standards, structural integrity assessment procedures and corresponding research is reviewed.
It is concluded that the state of regulation is partly insufficient and wrong. There is a wide gap between the state of knowledge in the field of materials testing and the requirements of product standards and structural integrity assessment procedures. The present paper aims at boosting and supporting the necessary discussion among the parties involved to raise the level of technical safety. Correspondingly, a large experimental database was created by Charpy impact testing of popular modern structural Steels with nominal yield strength from 235 MPa to 960 MPa. KV-T data were generated using test pieces with thicknesses between 2.5 mm and 10 mm. Different strategies for KV-T curve fitting, definition of transition temperatures, as well as upper and lower shelf energy levels were followed, and different scaling procedures were applied to the sub-size test piece results. The results show that proportional scaling of sub-size to full-size test piece results in terms of KV should be disallowed because it is a wrong approach.
Regulations still incorporating such procedures should be revised as soon as possible. Existing nonproportional scaling and conversion procedures were applied. The results obtained illustrate that neither an overall nor consistent conservatism nor an adequate conservatism level can be achieved. In summary, the standardizing bodies should enforce the discussion to revise relevant test standards considering more precise specifications on Charpy data fitting. Furthermore, proposals are made for an improved management of sub-size test piece results.
The presentation shows systematic investigations to describe the corrosion and corrosion product formation processes of pure zinc under the climatic conditions currently prevailing in the Federal Republic of Germany. The investigations in their entirety aim at questioning current and establishing new ways of looking at the formation of corrosion products of pure zinc under atmospheric corrosion conditions. Thus, they make a significant contribution in understanding corrosion protection by zinc and zinc coatings. In particular, the focus is placed on the initial stage of the corrosion product formation. A systematic investigation of this time range, which is characterized by very reactive corrosion products, is only made possible by using gel-type electrolytes. The short periods of time at the beginning of weathering is now measurable and their influence on the formation of corrosion products and the kinetics of layer formation describable. By combining the new electrochemical approach with gravimetric, microscopic and analytical methods, new insights could be gained both on a methodic and scientific level.
Duplex stainless steels (DSS) are frequently used, especially in applications requiring high strength combined with high corrosion resistance in aggressive media. Examples include power plant components and maritime structures. During welding of these steels, local variations in chemical composition can occur. This results in ferritization of the material and negatively affects the mechanical properties of the components. In this work, tungsten inert gas (TIG) welding experiments were performed with DSS. Chemical composition analysis was realized in situ by using Laser Induced Breakdown Spectroscopy (LIBS). The aim of the work is to quantitatively measure the chemical composition in the weld seam of various DSS and to identify possible influences of welding parameters on the microstructure of the material. The chemical concentrations of the main alloying elements Cr, Ni, Mn on the surface of the sample during the welding process and the cooling process were measured. Mn and Ni are austenite stabilizers and their content increases during welding by using certain high alloyed filler material. Spectra were recorded every 1.3 s at a spacing of approximately 2 mm. During the cooling process the location of the measurement was not changed. The LIBS method is proofed to be suitable for the quantitative representation of the chemical compositions during the welding process.
Laser powder-based directed energy deposition (DED-L) is a technology that offers the possibility for 3D material deposition over hundreds of layers and has thus the potential for application in additive manufacturing (AM). However, to achieve broad industrial application as AM technology, more data and knowledge about the fabricated materials regarding the achieved properties and their relationship to the manufacturing process and the resulting microstructure is still needed. In this work, we present data regarding the low-cycle fatigue (LCF) behavior of Ti-6Al-4V. The material was fabricated using an optimized DED-L process. It features a low defect population and excellent tensile properties. To assess its LCF behavior two conventionally manufactured variants of the same alloy featuring different microstructures were additionally tested. The strain-controlled LCF tests were carried out in fully reversed mode with 0.3 % to 1.0 % axial strain amplitude from room temperature up to 400°C. The LCF behavior and failure mechanisms are described. For characterization, optical microscopy (OM), scanning electron microscopy (SEM), and micro-computed tomography (µCT) were used. The low defect population allows for a better understanding of the intrinsic material’s properties and enables a fairer comparison against the conventional variants. The fatigue lifetimes of the DED-L material are nearly independent of the test temperature. At elevated test temperatures, they are similar or higher than the lifetimes of the conventional counterparts. At room temperature, they are only surpassed by the lifetimes of one of them. The principal failure mechanism involves multiple crack initiation sites.
