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Year of publication
Document Type
- Article (2238) (remove)
Language
- English (2238) (remove)
Is part of the Bibliography
- yes (2238)
Keywords
- Conformational analysis (14)
- biomaterials (13)
- nanoparticles (13)
- fluorescence (12)
- Palladium (11)
- photochemistry (11)
- singlet oxygen (11)
- Fluorescence (10)
- SERS (10)
- block copolymers (10)
Institute
- Institut für Chemie (2238) (remove)
Hybrid nanophotonic elements, fabricated by organic and inorganic materials, are going to be key components of modern devices.
Coupled systems of photoemitters with a plasmonic waveguide serve the demand for nanoscopic frequency converters.
However, processes like the degradation of the photoemitters via photobleaching occur and need to be monitored and controlled, to realize future successful devices.
We introduce a hybrid perylene-diimide / silver nanowire as plasmon frequency converter. A versatile method is presented to monitor and analyze the bleaching process. It is based on a time series of photoluminescence images, during the operation of a single converter.
An analytical model is applied on the data and unveils that the photobleaching rate is constant and independent of the operation of the plasmon converter.
Lanthanide based ceria nanomaterials are important practical materials due to the redox properties that are useful in the avenues pertaining to technology and life sciences. Sub 10 nm spherical and highly monodisperse Ce1−xYbxO2−y (0.04 ≤ x ≤ 0.22) nanoparticles were synthesized by thermal decomposition, annealed separately at 773 K and 1273 K for 2 hours and characterized. Elemental mapping for Yb3+ doped ceria nanoparticles shows homogeneous distribution of Yb3+ atoms in the ceria with low Yb3+ content annealed at 773 K and 1273 K for 2 hours. However, clusters are observed for 773 K annealed ceria samples with high concentration of Yb3+. These clusters are not detected in 1273 K annealed nanomaterials. Introducing small amounts of Yb3+ ions into the ceria lattice as spectroscopic probes can provide detailed information about the atomic structure and local environments allowing the monitoring of small structural changes, such as clustering. The emission spectra observed at room temperature and at 4 K have a manifold of bands that corresponds to the 2F5/2 → 2F7/2 transition of Yb3+ ions. Some small shifts are observed in the Stark splitting pattern depending on the sample and the annealing conditions. The deconvolution by PARAFAC analysis yielded luminescence decay kinetics as well as the associated luminescence spectra of three species for each of the low Yb3+ doped ceria samples annealed at 773 K and one species for the 1273 K annealed samples. However, the ceria samples with high concentration of Yb3+ annealed at the two temperatures showed only one species with lower decay times as compared to the low Yb3+ doped ceria samples.
Photo-iniferter (PI)-RAFT polymerization, the direct activation of chain transfer agents via light, is a fascinating polymerization technique, as it overcomes some restriction of conventional RAFT polymerization.
As such, we elucidated the role of reversible deactivation in this context using a monomer-CTA pair with low chain transfer capabilities.
Tests with varying targeted degrees of polymerization (DP) or monomer concentrations revealed no significant improvement of polymerization control using the PI-process. Control can however be achieved via slow monomer addition, increasing the number of activation/deactivation events per monomer addition.
More importantly, the livingness of the polymerization was found to be extraordinarily high, enabling the straightforward and rapid synthesis of multiblock copolymers with up to 20 blocks and a high number of repeating units per block (DP = 25-100) maintaining an overall excellent definition (M-n = 90 300 g mol(-1), D = 1.29).
This study highlights the enormous potential of PI-RAFT polymerization for the synthesis of polymeric materials.
Mechanism comics as a task in a written exam in organic chemistry for pre-service chemistry teachers
(2022)
In this paper, we describe and evaluate a study on the use of mechanism comics for writing solutions to a task in a written exam for the course "Organic Chemistry I for Pre-Service Chemistry Teachers."
