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Erscheinungsjahr
- 2020 (1334) (entfernen)
Dokumenttyp
- Zeitschriftenartikel (622)
- Vortrag (398)
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- Posterpräsentation (81)
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- Deutsch (273)
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- Polnisch (1)
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Schlagworte
- Nanoparticles (45)
- Korrosion (29)
- Additive manufacturing (27)
- Fluorescence (27)
- Corrosion (25)
- Nanoparticle (18)
- Laser beam welding (15)
- Additive Manufacturing (14)
- Electron microscopy (14)
- Laser-induced periodic surface structures (LIPSS) (14)
Organisationseinheit der BAM
- 6 Materialchemie (284)
- 1 Analytische Chemie; Referenzmaterialien (219)
- 8 Zerstörungsfreie Prüfung (213)
- 7 Bauwerkssicherheit (195)
- 9 Komponentensicherheit (151)
- 4 Material und Umwelt (135)
- 5 Werkstofftechnik (110)
- 3 Gefahrgutumschließungen; Energiespeicher (93)
- 6.3 Strukturanalytik (84)
- 6.1 Oberflächen- und Dünnschichtanalyse (81)
Paper des Monats
- ja (17)
Länderübergreifende und vereinheitlichte Kriterien zur Einstufung von gefährlichen Chemikalien und zu ihrer Gefahrenkommunikation sind ein wichtiges Element für die Sicherheit im Umgang mit Gefahrstoffen. Das globale System zur Einstufung und Kennzeichnung von Chemikalien – das Globally Harmonized System der Vereinten Nationen (UN) – oder kurz GHS – unterstützt dieses Anliegen und hat auch Eingang in die europäischen Rechtsvorschriften gefunden. Die Vereinten Nationen (UN) haben sich nunmehr einiger systematischer Probleme im GHS angenommen und verändern in diesem Zuge auch das Einstufungssystem für Explosivstoffe. Die Fachdiskussionen im Kreis der Experten bei UN sind komplex und nicht leicht zu verfolgen. Es soll daher hier ein Zwischenstand über die bislang vorliegenden Ergebnisse der damit befassten Arbeitsgruppen dargestellt werden.
Spectroscopy in Catalysis
(2020)
Knowledge-based catalyst development is always an interaction between preparation, analysis and catalytic testing. Only if these three factors fit together can success be expected. For the analytic side of this triangle, spectroscopic methods play a crucial role. Whereas with diffraction, scattering and microscopy, decisive insights into the structure and morphology of the catalysts can be obtained, spectroscopy produces new knowledge about the chemical nature of the catalyst, e.g., its bonding and valence states.
Connecting Diffraction-Based Strain with Macroscopic Stresses in Laser Powder Bed Fused Ti-6Al-4V
(2020)
Mishurova, Tatiana ; Artzt, K. ; Haubrich, J. ; Evsevleev, Sergei ; Evans, Alexander ; Meixner, M. ; Serrano Munoz, Itziar ; Sevostianov, I. ; Requena, G. ; Bruno, Giovanni
The laser powder bed fusion (LPBF) production process often results in large residual stress (RS) in the parts. Nondestructive techniques to determine RS are badly needed. However, a reliable quantification of macro-RS (i.e., stress at the component level) by means of diffraction-based techniques is still a great challenge, because the link between diffraction-based strain and macro-RS is not trivial. In this study, we experimentally determine (by means of in-situ synchrotron radiation diffraction) this link for LPBF Ti-6Al-4V. We compare our results with commonly used models to determine the so-called diffraction elastic constants (DECs). We show that LPBF materials possess different DECs than wrought alloys, simply because their microstructural and mechanical properties are different. We also show that the existing models can be used to calculate DECs only if high accuracy of the RS values is not required. If the peculiarities of the microstructure have to be taken into account (as is the case of additively manufactured materials), a radically new approach is desirable.
