Wissenschaftliche Artikel der BAM
Filtern
Erscheinungsjahr
Dokumenttyp
- Zeitschriftenartikel (2018) (entfernen)
Sprache
- Englisch (1975)
- Deutsch (40)
- Mehrsprachig (2)
- Portugiesisch (1)
Schlagworte
- Additive manufacturing (62)
- Fluorescence (54)
- SAXS (46)
- Nanoparticles (44)
- Concrete (37)
- MALDI-TOF MS (36)
- Corrosion (34)
- Quantum yield (34)
- Mechanochemistry (29)
- Polylactide (28)
Organisationseinheit der BAM
- 6 Materialchemie (422)
- 1 Analytische Chemie; Referenzmaterialien (342)
- 8 Zerstörungsfreie Prüfung (308)
- 9 Komponentensicherheit (199)
- 5 Werkstofftechnik (186)
- 7 Bauwerkssicherheit (178)
- 4 Material und Umwelt (176)
- 6.3 Strukturanalytik (163)
- 8.5 Röntgenbildgebung (115)
- 6.1 Oberflächen- und Dünnschichtanalyse (95)
Paper des Monats
- ja (66)
Driven mostly by the search for chemical syntheses under biocompatible conditions, so called "click" chemistry rapidly became a growing field of research. The resulting simple one-pot reactions are so far only scarcely accompanied by an adequate optimization via comparably straightforward and robust analysis techniques possessing short set-up times. Here, we report on a fast and reliable calibration-free online NMR monitoring approach for technical mixtures. It combines a versatile fluidic system, continuous-flow measurement of 1H spectra with a time interval of 20 s per spectrum, and a robust, fully automated algorithm to interpret the obtained data. As a proof-of-concept, the thiol-ene coupling between N-boc cysteine methyl ester and allyl alcohol was conducted in a variety of non-deuterated solvents while its time-resolved behaviour was characterized with step tracer experiments. Overlapping signals in online spectra during thiol-ene coupling could be deconvoluted with a spectral model using indirect hard modeling and were subsequently converted to either molar ratios (using a calibrationfree approach) or absolute concentrations (using 1-point calibration). For various solvents the kinetic constant k for pseudo-first order reaction was estimated to be 3.9 h-1 at 25 °C. The obtained results were compared with direct integration of non-overlapping signals and showed good agreement with the implemented mass balance.
Ein wesentliches Grundbedürfnis ist die Sicherheit, d. h. die Gewissheit, in einer sicheren Umgebung zu leben und zu arbeiten. Die existenzielle Sicherheit ist eine notwendige Voraussetzung zur Befriedigung aller weiteren notwendigen Bedürfnisse. Auch die Technik ist ohne Sicherheit nicht denkbar. Trotz aller Bemühungen kommt es aber immer wieder zu Unfällen, aus welchen Gründen auch immer. Eine Strategie, Unfälle zu verhindern bzw. deren Eintrittswahrscheinlichkeit zu minimieren ist es, zwischen einem Objekt mit einem hohen Gefährdungspotenzial und seiner Nachbarschaft, Barrieren zu errichten, z. B. durch eine schützende Isolierung, Sicherheitsabstände oder durch eine Erdüberdeckung. Die erdgedeckte Verlegung von Pipelines ist Stand der Technik. Über die Überdeckungshöhen scheint es jedoch verschiedene Auffassungen zu geben. Im folgenden Beitrag werden dazu einige Beispiele vorgestellt.
This paper reports the formation of zinc phosphate nanoparticles from the artificial digestion of zinc chloride. Initially, the formation of amorphous primary particles with a mean radius of 1.1 nm is observed, alongside the formation of larger, protein stabilized aggregates. These aggregates, with a radius of gyration of 37 nm, are observed after 5 minutes of exposure to artificial saliva and are shown to be colloidally stable for a minimum time of two weeks. The initially formed primary particles are thought to consist of amorphous zinc phosphate, which is then transformed into crystalline Zn3(PO4)2·4H2O over the course of two weeks. Our results demonstrate that the interaction of inorganic salts with bodily fluids can induce the formation of de novo nanoparticles, which in turn, provides insights into how zinc‐enriched foods may also facilitate the formation of nanoparticles upon contact with saliva. As such, this may be considered as an undesirable (bio)mineralization.
