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Organisationseinheit der BAM
- 6 Materialchemie (1637) (entfernen)
Paper des Monats
- ja (16)
Low temperature functionalization of two-dimensional boron nitride for electrochemical sensing
(2019)
Two-dimensional hexagonal boron nitride(h-BN)as an emerging nanomaterial exhibits uniquephysicochemical properties, making it suitable candidate for a wide spectrum of applications.However, due to its poor functionality, the processability of this nanomaterial is low. In this work, wereport on a straightforward and scalable approach for the functionalization of h-BN by nitrene[2+1]cycloaddition at room temperature. The triazine-functionalized h-BN(Trz-BNs)showed ahigh reactivity toward nucleophiles, through which post-modifications are performable. The post-modification of Trz-BNs by L-cysteine was studied using cyclic voltammetry and differential pulsevoltammetry. Taking advantage of the scalable and straightforward functionalization as well as abilityof triazine functional groups for the controlled post-modifications, Trz-BNs is a promisingnanoplatform for a wide range of future applications.
Metal carbides have shown great promise in a wide range of applications due to their unique catalytic, electrocatalytic and magnetic properties. However, the scalable production of dispersible metal carbide nanoparticles remains a challenge. Here, we report a simple and scalable route to dispersible iron carbide (Fe3C) nanoparticles. This uses MgO nanoparticles as a removable ‘cast’ to synthesize Fe3C nanoparticles from Prussian blue (KFeIII[FeII(CN)6]). Electron tomography demonstrates how nanoparticles of the MgO cast encase the Fe3C nanoparticles to prevent sintering and agglomeration during the high-temperature synthesis. The MgO cast is readily removed with ethylenediaminetetraacetic acid (EDTA) to generate Fe3C nanoparticles that can be used to produce a colloidal ferrofluid or dispersed on a support material.
Polyether and -ester urethanes (PU) were exposed to artificial weathering at 40 °C and artificial UV radiation in a weathering chamber. In 3 parallel exposures, humidity was varied between dry, humid, and wet conditions. Material alteration was investigated by various analytical techniques like size exclusion chromatography
(SEC), liquid chromatography-infrared spectroscopy (LC-FTIR), thermal-desorption gas chromatography-mass spectrometry (TD-GC-MS), fluorescence mapping and dynamic mechanical analysis (DMA). Our results show that depending on the weathering conditions, different degradation effects can be observed. By means of SEC an initial strong decrease of the molar masses and a broadening of the mass distributions was found. After a material dependent time span this was followed by a plateau where molar mass changes were less significant. A minor moisture-dependent degradation effect was only found for polyester PU. Fluorescence measurements on two materials revealed an increase in the luminescence intensity upon weathering process reaching a saturation level after about 500 h. The changes in the optical properties observed after different exposure conditions and times were very similar. The TD-GC-MS data showed the fate of the stabilizers and antioxidant in the course of weathering. LC-FTIR measurements revealed a change in peak intensities and the ratio of urethane and carbonyl bands.
Size-exclusion chromatography (SEC) was used to monitor changes of the molecular masses of thermoplastic polyether – and polyester urethane (TPU) exposed to thermal, hydrolytic, and photo-oxidative (UV) Degradation conditions for several days. The thermal treatment was performed at elevated temperatures (100–200 °C) under oxidative (air) as well as non-oxidative (nitrogen) conditions to evaluate the specific influence of oxygen on the degradation. At higher temperatures (≥175 °C) a fast decrease of the molecular masses of both PU accompanied by a high degree of crosslinking was found. At lower temperatures (≤150 °C) the polymers remained widely unaffected by thermal degradation within the investigated degradation interval of up to two weeks. Surprisingly, the influence of oxygen (air) was found to be less distinct. In contrast to that, UV treatment at 25 °C at less than 10% rel. humidity (RH) resulted in a fast crosslinking, whereas the molecular masses of both PU decreased slower than for thermal treatments. The depth of penetration of the UV radiation was estimated using 3D printed PU samples with different thicknesses. Hydrolysis based degradation effects were less significant. Only slight molecular mass changes were detected at temperatures ≤80 °C within a time span of 14 days, while no crosslinking could be measured. Considering the degradation results at the investigated exposure parameters, it could be shown that esterbased PU in general exhibits a significant higher stability compared to ether-based materials.
Polymers of Intrinsic Microporosity (PIMs) of high performance have developed as materials with a wide application range in gas separation and other energy-related fields. Further optimization and long-term behavior of devices with PIMs require an understanding of the structure-property relationships including physical aging. In this context the glass transi-tion plays a central role, but with conventional thermal analysis a glass transition is usually not detectable for PIMs be-fore their thermal decomposition. Fast scanning calorimetry provides evidence of the glass transition for a series of PIMs, as the time scales responsible for thermal degradation and for the glass transition are decoupled by employing ultrafast heating rates of tens of thousands K s-1. The investigated PIMs were chosen considering the chain rigidity. The estimated glass transition temperatures follow the order of the rigidity of the backbone of the PIMs.