Explaining Deviatoric Residual Stresses in Aluminum Matrix Composites with Complex Microstructure
(2020)
Evsevleev, Sergei ; Sevostianov, I. ; Mishurova, Tatiana ; Hofmann, M. ; Garcés, G. ; Bruno, Giovanni
The residual stresses in multiphase metal Matrix composites with both random planar-oriented short fibers and particles were studied by neutron diffraction and by a model based on the reformulation of classic Maxwell’s homogenization method. Contrary to common understanding and state-of-the-art models, we experimentally observed that randomly oriented phases possess non-hydrostatic residual stress. The recently developed modeling Approach allows calculating the residual stress in all phases of the composites. It rationalizes the presence of deviatoric stresses Accounting for the interaction of random oriented phases with fibers having preferential orientation.
More sustainable waste management practices are an important element in the Transformation towards a circular economy (CE). Activities in this area should be dedicated to all groups of waste, including those generated in the water and sewage sector. This paper presents the characteristics of sewage sludge ash (SSA) coming from Polish municipal waste incineration plants. Due to the high content of nutrients such as phosphorus (8.01% P2O5), calcium (5.11% CaO) and magnesium (2.75% MgO), the analyzed SSA may constitute a valuable source of raw materials for the fertilizer industry.
Despite the good fertilizing properties of the SSA, in some cases the presence of heavy metals such as cadmium (0.74–1.4 mg/kg dry matter), lead (49.8–99 mg/kg dry matter), mercury (3.93 mg/kg dry matter) and arsenic (4.23–4.43 mg/kg dry matter) and poor bioavailability of P from SSA disqualifies this waste from direct use as a fertilizer. Therefore, it is necessary to look for methods that will allow the municipal SSA to be processed, for example, technologies for the extraction of phosphorus and the production of phosphate fertilizer. This way of SSA management is in the line with the CE assumptions, in which waste becomes a valuable source of secondary raw materials. Fertilizer produced from waste meeting quality, safety and labelling requirements and limits of organic, microbiological and physical contaminants will be able to be traded freely within the European Union (EU) and receive the CE marking. The idea of use of SSA for fertilizer purposes is consistent not only with the objectives of the CE but also with the Polish National Waste Management Plan 2022 and the Municipal Sewage Sludge Strategy 2019–2022, which emphasizes the necessity to maximize the use of biogenic substances contained in wastewater. Therefore, sustainable management of SSA, in particular its storage in a way enabling the recovery of phosphorus, should be promoted.
Ring–Ring Equilibration in Solid, Even-Numbered Cyclic Poly(l-lactide)s and their Stereocomplexes
(2020)
Even-numbered cyclic poly(d-lactide) and poly(l-lactide) are prepared by ringexpansion polymerization. The cyclic pol(l-lactide) is annealed either at 120 or at 160 °C for several days. The progress of transesterification in the solid state is monitored by the formation of odd-numbered cycles via matrix-assisted laser desorption/ionization-time of flight mass spectrometry. The changes of the crystallinity are monitored by differential scanning calorimetry, wideand small-angle x-ray scattering (WAXS and SAXS) measurements. Despite total even-odd equilibration at 160 °C, the crystallinity of poly(l-lactide) is not reduced. Furthermore, the crystallinity of the stereocomplexes of both cyclic polylactides do not decrease or vanish, as expected, when a blocky or random stereosequence is formed by transesterification. This conclusion is confirmed by 13C NMR spectroscopy. These measurements demonstrate that transesterification is a ring–ring equilibration involving the loops on the surfaces of the lamellar crystallites thereby improving crystallinity and 3D packing of crystallites without significant broadening of the molecular weight distribution.
BAM Report 2019
(2020)
Dieser BAM-Report erscheint zwischen zwei historischen Jubiläen: dem 30. Jahrestag des Mauerfalls am 9. November 1989 und dem der staatlichen Einheit Deutschlands am 3. Oktober 1990.