The students had to design a reaction mechanism for a reaction that was unknown to them and write captions explaining every step of their reaction mechanism.
The students' work was evaluated using the method of qualitative content analysis in four rounds by both authors. The majority of the captions were coded as "descriptive" and only a minority as "causal."
This means that the students mostly described "what" happened, but seldom "why" this happened. Implicit electron movement was also described more often than explicit electron movement. The majority of the captions were technically correct. In summary, the students were capable of designing and describing a reaction mechanism for a previously unknown reaction.
The quality of their reasoning could be improved, however. In the new course, the quality of students' mechanistic reasoning and then especially their explanations of "why" mechanistic steps occur will be given much clearer emphasis.
Azobenzene is a prototypical molecular photoswitch, widely used to trigger a variety of transformations at different length scales.
In systems like self-assembled monolayers or micelles, azobenzene chromophores may interact with each other, which gives rise to the emergence of exciton states.
Here, using first-principles calculations, we investigate how conformational disorder (induced, e.g., by thermal fluctuations) affects localization of these states, on an example of an H-type azobenzene tetramer.
We find that conformational disorder leads to (partial) exciton localization on a single-geometry level, whereas ensemble-averaging results in a delocalized picture. The pi pi* and n pi* excitons at high and low temperatures are discussed.
The regioselectivity of two mechanistically distinct alkenylation reactions catalyzed by in situ-formed cationic transition metal complexes was studied using
N-allyl-N-phenylethenesulfonamide as a model compound.
Orthogonal selectivity was observed for the Ru-catalyzed C-H-activating alkenylation with acetanilides, which occurs preferentially at the electron deficient double bond, and for a Pd-catalyzed Heck-type coupling with arene diazonium salts, which occurs preferentially at the more electron rich double bond of the N-allyl substituent.
The quantification and identification of aerosols in industry plays a key role in process monitoring and control and lays the foundation for process automation aspired by the industry 4.0 initiative.
However, measuring particulate matter's mass and number concentrations in harsh environments poses great analytical constraints.
The presented approach comprises a comprehensive set of light-and imaging-based techniques, all contactless, in-line, and real-time. It includes, but is not limited to, stroboscopic imaging, laser-induced breakdown spectroscopy (LIBS) and laser-induced incandescence (LII). Stroboscopic imaging confirmed the particles sphericity and was used to measure the particle number density. A phase-selective LIBS setup with low fluence and 500 Hz repetition rate was used to classify each particle with a single-pulse and in real time. Simultaneously, the created plasma was captured by CCD imaging to determine the detection volume and hit rate of the LIBS setup.
Both data sets combined were converted to a particle number density, which was consistent with the particle number density of the stroboscopic measurements. Furthermore, using a photodiode and microphone in parallel to the LIBS setup allowed for the photoacoustic normalization of the spectral line intensity at the laser repetition rate of 500 Hz.
This was done as a partial photoacoustic normalization method with the cut-off based on the coefficient of variation (CV), reducing it by 25%. Aside from that photodiode and microphone were proven to be valuable event counting with the advantage of the less spatially constricted. A second laser setup was used for laser -induced incandescence (LII) making it possible to classify the particles based on their incandescence tendency. Given its larger probing volume, LII could be employed at very low particle number densities.
With respect to the current literature, this is the first approach of using LII as an in-line, real-time analytical technique for the compositional classification of metal-bearing aerosols.
We report on the triplet sensitization of the intramolecular Photo-Dehydro-Diels-Alder (PDDA) reaction of two diaryl suberates bearing methyl propiolate chromophors. Compared with the non-sensitized irradiation, considerably increased yields could be observed.
Moreover, it is possible to use the more efficient UVA lamps instead of UVB lamps.
Among three investigated sensitizers (xanthone, benzophenone, thioxanthone) xanthone gave the best results.