In this study, the influence of aging and mean stress on fatigue of the aluminium-alloy EN AW-2618A is investigated. Therefore axial fatigue tests are carried out on smooth specimens. The experiments show that the fatigue life decreases with increasing mean stress. Furthermore, the tests with the overaged specimens demonstrate that the number of cycles to failure is decreasing with increasing aging time.
Catalysts are important components in chemical processes because they lower the activation energy and thus determine the rate, efficiency and selectivity of a chemical reaction. This property plays an important role in many of today’s processes, including the electrochemical splitting of water. Due to the continuous development of catalyst materials, they are becoming more complex, which makes a reliable evaluation of physicochemical properties challenging even for modern analytical measurement techniques and industrial manufacturing.
We present a fast, vacuum-free and non-destructive analytical approach using multi-sample spectroscopic ellipsometry to determine relevant material parameters such as film thickness, porosity and composition of mesoporous IrOx–TiOy films. Mesoporous IrOx–TiOy films were deposited on Si wafers by sol–gel synthesis, varying the composition of the mixed oxide films between 0 and 100 wt%Ir. The ellipsometric modeling is based on an anisotropic Bruggeman effective medium approximation (a-BEMA) to determine the film thickness and volume fraction of the material and pores. The volume fraction of the material was again modeled using a Bruggeman EMA to determine the chemical composition of the materials. The ellipsometric fitting results were compared with complementary methods, such as scanning electron microscopy (SEM), electron probe microanalysis (EPMA) as well as environmental ellipsometric porosimetry (EEP).
Advanced peptide-based nanomaterials composed of self-assembling peptides (SAPs) are of emerging interest in pharmaceutical and biomedical applications. The introduction of fluorine into peptides, in fact, offers unique opportunities to tune their biophysical properties and intermolecular interactions. In particular, the degree of fluorination plays a crucial role in peptide engineering as it can be used to control the characteristics of fluorine-specific interactions and, thus, peptide conformation and self-assembly. Here, we designed and explored a series of amphipathic peptides by incorporating the fluorinated amino acids (2S)-4-monofluoroethylglycine (MfeGly), (2S)-4,4-difluoroethylglycine (DfeGly) and (2S)-4,4,4-trifluoroethylglycine (TfeGly) as hydrophobic components. This approach enabled studying the impact of fluorination on secondary structure formation and peptide self-assembly on a systematic basis. We show that the interplay between polarity and hydrophobicity, both induced differentially by varying degrees of side chain fluorination, does affect peptide folding significantly. A greater degree of fluorination promotes peptide fibrillation and subsequent formation of physical hydrogels in physiological conditions. Molecular simulations revealed the key role played by electrostatically driven intra-chain and inter-chain contact pairs that are modulated by side chain fluorination and give insights into the different self-organization behaviour of selected peptides. Our study provides a systematic report about the distinct features of fluorinated oligomeric peptides with potential applications as peptide-based biomaterials.
Die zerstörungsfreie Prüfung von metallischen Bauteilen hergestellt mit additiver Fertigung (Additive Manufacturing - AM) gewinnt zunehmend an industrieller Bedeutung. Grund dafür ist die Feststellung von Qualität, Reproduzierbarkeit und damit auch Sicherheit für Bauteile, die mittels AM gefertigt wurden. Jedoch wird noch immer ex-situ geprüft, wobei Defekte (z.B. Poren, Risse etc.) erst nach Prozessabschluss entdeckt werden. Übersteigen Anzahl und/oder Abmessung die vorgegebenen Grenzwerte für diese Defekte, so kommt es zu Ausschuss, was angesichts sehr langer Bauprozessdauern äußerst unrentabel ist. Eine Schwierigkeit ist dabei, dass manche Defekte sich erst zeitverzögert zum eigentlichen Materialauftrag bilden, z.B. durch thermische Spannungen oder Schmelzbadaktivitäten. Dementsprechend sind reine Monitoringansätze zur Detektion ggf. nicht ausreichend.
Daher wird in dieser Arbeit ein Verfahren zur aktiven Thermografie an dem AM-Prozess Laser Powder Bed Fusion (L-PBF) untersucht. Das Bauteil wird mit Hilfe des defokussierten Prozesslasers bei geringer Laserleistung zwischen den einzelnen gefertigten Lagen unabhängig vom eigentlichen Bauprozess erwärmt. Die entstehende Wärmesignatur wird ort- und zeitaufgelöst durch eine Infrarotkamera erfasst. Durch diese der Lagenfertigung nachgelagerte Prüfung werden auch zum Bauprozess zeitversetzte Defektbildungen nachweisbar.