Für unser Land bedeuten beide Daten eine glückliche Zäsur. Und auch für die Bundesanstalt für Materialforschung und -prüfung (BAM), die in den Jahren der Teilung ihren Sitz im westlichen Teil Berlins behalten hatte, waren sie mit guten Veränderungen verbunden: Zur BAM sind über 500 Wissenschaftler*innen des ostdeutschen Amtes für Standardisierung, Messwesen und Warenprüfung sowie aus den Instituten der Akademie der Wissenschaften in Berlin-Adlershof dazugekommen. Die BAM hat damals neue Tätigkeitsschwerpunkte gewonnen, vor allem auf dem Gebiet der Analytischen Chemie, und konnte sich als Teil des sich auch heute noch rasant entwickelnden Wissenschaftsstandortes Berlin-Adlershof positionieren.
Blicken wir heute auf die bewegten und bewegenden Monate vor 30 Jahren zurück, so tun wir dies aus einer deutlich veränderten Gegenwart: Aktuell beschäftigen uns große gesellschaftliche Herausforderungen wie die digitale Transformation, Energiesicherheit, demografische Veränderungen und der Klimawandel. Berlin ist inmitten dieser Herausforderungen ein Ort der Innovation und des Aufbruchs in der Mitte Europas. Dafür steht beispielhaft die Ansiedlung des Werner von Siemens Centre for Industry & Science, das in den kommenden Jahren im Nordwesten der Stadt wachsen wird. Die BAM ist auch hier Partner des Zukunftsprojekts.
Sicherheit in Technik und Chemie zu gewährleisten - unser Kernauftrag bleibt inmitten dieses beschleunigten Wandels unverändert gültig. Aber er bezieht sich heute auf die Sicherheit von Nanopartikeln, von Werkstücken aus dem 3D-Drucker oder die Speicher von Wasserstoffautos und morgen auf ganz neue Technologien. Dazu forschen wir in unseren fünf Themenfeldern Energie, Infrastruktur, Umwelt, Material und Analytical Sciences weltweit vernetzt.
Über alle Umbrüche hinweg leitet uns dabei eine Idee: Sicherheit macht Märkte. Technologischer Wandel, Kreativität und Erfinder*innengeist ermöglichen den Wohlstand unserer Gesellschaft. Zugleich aber gilt: Erst die Verlässlichkeit neuer Technologien und Materialien schafft das Vertrauen der Menschen in den Wandel und sichert so langfristig unsere Zukunft.
Cyclic poly(L-lactide)s were prepared by ring-opening polymerization combined with simultaneous polycondensation (ROPPOC) in bulk at 160 ° with dibutyltin bis(4-cyanophenoxide) as catalyst. It is demonstrated by MALDI TOF mass spectrometry and 1H NMR end group analyses that cycles are formed by endto-end cyclization in addition to “back-biting” transesterification. Formation of high molar mass cyclic poly L-lactide)s by means of several more reactive ROPPOC catalysts presented previously and in new experiments is discussed. These experimental results, together with theoretical arguments, prove that part of the Jacobson–Stockmayer theory is wrong. The critical monomer concentration, above which end-toend cyclization is seemingly impossible, does not exist and reversible like irreversible polycondensations can theoretically proceed up to 100% conversion, so that finally all reaction products will necessarily adopt a cyclic architecture.