Low-energy (5-20 eV) electron-induced single and double strand breaks in well-defined DNA sequences
(2022)
Ionizing radiation is used in cancer radiation therapy to effectively damage the DNA of tumors. The main damage is due to generation of highly reactive secondary species such as low-energy electrons (LEEs). The accurate quantification of DNA radiation damage of well-defined DNA target sequences in terms of absolute cross sections for LEE-induced DNA strand breaks is possible by the DNA origami technique; however, to date, it is possible only for DNA single strands. In the present work DNA double strand breaks in the DNA sequence 5 '-d(CAC)4/5 ' d(GTG)4 are compared with DNA single strand breaks in the oligonucleotides 5 '-d(CAC)4 and 5 '-d(GTG)4 upon irradiation with LEEs in the energy range from 5 to 20 eV. A maximum of strand break cross section was found around 7 and 10 eV independent of the DNA sequence, indicating that dissociative electron attachment is the underlying mechanism of strand breakage and confirming previous studies using plasmid DNA.
Erler, Alexander ; Riebe, Daniel ; Beitz, Toralf ; Löhmannsröben, Hans-Gerd ; Leenen, Mathias ; Pätzold, Stefan ; Ostermann, Markus ; Wójcik, Michał
In precision agriculture, the estimation of soil parameters via sensors and the creation of nutrient maps are a prerequisite for farmers to take targeted measures such as spatially resolved fertilization. In this work, 68 soil samples uniformly distributed over a field near Bonn are investigated using laser-induced breakdown spectroscopy (LIBS). These investigations include the determination of the total contents of macro- and micronutrients as well as further soil parameters such as soil pH, soil organic matter (SOM) content, and soil texture. The applied LIBS instruments are a handheld and a platform spectrometer, which potentially allows for the single-point measurement and scanning of whole fields, respectively. Their results are compared with a high-resolution lab spectrometer. The prediction of soil parameters was based on multivariate methods. Different feature selection methods and regression methods like PLS, PCR, SVM, Lasso, and Gaussian processes were tested and compared. While good predictions were obtained for Ca, Mg, P, Mn, Cu, and silt content, excellent predictions were obtained for K, Fe, and clay content. The comparison of the three different spectrometers showed that although the lab spectrometer gives the best results, measurements with both field spectrometers also yield good results. This allows for a method transfer to the in-field measurements.
Efficient Removal of Tetracycline and Bisphenol A from Water with a New Hybrid Clay/TiO2 Composite
(2023)
Adesina, Morenike O. ; Block, Inga ; Günter, Christina ; Unuabonah, Emmanuel Iyayi ; Taubert, Andreas
New TiO2 hybrid composites were prepared fromkaolinclay, predried and carbonized biomass, and titanium tetraisopropoxideand explored for tetracycline (TET) and bisphenol A (BPA) removalfrom water. Overall, the removal rate is 84% for TET and 51% for BPA.The maximum adsorption capacities (q (m))are 30 and 23 mg/g for TET and BPA, respectively. These capacitiesare far greater than those obtained for unmodified TiO2. Increasing the ionic strength of the solution does not change theadsorption capacity of the adsorbent. pH changes only slightly changeBPA adsorption, while a pH > 7 significantly reduces the adsorptionof TET on the material. The Brouers-Sotolongo fractal modelbest describes the kinetic data for both TET and BPA adsorption, predictingthat the adsorption process occurs via a complex mechanism involvingvarious forces of attraction. Temkin and Freundlich isotherms, whichbest fit the equilibrium adsorption data for TET and BPA, respectively,suggest that adsorption sites are heterogeneous in nature. Overall,the composite materials are much more effective for TET removal fromaqueous solution than for BPA. This phenomenon is assigned to a differencein the TET/adsorbent interactions vs the BPA/adsorbent interactions:the decisive factor appears to be favorable electrostatic interactionsfor TET yielding a more effective TET removal.