In dieser Arbeit finden die Untersuchungen als Proof-of-Concept, losgelöst vom AM-Prozess, an einem typischen metallischen Testkörper statt. Dieser besitzt eine Nut als oberflächlichen Defekt. Die durchgeführten Messungen finden an einer eigens entwickelten L-PBF-Forschungsanlage innerhalb der Prozesskammer statt. Damit wird ein neuartiger Ansatz zur aktiven Thermografie für L-PBF erforscht, der eine größere Bandbreite an Defektarten auffindbar macht. Der Ansatz wird validiert und Genauigkeit sowie Auflösungsvermögen geprüft. Eine Anwendung am AM-Prozess wird damit direkt forciert und die dafür benötigten Zusammenhänge werden präsentiert.
Functionalized nanomaterials (NM) with their unique size-dependent properties are of increasing relevance for current and future developments in various fields such as medical and pharmaceutical industry, computing, electronics or food and consumer products. The performance and safety of NM are determined by the sum of their intrinsic physicochemical properties.1 Besides other key parameters, the particle surface chemistry, which is largely controlled by the chemical nature and density of functional groups and ligands, must be considered for a better performance, stability, and processibility of NM, as well as their interaction with the environment. Thus, particle standards with well-designed surfaces and methods for functional group quantification can foster the sustainable development of functional and safe(r) NM.2 Here we provide a brief overview of the ongoing research in division Biophotonics to design tailored amorphous silica reference particles with bioanalytically relevant functional groups and ligands, for the development of standardized and validated surface functional group quantification methods.
Poly (ether ether ketone) (PEEK) has a high continuous service temperature, excellent mechanical properties, and good solvent and abrasion resistance, which can be further improved through the addition of carbon nanotubes (CNTs). CNT-PEEK nanocomposites are promising matrices for continuous carbon fibre composites; powder processing can mitigate the high melt viscosities in these systems. In this study, model single fibre (hierarchical) composites were produced by embedding sized and desized carbon fibres in nanocomposite CNTPEEK powders followed by single fibre pull-out tests to assess interfacial characteristics. Carbon fibre-PEEK interfacial shear strength is typically 40–45 MPa. Increasing CNT loadings increased fibre-matrix interfacial shear strength linearly up to ~70 MPa at 5.0 wt%, which was attributed to the CNT-based mechanical modification of the PEEK matrix. Apparent interfacial shear strength was inversely correlated with the embedded fibre length irrespective of carbon fibre sizing or CNT loading, indicating brittle fracture of the fibre-matrix interface.
Pulled out carbon fibres were still coated with the matrix, which indicated strong adhesion at the interface in all samples, likely related to a transcrystalline region. Adhesion was, however, negatively affected by the presence of epoxy sizings. Frictional shear strength was independent of embedded fibre length and CNT content for all samples.
Chemical heuristics are essential to understanding molecules and materials in chemistry. The periodic table, atomic radii, and electronegativities are only a few examples. Initially, they have been developed by a combination of physical insight and a limited amount of data. It is now possible to test these heuristics and generate new ones using automation based on Materials Informatic tools like pymatgen and greater amounts of data from databases such as a Materials Project. In this session, I'll speak about heuristics and design rules based on coordination environments and the concept of chemical bonding. For example, we have tested the Pauling rules which describe the stability of materials based on coordination environments and their connections on 5000 oxides from the Materials Project. In addition, we have created automated processes for analyzing the chemical bonding situation in crystalline materials with Lobster (www.cohp.de) in order to discover new heuristics and design rules.
Inspired by the chemistry of mussel adhesive proteins, polydopamine (PDA) exhibits strong adhesion to nearly any kind of organic or inorganic surface and shows high ability for surface post-modification and secondary reactions. As a result, PDA has been widely used as a base adlayer to enable versatile surface chemistry and functionalization. It has shown great potential in wide range of applications including biomedical field (e.g., drug delivery, adhesives, photothermal therapy, bone and tissue engineering, cell adhesion, biosensing). However, implementation of PDA in microdevices is still hindered by insufficient spatial and temporal control of excited deposition methods.