The mechanism of ternary cocrystal formation, and the potential role of intermediate binary phases, has been debated for some time. We report here the first in situ real-time monitoring of two prototypic ternary cocrystals. Our results suggest that the question is more complicated than previously considered. The mechanism of mechanochemical ternary cocrystal formation depends on the milling conditions, here the milling frequency and addition of liquid. Binary phases can form under certain conditions, but do not act as intermediates in the formation of the ternary cocrystals. Rather, binary phases are competitive with the ternary phase, and their formation appears to compete with that of the ternary components. The presence of binary phases leads to an increase in the overall reaction time. The results reported here offer the first insights into the true complexities of mechanochemical multi-component synthesis of higher order multi-component crystals and demonstrate a new understanding of the influence of milling condition for the study of mechanisms and kinetics.
Structural modularity of polymer frameworks is a key advantage of covalent organic polymers, however, only C, N, O, Si and S have found their way into their building blocks so far. Here, we expand the toolbox available to polymer and materials chemists by one additional nonmetal, phosphorus. Starting with a building block that contains a λ⁵‐phosphinine (C₅P) moiety, we evaluate a number of polymerisation protocols, finally obtaining a π‐conjugated, covalent phosphinine‐based framework (CPF‐1) via Suzuki‐Miyaura coupling. CPF‐1 is a weakly porous polymer glass (72.4 m2 g‐1 N2 BET at 77 K) with green fluorescence (λmax 546 nm) and extremely high thermal stability. The polymer catalyzes hydrogen evolution from water under UV and visible light irradiation without the need for additional co‐catalyst at a rate of 33.3 μmol h‐¹ g‐¹. Our results demonstrate for the first time the incorporation of the phosphinine motif into a complex polymer framework. Phosphinine‐based frameworks show promising electronic and optical properties that might spark future interest in their applications in light‐emitting devices and heterogeneous catalysis.
The movement of the macroscopic magnetic moment in ferromagnetic systems can be described by the Landau-Lifshitz (LL) or Landau-Lifshitz-Gilbert (LLG) equation. These equations are strictly valid only at absolute zero temperature. To include temperature effects a stochastic version of the LL or LLG equation for a spin density of one per unit cell can be used instead. To apply the stochastic LL to micromagnetic simulations, where the spin density per unit cell is generally higher, a conversion regarding simulation cell size and temperature has to be established. Based on energetic considerations, a conversion for ferromagnetic bulk and thin film systems is proposed. The conversion is tested in micromagnetic simulations which are performed with the Object Oriented Micromagnetic Framework (OOMMF). The Curie temperatures of bulk Nickel, Cobalt and Iron systems as well as Nickel thin-film systems with thicknesses between 6.3 mono layer (ML) and 31ML are determined from micromagnetic simulations. The results show a good agreement with experimentally determined Curie temperatures of bulk and thin film systems when temperature scaling is performed according to the presented model.
In September 2018, the First European Workshop on Metal Phosphonates Chemistry brought together some prominent researchers in the field of metal phosphonates and phosphinates with the aim of discussing past and current research efforts and identifying future directions. The scope of this perspective article is to provide a critical overview of the topics discussed during the workshop, which are divided into two main areas: synthesis and characterisation, and applications. In terms of synthetic methods, there has been a push towards cleaner and more efficient approaches. This has led to the introduction of high-throughput synthesis and mechanochemical synthesis. The recent success of metal–organic frameworks has also promoted renewed interest in the synthesis of porous metal phosphonates and phosphinates. Regarding characterisation, the main advances are the development of electron diffraction as a tool for crystal structure determination and the deployment of in situ characterisation techniques, which have allowed for a better understanding of reaction pathways. In terms of applications, metal phosphonates have been found to be suitable materials for several purposes: they have been employed as heterogeneous catalysts for the synthesis of fine chemicals, as solid sorbents for gas separation, notably CO2 capture, as materials for electrochemical devices, such as fuel cells and rechargeable batteries, and as matrices for drug delivery.
In der DIN EN ISO 14577 Metallische Werkstoffe – Instrumentierte Eindringprüfung zur Bestimmung der Härte und anderer Werkstoffparameter sind die Durchführung und Auswertung des Verfahrens, sowie die Kalibrierung der zu verwendenden Prüfmaschine genormt. In dieser Norm werden auch grundsätzliche Aussagen zur Bestimmung der Messunsicherheit gemacht.
An Beispielen aus der täglichen Prüfpraxis werden verschiedene Möglichkeiten, aber auch die Grenzen der Bestimmung der Messunsicherheitbei der Instrumentierten Eindringprüfung beschrieben und kritisch diskutiert.