Graphene is well-knownfor its unique combination of electricaland mechanical properties. However, its vanishing band gap limitsthe use of graphene in microelectronics. Covalent functionalizationof graphene has been a common approach to address this critical issueand introduce a band gap. In this Article, we systematically analyzethe functionalization of single-layer graphene (SLG) and bilayer graphene(BLG) with methyl (CH3) using periodic density functionaltheory (DFT) at the PBE+D3 level of theory. We also include a comparisonof methylated single-layer and bilayer graphene, as well as a discussionof different methylation options (radicalic, cationic, and anionic).For SLG, methyl coverages ranging from 1/8 to 1/1, (i.e.,the fully methylated analogue of graphane) are considered. We findthat up to a coverage theta of 1/2, graphene readily accepts CH3, with neighbor CH3 groups preferring trans positions. Above theta = 1/2, the tendency to accept further CH3 weakens and the lattice constant increases. The band gapbehaves less regularly, but overall it increases with increasing methylcoverage. Thus, methylated graphene shows potential for developingband gap-tuned microelectronics devices and may offer further functionalizationoptions. To guide in the interpretation of methylation experiments,vibrational signatures of various species are characterized by normal-modeanalysis (NMA), their vibrational density of states (VDOS), and infrared(IR) spectra, the latter two are obtained from ab initio moleculardynamics (AIMD) in combination with a velocity-velocity autocorrelationfunction (VVAF) approach.
Geometry, 11B, 13C chemical shifts and the spatial magnetic properties (Through-Space NMR Shieldings -TSNMRS) of both cations and anions of boron-trapped N-heterocyclic carbenes (NHCs) and cyclic (alkyl)(amino)carbenes (CAACs) and of the corresponding diborane/diborene/diboryne dis-carbene adducts have been calculated using the GIAO perturbation method employing the nucleus independent chemical shift (NICS) concept; the TSNMRS results are visualized as iso-chemical-shielding surfaces (ICSS) of various size and direction. The ICSS of the TSNMRS (actually the anisotropy effects measurable in 1H NMR spectroscopy) are employed to qualify and quantify the present multiple bond character of the Carbene-Boron bond in the trapped NHCs and CAACs. Results are confirmed by bond length and 11B/13C chemical shift variations. Thus the partial multiple bond character of the Carbene-Boron bond cannot be expressed by the arrow of weak, much longer dative bonds and should be omitted as in other covalent lone pair-it or triel bonds. & COPY; 2023 Elsevier Ltd. All rights reserved.
High-solid-content polystyrene and polyvinyl acetate dispersions of polymer particles with a 50 nm to 500 nm mean particle diameter and 12-55% (w/w) solid content have been produced via emulsion polymerization and characterized regarding their optical and physical properties. Both systems have been analyzed with common particle-size-measuring techniques like dynamic light scattering (DLS) and static light scattering (SLS) and compared to inline particle size distribution (PSD) measurements via photon density wave (PDW) spectroscopy in undiluted samples. It is shown that particle size measurements of undiluted polystyrene dispersions are in good agreement between analysis methods. However, for polyvinyl acetate particles, size determination is challenging due to bound water in the produced polymer. For the first time, water-swelling factors were determined via an iterative approach of PDW spectroscopy error (X-2) minimization. It is shown that water-swollen particles can be analyzed in high-solid-content solutions and their physical properties can be assumed to determine the refractive index, density, and volume fraction in dispersion. It was found that assumed water swelling improved the reduced scattering coefficient fit by PDW spectroscopy by up to ten times and particle size determination was refined and enabled. Particle size analysis of the water-swollen particles agreed well with offline-based state-of-the-art techniques.