In this work we present a novel approach to fabricate tunable micropatterned substrates where mussel-inspired chemistry provides base for various surface modification [2]. Current approach applies Multiphoton Lithography (MPL) to initiate local PDA formation, and, therefore, does not require use of microstamp or photomask. As a result, the microstructures of complex designs can be produced with the spatial resolution down to 0.8 μm (Figure 1). The desired design can be easily altered by adjusting the stl model or the fabrication code. Unlike the conventional deposition of PDA based on dopamine auto-oxidation, our method does not require presence of strong oxidants, metal ions or alkaline pH. Herein-demonstrated deposition approach will significantly facilitate applications of polydopamine and other mussel-inspired materials in microdevices and high-resolution active microcomponents (e.g., in MEMS and microfluidics).
Adjustment of MPL parameters revealed that the morphology and thickness of resulted PDA microstructures can be controlled by altering the laser power and its scanning velocity. As a result, it also enables the production of micropatterns with structural gradient. Apart from the glass substrate, we performed PDA patterning at surfaces of different nature such as polychlorotrifluoroethylene, polydimethylsiloxane, polyethylene terephthalate, silicon wafers, and fluorinated glass coverslips. We tested different composition of dopamine solution for its ability of PDA buildup. Solutions containing Tris buffer, phosphate buffer or DI water only as well as different pH (6.0, 7.0 and 8.5) could be successfully applied for high-precision PDA micropatterning. Moreover, the effect of antioxidants and purging of the solution with oxygen and nitrogen was investigated. In all cases, no decrease of deposition efficiency was observed. The chemical nature of PDA was confirmed by locally recorded vibrational and x-ray photoelectron spectra. To ensure post-modification potential of MPL deposited PDA we demonstrated one-step deposition of micropatterns with trypsin. Obtained bio-functionalised surface can be further applied as a protein sensing active microelement.
Asymmetrically bridged aroyl-S,N-ketene acetals and aroyl-S,N-ketene acetal multichromophores can be readily synthesized in consecutive three-, four-, or five-component syntheses in good to excellent yields by several successive Suzuki-couplings of aroyl-S,N-ketene acetals and bis(boronic)acid esters. Different aroyl-S,N-ketene acetals as well as linker molecules yield a library of 23 multichromophores with substitution and linker pattern-tunable emission properties. This allows control of different communication pathways between the chromophores and of aggregation-induced emission (AIE) and energy transfer (ET) properties, providing elaborate aggregation-based fluorescence switches.
Current trends in materials and life sciences are flanked by the need to push detection limits to single molecules or single cells, enable the characterization of increasingly complex matrices or sophisticated nanostructures, speed up the time of analysis, reduce instrument complexity and costs, and improve the reliability of data. This requires suitable analytical tools such as spectroscopic, separation and imaging techniques, mass spectrometry, and hyphenated techniques as well as sensors and their adaptation to application-specific challenges in the environmental, food, consumer product, health sector, nanotechnology, and bioanalysis. Increasing concerns about health threatening known or emerging pollutants in drinking water, consumer products, and food and about the safety of nanomaterials led to a new awareness of the importance of analytical sciences. Another important driver in this direction is the increasing demand by legislation, particularly in view of the 17 sustainable development goals by the United Nations addressing clean energy, industry, and innovation, sustainable cities, clean water, and responsible consumption and production. In this respect, also the development of analytical methods that enable the characterization of material flows in production processes and support recycling concepts of precious raw materials becomes more and more relevant. In the future, this will provide the basis for greener production in the chemical industry utilizing recycled or sustainable starting materials.
This makes analytical chemistry an essential player in terms of the circular economy helping to increase the sustainability of production processes. In the life sciences sector, products based on proteins, such as therapeutic and diagnostic antibodies, increase in importance. These increasingly biotechnologically produced functional biomolecules pose a high level of complexity of matrix and structural features that can be met only by highly advanced methods for separation, characterization, and detection. In addition, metrological traceability and target definition are still significant challenges for the future, particularly in the life sciences.
However, innovative reference materials as required for the health and food sector and the characterization of advanced materials can only be developed when suitable analytical protocols are available. The so-called reproducibility crisis in sciences underlines the importance of improved measures of quality control for all kinds of measurements and material characterization. This calls for thorough method validation concepts, suitable reference materials, and regular interlaboratory comparisons of measurements as well as better training of scientists in analytical sciences.
The important contribution of analytical sciences to these developments is highlighted by a broad collection of research papers, trend articles, and critical reviews from these different application fields. Special emphasis is dedicated to often-overlooked quality assurance and reference materials.
