Institut für Chemie
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Microwave-Assisted Synthesis of 5 '-O-methacryloylcytidine Using the Immobilized Lipase Novozym 435
(2022)
Nucleobase building blocks have been demonstrated to be strong candidates when it comes to DNA/RNA-like materials by benefiting from hydrogen bond interactions as physical properties. Modifying at the 5 ' position is the simplest way to develop nucleobase-based structures by transesterification using the lipase Novozym 435. Herein, we describe the optimization of the lipase-catalyzed synthesis of the monomer 5 '-O-methacryloylcytidine with the assistance of microwave irradiation. Variable reaction parameters, such as enzyme concentration, molar ratio of the substrate, reaction temperature and reaction time, were investigated to find the optimum reaction condition in terms of obtaining the highest yield.
Enzymes can support the synthesis or degradation of biomacromolecules in natural processes. Here, we demonstrate that enzymes can induce a macroscopic-directed movement of microstructured hydrogels following a mechanism that we call a "Jack-in-the-box" effect. The material's design is based on the formation of internal stresses induced by a deformation load on an architectured microscale, which are kinetically frozen by the generation of polyester locking domains, similar to a Jack-in-thebox toy (i.e., a compressed spring stabilized by a closed box lid). To induce the controlled macroscopic movement, the locking domains are equipped with enzyme-specific cleavable bonds (i.e., a box with a lock and key system). As a result of enzymatic reaction, a transformed shape is achieved by the release of internal stresses. There is an increase in entropy in combination with a swelling-supported stretching of polymer chains within the microarchitectured hydrogel (i.e., the encased clown pops-up with a pre-stressed movement when the box is unlocked). This utilization of an enzyme as a physiological stimulus may offer new approaches to create interactive and enzyme-specific materials for different applications such as an optical indicator of the enzyme's presence or actuators and sensors in biotechnology and in fermentation processes.
Lanthanide based ceria nanomaterials are important practical materials due to their redox properties that are useful in technology and life sciences. This PhD thesis examined various properties and potential for catalytic and bio-applications of Ln3+-doped ceria nanomaterials. Ce1-xGdxO2-y: Eu3+, gadolinium doped ceria (GDC) (0 ≤ x ≤ 0.4) nanoparticles were synthesized by flame spray pyrolysis (FSP) and studied, followed by 15 % CexZr1-xO2-y: Eu3+|YSZ (0 ≤ x ≤ 1) nanocomposites. Furthermore, Ce1-xYb xO2-y (0.004 ≤ x ≤ 0.22) nanoparticles were synthesized by thermal decomposition and characterized. Finally, CeO2-y: Eu3+ nanoparticles were synthesized by a microemulsion method, biofunctionalized and characterized. The studies undertaken presents a novel approach to structurally elucidate ceria-based nanomaterials by way of Eu3+ and Yb3+ spectroscopy and processing the spectroscopic data with the multi-way decomposition method PARAFAC. Data sets of the three variables: excitation wavelength, emission wavelength and time were used to perform the deconvolution of spectra.
GDC nanoparticles from FSP are nano-sized and of roughly cubic shape and crystal structure (Fm3̅m). Raman data revealed four vibrational modes exhibited by Gd3+ containing samples whereas CeO2-y: Eu3+ displays only two. The room temperature, time-resolved emission spectra recorded at λexcitation = 464 nm show that Gd3+ doping results in significantly altered emission spectra compared to pure ceria. The PARAFAC analysis for the pure ceria samples reveals two species; a high-symmetry species and a low-symmetry species. The GDC samples yield two low-symmetry spectra in the same experiment. High-resolution emission spectra recorded at 4 K after probing the 5D0-7F0 transition revealed additional variation in the low symmetry Eu3+ sites in pure ceria and GDC. The data of the Gd3+-containing samples indicates that the average charge density around the Eu3+ ions in the lattice is inversely related to Gd3+ and oxygen vacancy concentration.
The particle crystallites of the 773 K and 1273 K annealed Yb3+ -ceria nanostructure materials are nano-sized and have a cubic fluorite structure with four Raman vibrational modes. Elemental maps clearly show that cluster formation occurs for 773 K annealed with high Yb3+ ion concentration from 15 mol % in the ceria lattice. These clusters are destroyed with annealing to 1273 K. The emission spectra observed from room temperature and 4 K measurements for the Ce1-xYb xO2-y samples have a manifold that corresponds to the 2F5/2-2F7/2 transition of Yb3+ ions. Some small shifts are observed in the Stark splitting pattern and are induced by the variations of the crystal field influenced by where the Yb3+ ions are located in the crystal lattices in the samples. Upon mixing ceria with high Yb3+ concentrations, the 2F5/2-2F7/2 transition is also observed in the Stark splitting pattern, but the spectra consist of two broad high background dominated peaks. Annealing the nanomaterials at 1273 K for 2 h changes the spectral signature as new peaks emerge. The deconvolution yielded luminescence decay kinetics as well as the accompanying 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 Yb3+ concentration annealed at the two temperatures yielded one species with lower decay times as compared to the Yb3+ doped ceria samples after PARAFAC analysis.
