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- 2020 (7) (entfernen)
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- 6 Materialchemie (3)
- 6.1 Oberflächen- und Dünnschichtanalyse (3)
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- 1.2 Biophotonik (2)
- 8 Zerstörungsfreie Prüfung (2)
- 4 Material und Umwelt (1)
- 4.3 Schadstofftransfer und Umwelttechnologien (1)
- 4.4 Thermochemische Reststoffbehandlung und Wertstoffrückgewinnung (1)
- 8.2 Zerstörungsfreie Prüfmethoden für das Bauwesen (1)
- 8.5 Röntgenbildgebung (1)
Controlling thickness and tightness of surface passivation shells is crucial for many applications of core–shell nanoparticles (NP). Usually, to determine shell thickness, core and core/shell particle are measured individually requiring the availability of both nanoobjects. This is often not fulfilled for functional nanomaterials such as many photoluminescent semiconductor quantum dots (QD) used for bioimaging, solid state lighting, and display technologies as the core does not show the applicationrelevant functionality like a high photoluminescence (PL) quantum yield, calling for a whole nanoobject approach. By combining high-resolution transmission electron microscopy (HR-TEM) and X-ray photoelectron spectroscopy (XPS), a novel whole nanoobject approach is developed representatively for an ultrabright oleic acid-stabilized, thick shell CdSe/CdS QD with a PL quantum yield close to unity. The size of this spectroscopically assessed QD, is in the range of the information depth of usual laboratory XPS. Information on particle size and monodispersity were validated with dynamic light scattering (DLS) and small angle X-ray scattering (SAXS) and compared to data derived from optical measurements. In addition to demonstrating the potential of this novel whole nanoobject approach for determining architectures of small nanoparticles, the presented results also highlight challenges faced by different sizing and structural analysis methods and method-inherent uncertainties.
The material and damage behaviour of additively manufactured polyamide 12 under cyclic loading was characterized by cyclic tests and microstructure analysis by using microscopy, X-ray refraction, and computed tomography. The results were used to determine parameters for the viscoplastic material model by Chaboche and a damage model by Gurson-Tvergaard-Needleman. The temperature was monitored during the experiments and the self-heating effect was observed. By including this effect, a higher accuracy could be achieved with the results of mechanical experiments.
Dynamic stall often occurs under conditions of simultaneous unsteady pitching and surging (e.g., rotorcraft and wind turbines), butmanymodels employ a dimensionless time base that implicitly assumes that surging is superimposed, in a quasi-steady manner, on dynamic pitching. An unsteady wind tunnel was used to examine this assumption, where a technique was developed to quantify the unsteady effects of surging on a pitching NACA 0018 airfoil. The technique involved performing multiple harmonic pitching experiments under nominally steady freestream conditions that bracketed a corresponding 50% surging amplitude (1.25 ⋅ 105 ≤ Re ≤ 3.75 ⋅ 105). By interpolating these data, unsteady-pitching/quasi-steady-surging data sets were constructed and compared with de facto synchronous pitch and surging experiments, thereby isolating the unsteady effects of surging on a pitching airfoil. Both large and small poststall maximum angles of attack (αs + 5° and αs + 15°) were considered at multiple pitch-surge phase differences. During deep dynamic stall (αs 15°), with large-scale separation, surging was seen to have a secondary effect on the unsteady aerodynamics. However, at small poststall maximum angles of attack (αs + 5°), either light or deep dynamic stall behavior was observed depending upon the pitch-surge phase difference. This was attributed to Reynolds number history effects, exemplified by boundary-layer transition, and thus it can be referred to as “transitional” dynamic stall.
The Brazilian sugarcane industry produced around 173 million tons (Mt) of bagasse in 2018. Bagasse is a by-product of juice extraction for ethanol and sugar production and is combusted in order to generate power, producing up to 10 Mt of ash per year. This ash contains various concentrations of plant nutrients, which allow the ash to be used as a crop fertilizer. However, the concentration and extractability of phosphorus (P), an essential plant nutrient, are low in bagasse ash. To increase the P content, we co-gasified and co-combusted bagasse with P-rich chicken manure. The resulting ash was thermochemically post-treated with alkali additives (Na2SO4 and K2SO4) to increase the availability of P to plants. We aimed to: (i) investigate the effect of thermochemical post-treatment of co-gasification residue and co-combustion ash on P availability to soybeans, (ii) explore the potential of chemical extraction methods (citric acid, neutral ammonium citrate, formic acid, and Mehlich-I) and diffusive gradients in thin films (DGT) to predict the availability of P to soybeans, and (iii) identify the responsible P-phases using X-ray diffraction . We evaluated P availability to soybeans growing in Brazilian Oxisol soil in two independent greenhouse pot experiments. The positive effect of thermochemical treatment on P availability from gasification residue was confirmed through the observation of increased P uptake and biomass in soybean plants. These findings were confirmed by chemical extraction methods and DGT. The gasification residue contained whitlockite as its main P-bearing phase. Thermochemical post-treatment converted whitlockite into highly soluble CaNaPO4. In contrast, co-combustion ash already contained highly soluble Ca(Na,K)PO4 as its main P-bearing phase, making thermochemical post-treatment unnecessary for increasing P availability. In conclusion, increased extractability and availability of P for soybeans were closely connected to the formation of calcium alkali phosphate. Our findings indicate that this combined methodology allows for the prediction of P-fertilization effects of ash.
Merocyanine–triarylamine bichromophores are readily synthesized by sequentially Pd-catalyzed insertion alkynylation–Michael–Suzuki four-component reactions. White-light emissive systems form upon aggregation in 1 : 99 and 0.1 : 99.9 vol% CH2Cl2–cyclohexane mixtures, ascribed to aggregation-induced dual emission (AIDE) in combination with partial energy transfer between both chromophore units as supported by spectroscopic studies.
Accurate and reproducible measurement of the structure and properties of high-value nanoparticles is extremely important for their commercialization. A significant proportion of engineered nanoparticle systems consist of some form of nominally core-shell structure, whether by design or unintentionally. Often, these do not form an ideal core-shell structure, with typical deviations including polydispersity of the core or shell, uneven or incomplete shells, noncentral cores, and others. Such systems may be created with or without intent, and in either case an understanding of the conditions for formation of such particles is desirable. Precise determination of the structure, composition, size, and shell thickness of such particles can prove challenging without the use of a suitable range of characterization techniques. Here, the authors present two such polymer core-shell nanoparticle systems, consisting of polytetrafluoroethylene cores coated with a range of thicknesses of either polymethylmethacrylate or polystyrene. By consideration of surface energy, it is shown that these particles are expected to possess distinctly differing coating structures, with the polystyrene coating being incomplete. A comprehensive characterization of these systems is demonstrated, using a selection of complementary techniques including scanning electron microscopy, scanning transmission electron microscopy, thermogravimetric analysis, dynamic light scattering, differential centrifugal sedimentation, and X-ray photoelectron spectroscopy. By combining the results provided by these techniques, it is possible to achieve superior characterization and understanding of the particle structure than could be obtained by considering results separately.
A variety of methods used to prepare nano-objects for surface analysis are described along with information about when they might be best applied. Intrinsic properties of NPs which complicate their characterization and need to be considered when planning for surface or other analyses of NPs are identified, including challenges associated with reproducible synthesis and functionalization of the particles as well as their dynamic nature. The relevant information about the sample preparation processes, along with analysis details and data that need to be added to the collection of material provenance information is identified. Examples of protocols that have been successfully used for preparation of nano-objects for surface analysis are included in an annex.