Xu, Yaolin ; Dong, Kang ; Jie, Yulin ; Adelhelm, Philipp ; Chen, Yawei ; Xu, Liang ; Yu, Peiping ; Kim, Junghwa ; Kochovski, Zdravko ; Yu, Zhilong ; Li, Wanxia ; LeBeau, James ; Shao-Horn, Yang ; Cao, Ruiguo ; Jiao, Shuhong ; Cheng, Tao ; Manke, Ingo ; Lu, Yan
In recent years, due to its great promise in boosting the energy density of lithium batteries for future energy storage, research on the Li metal anode, as an alternative to the graphite anode in Li-ion batteries, has gained significant momentum. However, the practical use of Li metal anodes has been plagued by unstable Li (re)deposition and poor cyclability. Although tremendous efforts have been devoted to the stabilization of Li metal anodes, the mechanisms of electrochemical (re-)deposition/dissolution of Li and solid-electrolyte-interphase (SEI) formation remain elusive. This article highlights the recent mechanistic understandings and observations of Li deposition/dissolution and SEI formation achieved from advanced characterization techniques and simulation methods, and discusses major limitations and open questions in these processes. In particular, the authors provide their perspectives on advanced and emerging/potential methods for obtaining new insights into these questions. In addition, they give an outlook into cutting-edge interdisciplinary research topics for Li metal anodes. It pushes beyond the current knowledge and is expected to accelerate development toward a more in-depth and comprehensive understanding, in order to guide future research on Li metal anodes toward practical application.
Self-assembly of plasmonic nanoantenna-waveguide structures for subdiffractional chiral sensing
(2021)
Rothe, Martin ; Zhao, Yuhang ; Müller, Johannes ; Kewes, Günter ; Koch, Christoph T. ; Lu, Yan ; Benson, Oliver
Spin-momentum locking is a peculiar effect in the near-field of guided optical or plasmonic modes. It can be utilized to map the spinning or handedness of electromagnetic fields onto the propagation direction. This motivates a method to probe the circular dichroism of an illuminated chiral object. In this work, we demonstrate local, subdiffraction limited chiral coupling of light and propagating surface plasmon polaritons in a self-assembled system of a gold nanoantenna and a silver nanowire. A thin silica shell around the nanowire provides precise distance control and also serves as a host for fluorescent molecules, which indicate the direction of plasmon propagation. We characterize our nanoantenna-nanowire systems comprehensively through correlated electron microscopy, energy-dispersive X-ray spectroscopy, dark-field, and fluorescence imaging. Three-dimensional numerical simulations support the experimental findings. Besides our measurement of far-field polarization, we estimate sensing capabilities and derive not only a sensitivity of 1 mdeg for the ellipticity of the light field, but also find 10(3) deg cm(2)/dmol for the circular dichroism of an analyte locally introduced in the hot spot of the antenna-wire system. Thorough modeling of a prototypical design predicts on-chip sensing of chiral analytes. This introduces our system as an ultracompact sensor for chiral response far below the diffraction limit.
Ning, Jiaoyi ; Yu, Hongtao ; Mei, Shilin ; Schütze, Yannik ; Risse, Sebastian ; Kardjilov, Nikolay ; Hilger, André ; Manke, Ingo ; Bande, Annika ; Ruiz, Victor G. ; Dzubiella, Joachim ; Meng, Hong ; Lu, Yan
Herein, the concept of constructing binder- and carbon additive-free organosulfur cathode was proved based on thiol-containing conducting polymer poly(4-(thiophene-3-yl) benzenethiol) (PTBT). The PTBT featured the polythiophene-structure main chain as a highly conducting framework and the benzenethiol side chain to copolymerize with sulfur and form a crosslinked organosulfur polymer (namely S/PTBT). Meanwhile, it could be in-situ deposited on the current collector by electro-polymerization, making it a binder-free and free-standing cathode for Li-S batteries. The S/PTBT cathode exhibited a reversible capacity of around 870 mAh g(-1) at 0.1 C and improved cycling performance compared to the physically mixed cathode (namely S&PTBT). This multifunction cathode eliminated the influence of the additives (carbon/binder), making it suitable to be applied as a model electrode for operando analysis. Operando X-ray imaging revealed the remarkable effect in the suppression of polysulfides shuttle via introducing covalent bonds, paving the way for the study of the intrinsic mechanisms in Li-S batteries.