The continuously increasing use of plastics is supposed to result in a rising exposure of MNPs to humans. Available data on human health risks of microplastics after oral uptake increased immensely in the past years and indicates very likely only low risks after oral consumption. Concerning nanoplastics, uptake, transport and potential adverse effects after oral uptake are less well understood. This study aims to investigate differences between microplastic particles and particles in the submicron- and nanoscaled size derived from food-relevant polymers with a particle size range consistent with higher potential for cellular uptake, fate, and effects when applied to human intestinal and liver cells. This work includes the development of cellular and subcellular detection methods for synthetic polymeric particles in the micro- and nanometer-range, using Scanning Electron Microscopy, Small-Angle X-ray and Dynamic Light Scattering methods, Asymmetric Flow Field Flow Fractionation, octanol-water fractionation, fluorescence microscopy and flow cytometry. Polylactic acid (250 nm and 2 μm (polydisperse)), melamine formaldehyde (366 nm) and polymethylmethacrylate (25 nm) were thoroughly characterized. The submicro- and nanoplastic test particles showed an increased uptake and transport quantity through intestinal cells. Both types of particles resulted in observed differences of uptake behavior, most likely influenced by different lipophilicity, which varied between the polymeric test materials. Toxic effects were detected after 24 h only in overload situations for the particles in the submicrometer range. This study provides further evidence for gastrointestinal uptake of submicro- and nanoplastics and points towards differences regarding bioavailability between microplastics and smaller plastic particles that may result following the ingestion of contaminated food and beverages. Furthermore, the results reinforce the importance for studying nanoplastics of different materials of varying size, surface properties, polymer composition and hydrophobicity.
Biofilms are ubiquitous in nature and in the man-made environment. Given their harmful effects on human health, an in-depth understanding of biofilms and the monitoring of their formation and growth are important. Particularly relevant for many metabolic processes and survival strategies of biofilms is their extracellular pH. However, most conventional techniques are not suited for minimally invasive pH measurements of living biofilms. Here, a fluorescent nanosensor is presented for ratiometric measurements of pH in biofilms in the range of pH 4.5–9.5 using confocal laser scanning microscopy. The nanosensor consists of biocompatible polystyrene nanoparticles loaded with pH-inert dye Nile Red and is surface functionalized with a pH-responsive fluorescein dye. Its performance was validated by fluorometrically monitoring the time-dependent changes in pH in E. coli biofilms after glucose inoculation at 37 °C and 4 °C. This revealed a temperature-dependent decrease in pH over a 4-h period caused by the acidifying glucose metabolism of E. coli. These studies demonstrate the applicability of this nanosensor to characterize the chemical microenvironment in biofilms with fluorescence methods.
Im Vortrag werden das Messprinzip des Zentrifugen-Sedimentationsverfahrens erläutert und die Anforderungen der zugrundeliegenden Normen diskutiert. Es schließen sich umfangreiche Ausführungen zur praktischen Durchführung der Messung, insbesondere auch zu den vorbereitenden Arbeiten, sowie zur Auswertung der Rohdaten an. Gezeigt werden die Validierung sowie ein Beispiel zur regelmäßigen Verifizierung des Verfahrens. Nach Beispielen und Vergleichen zu Ergebnissen mit anderen Messverfahren, wird das Verfahren in einer Zusammenfassung bewertet.
This is the final report on the proficiency test (PT) „Measurement of the particle size distribution of ceramic powders by laser diffraction”. The PT was organized by the Federal Institute for Materials Research and Testing (BAM), division 5.5 “Advanced technical ceramics”. The measurements took place from 12/2021 to 03/2022. The aim of the interlaboratory comparison was the proficiency assessment of the participating laboratories.
Management and realization of PT were performed in accordance with DIN EN ISO/IEC 17043:2010.
The basis of the harmonized measuring procedure and the instructions for the interlaboratory comparison was the standard ISO 13320:2020.
The statistical analysis was performed in accordance with DIN ISO 13528:2020 by use of the software PROLab Plus (QuoData GmbH, Dresden, Germany).
A group of 44 laboratories from 17 countries participated in the PT. Laser diffraction analyzers produced by 7 different manufacturers were used. The three test materials were commercial products. Overall, the measured characteristic values of the particle distributions (d10, d50 and d90) were in the size range between 0.5 and 25 μm. The final report contains all individual results in an anonymous way.