Cryoadsorption on the inner surface of porous materials is a promising solution for safe, fast, and reversible hydrogen storage. Within the class of highly porous metal−organic frameworks, zeolitic imidazolate frameworks (ZIFs) show high thermal, chemical, and mechanical stability. In this study, we selected ZIF-8 synthesized mechanochemically by twin-screw extrusion as powder and pellets. The hydrogen storage capacity at 77 K and up to 100 bar has been analyzed in two laboratories applying three different measurement setups showing a high reproducibility. Pelletizing ZIF-8 increases the packing density close to the corresponding value for a single crystal without loss of porosity, resulting in an improved volumetric hydrogen storage capacity close to the upper limit for a single crystal. The high volumetric uptake combined with a low and constant heat of adsorption provides ca. 31 g of usable hydrogen per liter of pellet assuming a temperature−pressure swing adsorption process between 77 K − 100 bar and 117 K − 5 bar. Cycling experiments do not indicate any degradation in storage capacity. The excellent stability during preparation, handling, and operation of ZIF-8 pellets demonstrates its potential as a robust adsorbent material for technical application in pilot- and full-scale adsorption vessel prototypes.
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.
X‑ray emission during the ablative processing of biological materials by ultrashort laser pulses
(2023)
The ablative laser processing with ultrashort pulsed laser beams may cause secondary emission of hazardous X-rays. While the effect has recently been proven to be considered in working safety regulations when processing technical materials, such as metals, the X-ray emission rates during the ablative processing of biological tissue materials are widely unexplored yet.
Therefore, biological materials like water, isotonic saline solution, pig eyes, and human teeth were ablated with ultrashort laser pulses of 1030 nm wavelength, 600 fs pulse duration and 5 kHz pulse repetition rate, aiming to mimic typical surgery situations. Simultaneously, in-situ X-ray dose rate measurements were performed at a short distance from the plasma to display potential X-ray emission. For all four studied biological materials, our measurements prove the secondary emission of laser-induced X-rays.
Direct Laser Writing (DLW) and X-ray computed tomography (XCT) both offer unique possibilities in their respective fields. DLW produces full three-dimensional (3D) polymer structures on the microscale with resolutions below 100 nm. The fabricated structures can be analysed by XCT or X-ray microscopy (XRM), which incorporates additional X-ray lenses, in three dimensions down to a minimal basic spatial resolution of about 500 nm or 50 nm, respectively. In this work, two different DLW structures are analysed via XCT. Internal defects are detected and analysed for the purpose of quality control. Defects and structures with sizes down to 1.5 µm are successfully analysed. A 3D reconstruction and internal, hidden features of the fabricated structures are shown and discussed. In a first-of-its-kind study, we demonstrate the detectability of a single-voxel line inside a fabricated structure that would not be detectable with SEM or light microscopy. Furthermore, the direct fabrication on a PET substrate is shown to overcome the high X-ray absorbance of commonly used glass substrates. Attenuation spectra of SZ2080 and glass substrates are compared to a fabrication route direct on a 170 µm PET foil. The practical aspects of XCT measurements for DLW structures on different substrates will be discussed.
Selective Electron Beam Melting (SEBM) is a promising powder bed Additive Manufacturing technique for near-net-shape manufacture of high-value titanium components. However without post-manufacture HIPing the fatigue life of SEBM parts is currently dominated by the presence of porosity. In this study, the size, volume fraction, and spatial distribution of the pores in model samples have been characterised in 3D, using X-ray Computed Tomography, and correlated to the process variables. The average volume fraction of the pores (b0.2%) was measured to be lower than that usually observed in competing processes, such as selective laser melting, but a strong relationship was found with the differentbeamstrategies used to contour ,and infill by hatching, a part section. The majority of pores were found to be small spherical gas pores, concentrated in the infill hatched region; this was attributed to the lower energy density and less focused beam used in the infill strategy allowing less opportunity for gas bubbles to escape the melt pool. Overall, increasing the energy density or focus of the beam was found to correlate strongly to a reduction in the level of gas porosity. Rarer irregular shaped pores were mostly located in the contour region and have been attributed to a lack of fusion between powder particles.