Lau, Skadi ; Liu, Yue ; Maier, Anna ; Braune, Steffen ; Gossen, Manfred ; Neffe, Axel T. ; Lendlein, Andreas
In vitro thrombogenicity test systems require co-cultivation of endothelial cells and platelets under blood flow-like conditions. Here, a commercially available perfusion system is explored using plasma-treated cyclic olefin copolymer (COC) as a substrate for the endothelial cell layer. COC was characterized prior to endothelialization and co-cultivation with platelets under static or flow conditions. COC exhibits a low roughness and a moderate hydrophilicity. Flow promoted endothelial cell growth and prevented platelet adherence. These findings show the suitability of COC as substrate and the importance of blood flow-like conditions for the assessment of the thrombogenic risk of drugs or cardiovascular implant materials.
Neusser, David ; Sun, Bowen ; Tan, Wen Liang ; Thomsen, Lars ; Schultz, Thorsten ; Perdigon-Toro, Lorena ; Koch, Norbert ; Shoaee, Safa ; McNeill, Christopher R. ; Neher, Dieter ; Ludwigs, Sabine
Recent advances in organic solar cell performance have been mainly driven forward by combining high-performance p-type donor-acceptor copolymers (e.g.PM6) and non-fullerene small molecule acceptors (e.g.Y6) as bulk-heterojunction layers. A general observation in such devices is that the device performance, e.g., the open-circuit voltage, is strongly dependent on the processing solvent. While the morphology is a typically named key parameter, the energetics of donor-acceptor blends are equally important, but less straightforward to access in the active multicomponent layer. Here, we propose to use spectral onsets during electrochemical cycling in a systematic spectroelectrochemical study of blend films to access the redox behavior and the frontier orbital energy levels of the individual compounds. Our study reveals that the highest occupied molecular orbital offset (Delta E-HOMO) in PM6:Y6 blends is similar to 0.3 eV, which is comparable to the binding energy of Y6 excitons and therefore implies a nearly zero driving force for the dissociation of Y6 excitons. Switching the PM6 orientation in the blend films from face-on to edge-on in bulk has only a minor influence on the positions of the energy levels, but shows significant differences in the open circuit voltage of the device. We explain this phenomenon by the different interfacial molecular orientations, which are known to affect the non-radiative decay rate of the charge-transfer state. We compare our results to ultraviolet photoelectron spectroscopy data, which shows distinct differences in the HOMO offsets in the PM6:Y6 blend compared to neat films. This highlights the necessity to measure the energy levels of the individual compounds in device-relevant blend films.
Structure, mechanical properties and degradation behavior of electrospun PEEU fiber meshes and films
(2021)
The capability of a degradable implant to provide mechanical support depends on its degradation behavior. Hydrolytic degradation was studied for a polyesteretherurethane (PEEU70), which consists of poly(p-dioxanone) (PPDO) and poly(epsilon-caprolactone) (PCL) segments with a weight ratio of 70:30 linked by diurethane junction units. PEEU70 samples prepared in the form of meshes with average fiber diameters of 1.5 mu m (mesh1.5) and 1.2 mu m (mesh1.2), and films were sterilized and incubated in PBS at 37 degrees C with 5 vol% CO2 supply for 1 to 6 weeks. Degradation features, such as cracks or wrinkles, became apparent from week 4 for all samples. Mass loss was found to be 11 wt%, 6 wt%, and 4 wt% for mesh1.2, mesh1.5, and films at week 6. The elongation at break decreased to under 20% in two weeks for mesh1.2. In case of the other two samples, this level of degradation was achieved after 4 weeks. The weight average molecular weight of both PEEU70 mesh and film samples decreased to below 30 kg/mol when elongation at break dropped below 20%. The time period of sustained mechanical stability of PEEU70-based meshes depends on the fiber diameter and molecular weight.