Nichtrostende Duplexstähle (DSS) werden häufig verwendet, insbesondere bei Anwendungen, die eine hohe Festigkeit in Verbindung mit einer hohen Korrosionsbeständigkeit in aggressiven Medien erfordern. Beispiele hierfür sind Kraftwerkskomponenten und maritime Anwendungen. Beim Schweißen dieser Stähle kann es zu lokalen Schwankungen in der chemischen Zusammensetzung kommen. Dies führt zu einer Ferritisierung des Werkstoffs und beeinträchtigt die mechanischen Eigenschaften der Bauteile. In dieser Arbeit wurden Versuche zum Wolfram-Inertgas-Schweißen (WIG) mit DSS durchgeführt. Die Analyse der chemischen Zusammensetzung wurde in situ mit Hilfe der laserinduzierten Plasmaspektroskopie (LIBS) durchgeführt. Ziel der Arbeit ist es, die chemische Zusammensetzung in der Schweißnaht verschiedener DSS quantitativ zu messen und mögliche Einflüsse der Schweißparameter auf die Mikrostruktur des Werkstoffs zu ermitteln. Gemessen wurden die chemischen Konzentrationen der Hauptlegierungselemente Cr, Ni, Mn auf der Oberfläche der Probe während des Schweißprozesses und des Abkühlungsprozesses. Mn und Ni sind Austenitstabilisatoren, deren Gehalt beim Schweißen durch die Verwendung bestimmter hochlegierter Schweißzusatzwerkstoffe zunimmt. Die Spektren wurden alle 1,3 s in einem Abstand von etwa 2 mm aufgezeichnet. Während des Abkühlungsprozesses wurde der Ort der Messung nicht verändert. Die LIBS-Methode eignet sich nachweislich zur quantitativen Darstellung der chemischen Zusammensetzungen während des Schweißvorgangs.
This paper presents the results concerning monotropic nematic liquid crystals 4-pentylphenyl 40-alkyl benzoate (5PnB) (n = 3 or 5 carbon atoms in the alkyl chain). Their mesophase properties were supported by images of the polarized optical microscopy. Molecular dynamics in the bulk samples or in the composites prepared with aerosil A380 was investigated by broadband dielectric spectroscopy in a large temperature range, appropriately chosen. Thermo gravimetric and infrared investigations were additionally performed. The data were compared with those of structurally related nematics like cyanophenyl pentyl benzoates, which have a cyan group instead of the pentyl chain. The dielectric spectra of the bulk 3P5B and 5P5B demonstrate a dielectric behavior with several relaxation processes as expected for nematic liquid crystals. The temperature dependence of the relaxation rates (and of the dielectric strength) seems to have two distinguished regimes. Thus, in the isotropic state, at higher temperatures the data obey the Vogel–Fulcher–Tammann law, whereas an Arrhenius law is fitted at lower temperature, in a close similarity to the behavior of a constrained dynamic glass transition. Samples with a high density of silica (larger than 7 g aerosil/1 g of 5PnB) were prepared to observe a thin layer adsorbed on the particle surface; it was estimated that almost each guest 5PnB molecule interacts with the aerosil surface. For the composites only one main relaxation process is observed at frequencies much lower than those for the corresponding bulk, which was assigned to the dynamics of the molecules in the surface layer. Infrared spectroscopy shows that these molecules interact with the surface by the ester carbonyl group leading to the monolayer self-assembly at liquid–solid interface. We note once more the importance of the functional unit(s) for the interaction with the hydroxyl groups on the aerosil surface.
Emanating from developing flame retarded biocomposites, we have proposed renewable natural fibers (including keratin) taken from industrial waste as an authentic sustainable approach. More recently, we have investigated non-vegan flame retardant approaches. This paper loves to give you an insight into our ongoing projects on biogenic industrial wastes like leather, bone meal, and insects. Materials were characterized multi-methodically, flame retardant modes of action quantified, decomposition mechanism proposed, and synergisms explained. Considering the large quantities of leather waste (LW) in industrial-scale production, we underline LW as multifunctional bio-adjuvants. LW enhances the flame retardancy of poly(ethylene-vinyl acetate) (EVA) containing phosphorus flame retardants (P-FR). Products/by-products of the invertebrate and vertebrate farming, respectively, are promising bio-based adjuvants in flame retarded bio-epoxy thermosets. While the addition of bone meal yields the formation of an inorganic shield, protein-based powders from insects provide an intumescent behavior. In combination with a P-FR superior charring and self-extinguishing are obtained.
Acknowledgement: In part of this work was supported by the Volkswagen Foundation grant “Experiment!” No. 97437.