Radunz, Sebastian ; Kraus, Werner ; Bischoff, F. A. ; Emmerling, Franziska ; Resch-Genger, Ute ; Tschiche, Harald
We report on the temperature- and structural-dependent optical properties and photophysics of a set of boron dipyrromethene (BODIPY) dyes with different substitution patterns of their meso-aryl subunit. Single-crystal Xray diffraction analysis of the compounds enabled a classification of the dyes into a sterically hindered and a unhindered group. The steric hindrance refers to a blocked rotational motion of the aryl subunit around the bond connecting this moiety to the meso-position of the BODIPY core. The energy barriers related to this rotation were simulated by DFT calculations. As follows from the relatively low rotational barrier calculated to about 17 kcal/mol, a free rotation is only possible for sterically unhindered compounds. Rotational barriers of more than 40 kcal/mol determined for the sterically hindered compounds suggest an effective freezing of the rotational motion in These molecules. With the aid of temperature-dependent spectroscopic measurements, we could show that the ability to rotate directly affects the optical properties of our set of BODIPY dyes. This accounts for the strong temperature dependence of the fluorescence of the sterically unhindered compounds which show a drastic decrease in fluorescence quantum yield and a significant shortening in fluorescence lifetime upon heating. The optical properties of the sterically hindered compounds, however, are barely affected by temperature. Our results suggest a nonradiative deactivation of the first excited singlet state of the sterically unhindered compounds caused by a conical intersection of the potential energy surfaces of the Ground and first excited state which is accessible by rotation of the meso-subunit. This is in good agreement with previously reported deactivation mechanisms. In addition, our results suggest the presence of a second nonradiative depopulation pathway of the first excited singlet state which is particularly relevant for the sterically hindered compounds.
The catalytic behavior of iron phthalocyanine (FePc)-sensitized magnetic nanocatalysts was evaluated for their application in the oxidative treatment of Bisphenol A (BPA) under mild environmental conditions. Two types of FePc (Fe(II)Pc and Fe(III)Pc), which are highly photosensitive compounds, were immobilized on the surface of functionalized magnetite. The nanomaterials were characterized by high resolution transmission electron microscopy (HR-TEM), X-ray difraction (XRD), Fourier transform infrared spectroscopy (FTIR) and thermogravimetric analyses (TGA). The generation of singlet Oxygen by nanomaterials was also investigated. In the presence of UVA light exposure (365nm) and 15mM H2O2, the M@Fe(III)Pc photocatalyst gave the best results; for a catalyst concentration of 2.0gL −1, around 60% BPA was removed after 120min of reaction. These experimental conditions were further tested under natural solar light exposure, for which also M@Fe(III)Pc exhibited enhanced oxidative catalytic activity, being able to remove 83% of BPA in solution. The water samples were less cytotoxic after treatment, this being confrmed by the MCF-7 cell viability assay.
Kanerva, M. ; Matrenichev, V. ; Layer, R. ; Takala, T. M. ; Laurikainen, P. ; Sarlin, E. ; Elert, Anna Maria ; Yuding, V. ; Seitsonen, J. ; Ruokolainen, J. ; Saris, P.
The quantitative difference in the antibacterial response was measured for pine rosin and propolis against Staphylococcus aureus ATCC 12598. The activity was studied for fibrous networks that form entirely bio-based cellulose-acetate (CA) materials. The analysis considers the effects of bacterial input, additive dosage, solvent type, variation in preparation, as well as the effect of storage time. Based on the results, the electrospun network structure is dependent on the solvent and the concentration of rosin and propolis. Both rosin and propolis improved the cellulose acetate solution processability, yet they formed beads at high concentrations. Rosin and propolis created strong antibacterial properties when these material systems were immersed in the liquid for 24 h at room temperature. The response remained visible for a minimum of two months. The electrospun networks of water and DMAc solvent systems with 1 to 5 wt% rosin content were clearly more efficient (i.e., decrease of 4 to 6 logs in colony forming units per mL) than the propolis networks, even after two months. This efficiency is likely due to the high content of abietic acids present in the rosin, which is based on the Fourier transform infrared spectra. The results of the additional analysis and cell cultivation with dermal fibroblast cells indicated an impairing effect on skin tissue by the rosin at a 1 wt% concentration compared to the pure CA fibers.
Sieg, H. ; Krause, B.-C. ; Kästner, Claudia ; Böhmert, L. ; Lichtenstein, D. ; Tentschert, J. ; Jungnickel, H. ; Laux, P. ; Braeuning, A. ; Fessard, V. ; Thünemann, Andreas ; Luch, A. ; Lampen, A.