Die zerstörungsfreie Prüfung von metallischen Bauteilen hergestellt mit additiver Fertigung (Additive Manufacturing - AM) gewinnt zunehmend an industrieller Bedeutung. Grund dafür ist die Feststellung von Qualität, Reproduzierbarkeit und damit auch Sicherheit für Bauteile, die mittels AM gefertigt wurden. Jedoch wird noch immer ex-situ geprüft, wobei Defekte (z.B. Poren, Risse etc.) erst nach Prozessabschluss entdeckt werden. Übersteigen Anzahl und/oder Abmessung die vorgegebenen Grenzwerte für diese Defekte, so kommt es zu Ausschuss, was angesichts sehr langer Bauprozessdauern äußerst unrentabel ist. Eine Schwierigkeit ist dabei, dass manche Defekte sich erst zeitverzögert zum eigentlichen Materialauftrag bilden, z.B. durch thermische Spannungen oder Schmelzbadaktivitäten. Dementsprechend sind reine Monitoringansätze zur Detektion ggf. nicht ausreichend.
Daher wird in dieser Arbeit ein Verfahren zur aktiven Thermografie an dem AM-Prozess Laser Powder Bed Fusion (L-PBF) untersucht. Das Bauteil wird mit Hilfe des defokussierten Prozesslasers bei geringer Laserleistung zwischen den einzelnen gefertigten Lagen unabhängig vom eigentlichen Bauprozess erwärmt. Die entstehende Wärmesignatur wird ort- und zeitaufgelöst durch eine Infrarotkamera erfasst. Durch diese der Lagenfertigung nachgelagerte Prüfung werden auch zum Bauprozess zeitversetzte Defektbildungen nachweisbar.
In dieser Arbeit finden die Untersuchungen als Proof-of-Concept, losgelöst vom AM-Prozess, an einem typischen metallischen Testkörper statt. Dieser besitzt eine Nut als oberflächlichen Defekt. Die durchgeführten Messungen finden an einer eigens entwickelten L-PBF-Forschungsanlage innerhalb der Prozesskammer statt. Damit wird ein neuartiger Ansatz zur aktiven Thermografie für L-PBF erforscht, der eine größere Bandbreite an Defektarten auffindbar macht. Der Ansatz wird validiert und Genauigkeit sowie Auflösungsvermögen geprüft. Eine Anwendung am AM-Prozess wird damit direkt forciert und die dafür benötigten Zusammenhänge werden präsentiert.
We present an easy-to-apply method to predict structural trends in the internal nucleation tendency of oxide glasses. The approach is based on calculated crystal fracture surface energies derived from easily accessible diatomic bond energy and crystal lattice data. The applicability of the method is demonstrated on literature nucleation data for isochemically crystallizing oxide glasses.
The symmetry or structural stability of ABO3-type perovskite oxides depends largely on the size of ‘A’ and ‘B’ cations, which determines the material properties. The partial substitution of these cations may be used to tune these properties. The ionic sizes and valence states of the cations play an important role in improving the prop- erties of perovskite. In this study, the substitution of La3+ with Sr2+ with a larger ionic radius and Mn3+ with Fe3+ with a similar ionic radius favored both the crystal symmetry and the mixed ionic–electronic conductivity of the perovskite. Electrodes based on La0.7Sr0.3Mn0.5Fe0.5O3 (LSMFO55) exhibited a faradaic behavior with a specific capacity of 330 C g−1 (92 mAh g−1 ) at 12C rate, while this electrode maintained a capacity of 259 C g−1 at 240C (charge or discharge in 15 s). Additionally, exohedral carbon nano-onions (CNO) were introduced as a negative electrode to design an asymmetric hybrid supercapacitor (AHS) with a widened cell voltage. The use of CNO as a negative electrode in the AHS improved the rate capability drastically compared to the use of rGO. This device maintained a good energy density even at an extra-high charging rate (600C) owing to its outstanding rate capability. The high-rate performance of the LSMFO55//CNO AHS can be elucidated by successful fabrication with a mixed ionic–electronic conductive positive electrode and a CNO negative electrode. Tuning the electronic and ionic conductivities by cationic substitution and adopting an appropriate carbon-derived negative electrode (such as CNO) can provide a practical high-rate hybrid device using various perovskites.