Aluminum (Al) can be taken up from food, packaging, or the environment and thus reaches the human gastrointestinal tract. Its toxic potential after oral uptake is still discussed. The fate of different solid and ionic Al species during the passage through the digestive tract is the focus of this research, as well as the cellular effects caused by these different Al species. The present study combines the physicochemical processing of three recently studied Al species (metallic Al0, mineral Al2O3, and soluble AlCl3) in artificial digestion fluids with in vitro cell systems for the human intestinal barrier. Inductively coupled plasma mass spectrometry (ICP-MS) and small-angle X-ray scattering (SAXS) methods were used to characterize the Al species in the artificial digestion fluids and in cell culture medium for proliferating and differentiated intestinal Caco-2 cells. Cytotoxicity testing and cellular impedance measurements were applied to address the effects of digested Al species on cell viability and cell proliferation. Microarray-based transcriptome analyses and quantitative real-time PCR were conducted to obtain a deeper insight into cellular mechanisms of action and generated indications for cellular oxidative stress and an influence on xenobiotic metabolism, connected with alterations in associated signaling pathways. These cellular responses, which were predominantly caused by formerly ionic Al species and only at very high concentrations, were not impacted by artificial digestion. A two-directional conversion of Al between ionic species and solid particles occurred throughout all segments of the gastrointestinal tract, as evidenced by the presence of nanoscaled particles. Nevertheless, this presence did not increase the toxicity of the respective Al species.
Early Stage of Corrosion Formation on Pipeline Steel X70 Under Oxyfuel Atmosphere at Low Temperature
(2020)
The early stage of corrosion formation on X70 pipeline steel under oxyfuel atmosphere was investigated by applying a simulated gas mixture (CO2 containing 6700 ppmv O2, 100 ppmv NO2, 70 ppmv SO2 and 50 ppmv H2O) for 15 h at 278 K and ambient pressure. Short-term tests (6 h) revealed that the corrosion starts as local spots related to grinding marks progressing by time and moisture until a closed layer was formed. Acid droplets (pH 1.5), generated in the gas atmosphere, containing a mixture of H2SO4 and HNO3, were identified as corrosion starters. After 15 h of exposure, corrosion products were mainly X-ray amorphous and only partially crystalline. In-situ energy-dispersive X-ray diffraction (EDXRD) results showed that the crystalline fractions consist primarily of water-bearing iron sulfates. Applying Raman spectroscopy, water-bearing iron nitrates were detected as subordinated phases. Supplementary long-term tests exhibited a significant increase in the crystalline fraction and formation of additional water-bearing iron sulfates. All phases of the corrosion layer were intergrown in a nanocrystalline network. In addition, numerous globular structures have been detected above the corrosion layer, which were identified as hydrated iron sulphate and hematite. As a type of corrosion, shallow pit formation was identified, and the corrosion rate was about 0.1 mma−1. In addition to in-situ EDXRD, SEM/EDS, TEM, Raman spectroscopy and interferometry were used to chemically and microstructurally analyze the corrosion products.
This book by Scrivener Publishing contains 14 chapters written by 82 leading scientists, experienced in the field of coatings. They demonstrate mechanisms, usage and manipulation of cutting‐edge coating methods. Each chapter is well structured and ends with a conclusion, highlighting the content. The book is divided into 3 parts: “Materials and Methods”, “Coating Materials Nanotechnology” and “Advanced Coating Technology and Applications”.
Finally, this book provides a comprehensive insight into innovative research in advanced coating materials and state‐of‐the‐art technologies, without being a real textbook. It fulfills its intension of being beneficial both for technicians and scientists.
Wasserzeichen und Papierstrukturen können einen wesentlichen Beitrag bei der Analyse von Kunstobjekten auf Papier darstellen. Ausgangspunkt hierfür bildet die korrekte Dokumentation mit entsprechender Bildaufnahme und der richtigen Erfassung und Interpretation der Phänomene. An Fallbeispielen aus Forschungsprojekten zu niederländischen Zeichnungen am Kupferstich-Kabinett Dresden und der Grafischen Sammlung Weimar sollen die Möglichkeiten der Papier- und Wasserzeichenforschung als historische Hilfswissenschaft demonstriert werden. Dieser Abendvortrag dient zugleich als Einführung in die Technologie der (Hand-)Papierherstellung, Wasserzeichenerfassung und –recherche.