The studied aluminium alloy is EN AW-2618A (2618A). It is very widely used for exhaust gas turbo-charger compressor wheels. Due to long operating times, high cycle fatigue (HCF) and material aging under the influence of temperatures up to 230 °C is particularly relevant for the wheels. The wheels are typically milled from round wrought blanks. From such round blanks, different testpieces are extracted and a comprehensive series of HCF tests is conducted at room temperature. The tests investigate the materials fatigue performance in the T61 state for two load-ratios, namely R = -1 and R = 0.1. Additionally, two overaged material states are tested, accounting for the aging process the material undergoes during long operating times at high temperatures. The experimental results are evaluated and compared to each other.
Furthermore, the design process of notched specimens is presented. With the notched specimens, it is aimed to quantify the notch sensitivity of the material. Relating thereto, two potential model parameters for the fatigue lifetime model are introduced.
Die Integrität der Verstärkungsfasern in Komposit-Zahnstiften ist entscheidend für die Biegefestigkeit und die langfristige Haftung am Zement in den Wurzelkanälen. Es wurde vermutet, dass die Integrität von glasfaserverstärkten Zahnstiften durch das Beschleifen während der zahnmedizinischen Behandlung beeinträchtigt wird. Eine Beschädigung der Fasern führt zu einer erheblichen strukturellen Schwächung über den gesamten Stiftdurchmesser. Glasfragmente, die durch den Kontakt mit dem Zahnbohrer entstehen, können sich vom Stift lösen und die Haftfähigkeit erheblich verringern. Mit Hilfe hochauflösender Synchrotron-Röntgen-Refraktions-Radiographie (SXRR) konnte das Ausmaß der Schäden zuverlässig identifiziert und charakterisiert werden.
Dazu wurden die Glasfaserstifte sowohl im Herstellungszustand als auch nach der Bearbeitung mit einem Diamantbohrer untersucht. Die Datensätze wurden zur Visualisierung und Quantifizierung der morphologischen Charakteristika intakter und durch das Beschleifen beschädigter Regionen analysiert. Sie zeigen Schäden im bearbeiteten Bereich (z. B. Brüche, Splitter und Risse) sowie herstellungsbedingte Inhomogenitäten der Fasern mit einer signifikanten Zunahme der inneren Oberflächen in Probenregionen, die durch das Beschleifen beschädigt wurden.
Die Integrität der Verstärkungsfasern in Komposit-Zahnstiften ist entscheidend für die Biegefestigkeit und die langfristige Haftung am Zement in den Wurzelkanälen. Es wurde vermutet, dass die Integrität von glasfaserverstärkten Zahnstiften durch das Beschleifen während der zahnmedizinischen Behandlung beeinträchtigt wird. Eine Beschädigung der Fasern führt zu einer erheblichen strukturellen Schwächung über den gesamten Stiftdurchmesser. Glasfragmente, die durch den Kontakt mit dem Zahnbohrer entstehen, können sich vom Stift lösen und die Haftfähigkeit erheblich verringern. Mit Hilfe hochauflösender Synchrotron-Röntgen-Refraktions-Radiographie (SXRR) konnte das Ausmaß der Schäden zuverlässig identifiziert und charakterisiert werden.
Dazu wurden die Glasfaserstifte sowohl im Herstellungszustand als auch nach der Bearbeitung mit einem Diamantbohrer untersucht. Die Datensätze wurden zur Visualisierung und Quantifizierung der morphologischen Charakteristika intakter und durch das Beschleifen beschädigter Regionen analysiert. Sie zeigen Schäden im bearbeiteten Bereich (z. B. Brüche, Splitter und Risse) sowie herstellungsbedingte Inhomogenitäten der Fasern mit einer signifikanten Zunahme der inneren Oberflächen in Probenregionen, die durch das Beschleifen beschädigt wurden.
The processing of laser-induced periodic surface structures (LIPSS) represents a simple and robust way for the nanostructuring of solids that allows creating a wide range of surface functionalities featuring applications in optics, tribology, medicine, energy technologies, etc. While the currently available laser and scanner technology already allows surface processing rates at the m2/min level, industrial applications of LIPSS are sometimes hampered by the complex interplay between the nanoscale surface topography and the specific surface chemistry. This typically manifests in difficulties to control the processing of LIPSS and in limitations to ensure the long-term stability of the created surface functions. This presentation aims to identify some unsolved scientific problems related to LIPSS, discusses the pending technological limitations, and sketches the current state of theoretical modelling. Hereby, it is intended to stimulate further research and developments in the field of LIPSS for overcoming these limitations and for supporting the transfer of the LIPSS technology into industry.