Welding of 13CrMoV9-10 vanadium steel requires care due to an increased susceptibility to stress relief cracking during post weld heat treatment. Previous research into the crack formation in creep-resistant steels has focused on thermal and metallurgical factors; however, little knowledge has been gathered regarding the crack formation during post weld heat treatment considering real-life restraint conditions. This work is subdivided in two parts. Part I showed that an increasing heat input during submerged arc welding under restraint led to an increasing stress level in the joint prior to the post weld heat treatment. The magnitude of stress relief cracking observed in the heat-affected zone after the post weld heat treatment is affected by the heat input. In Part II of this work, the cracks and the associated microstructure which occurred under restraint were studied. The application of a Special acoustic emission analysis indicated that the cracks formed in a temperature range between 300 and 500 °C during the post weld heat treatment. The toughness in the heat-affected zone of the restrained welds was affected by the welding heat input.
Microstructural analyses of all specimens revealed accelerated aging due to precipitation of carbides during post weld heat treatment under restraint.
The avoidance of failures during the fabrication or operation of petrochemical reactors made of creep-resistant, low-alloy steels as 13CrMoV9-10 requires still research despite over 60 years of international investigations in the field of stress relief cracking. The quality of modern base materials and filler metals leads to the fact that previously known crack causes, such as impurities of S or P, recede into the background. Rather, the causes are increasingly to be found in the fabrication process. Investigations on the influence of heat control on the stresses in welded components and thus on the stress relief cracking sensitivity under realistic manufacturing conditions are not yet available. This work is subdivided in two parts. Part 1 of this study focused on the effect of heat control during submerged arc welding on the stresses. For this purpose, a testing facility was applied, which allows to observe the forces and moments accumulating during welding or heat treatment in a component-like specimen under shrinkage restraint. The stress acting in the specimen increases with higher preheat/interpass temperatures and higher heat input. During the heat treatment, the stresses are relieved. Nevertheless, cracks are formed already during heating. The total crack length correlates with the heat input.
Hot carriers (electrons and holes) generated from the decay of localized surface plasmon resonances can take a major role in catalytic reactions on metal nanoparticles. By obtaining surface enhanced Raman scattering (SERS) spectra of p-aminothiophenol as product of the reduction of p-nitrothiophenol by hot electrons, different catalytic activity is revealed here for nanoparticles of silver, gold, and copper. As a main finding, a series of different ligands, comprising halide and non-halide species, are found to enhance product formation in the reduction reaction on nanoparticles of all three metals. A comparison with the standard electrode potentials of the metals with and without the ligands and SERS data obtained at different electrode potential indicate that the higher catalytic activity can be associated with a higher Fermi level, thereby resulting in an improved efficiency of hot carrier generation. The concept of such a ligand-enhanced hot electron reduction provides a way to make light-to-chemical energy conversion more efficient due to improved electron harvesting.
In this study, the influence of the welding speed, the arc power, and the laser focal position on the solidification crack formation for partial penetration laser hybrid–welded thick-walled plates was investigated.
The solidification cracking in the weld root is a result of interaction between metallurgical and geometrical and thermomechanical factors.
Experimentally, a direct correlation between the welding speed and the crack number was observed. That is by reducing the welding velocity, the crack number was decreased. The focal position shows also a significant influence on the crack number. By focusing the laser on the specimen surface, the crack number has been significantly diminished.
The wire feed speed showed a very slight influence on the crack formation. That is due to the large distance between the critical region for cracking and the arc region.
The numerical model shows a high stress concentration in the weld root for both components (vertical and transversal).
Numerically, the reduced welding speed showed a strong impact on stress, as the model demonstrated a lower stress amount by decreasing the welding speed.
The metallurgical factors, such as the assumed accumulation of the low-melting eutectics in the weld root, should be a contribution for solidification cracking, where the tensile stress is acting.