Through the calcination of the nanocomposites at two high temperatures, the evolution of the emission patterns from specific Eu3+ lattice sites to indicate structural changes for the nanocomposites was followed. The spectroscopy results effectively complemented the data obtained from the conventional techniques. Annealing the samples at 773 K, resulted in amorphous, unordered domains whereas the TLS of the 1273 K nanocomposites reveal two distinct sites, with most red shifted Eu3+ species coming from pure Eu3+ doped ZrO2 on the YSZ support.
Finally, for Eu3+ doped ceria, successful transfer from hydrophobic to water phase and subsequent biocompatibility was achieved using ssDNA. PARAFAC analysis for the Eu3+ in nanoparticles dispersed in toluene and water revealed one Eu3+ species, with slightly differing surface properties for the nanoparticles as far as the luminescence kinetics and solvent environments were concerned. Several functionalized nanoparticles conjugated onto origami triangles after hybridization were visualized by atomic force microscopy (AFM). Putting all into consideration, Eu3+ and Yb3+ spectroscopy was used to monitor the structural changes and determining the feasibility of the nanoparticle transfer into water. PARAFAC proves to be a powerful tool to analyze lanthanide spectra in crystalline solid materials and in solutions, which are characterized by numerous Stark transitions and where measurements usually yield a superposition of different emission contributions to any given spectrum.
Hydrogel forming physical networks based on gelatin are an attractive approach toward multifunctional biomaterials with the option of reshaping, self-healing, and stimuli-sensitivity. However, it is challenging to design such gelatin-based hydrogels to be stable at body temperature. Here, gelatin functionalized with desaminotyrosine (DAT) or desaminotyrosyl tyrosine (DATT) side chains is crosslinked with cyclodextrin (CD) dimers under formation of inclusions complexes. The supramolecular networks displayed at room temperature decreased water uptake (200-600 wt% for DAT-based systems, 200 wt% for DATT based systems), and increased storage moduli up to 25.6 kPa determined by rheology compared to DAT(T) gelatin. The gel-sol transition temperature increased from 33 up to 42 degrees C. The presented system that is completely based on natural building blocks may form the basis for materials that may potentially respond by dissolution or changes of properties to changes in environmental conditions or to the presence of CD guest molecules.
Fifteen N-butylpyridinium salts - five monometallic [C4Py](2)[MBr4] and ten bimetallic [C4Py](2)[(M0.5M0.5Br4)-M-a-Br-b] (M=Co, Cu, Mn, Ni, Zn) - were synthesized, and their structures and thermal and electrochemical properties were studied. All the compounds are ionic liquids (ILs) with melting points between 64 and 101 degrees C. Powder and single-crystal X-ray diffraction show that all ILs are isostructural. The electrochemical stability windows of the ILs are between 2 and 3 V. The conductivities at room temperature are between 10(-5) and 10(-6) S cm(-1). At elevated temperatures, the conductivities reach up to 10(-4) S cm(-1) at 70 degrees C. The structures and properties of the current bromide-based ILs were also compared with those of previous examples using chloride ligands, which illustrated differences and similarities between the two groups of ILs.
A simple experimental setup for temperature dependent mass spectrometric measurements has been constructed. It consists of a heated sample chamber and a mass spectrometer and allows for measurements under inert gas and ambient air. Based on initial measurements on two extruded polystyrene (XPS) samples a methodology for the data analysis has been developed. With this methodology the outgassing temperature of volatile compounds, which were used as blowing agents, has been identified. Furthermore, the composition of the blowing agents has been analyzed by temperature dependent mass spectra. The results indicate the use of ambient air in one material and a mixture of the banned blowing agents R142b and R22, both hydrochlorofluorocarbons (HCFC), in the other material. The here described methodology provides an easy to use approach to identify such compounds, for example as part of environmental or quality control.
A multi-component particle system was developed that combines the properties of white color, white light emission and strong magnetism on the macroscopic and microscopic scale. The system is constituted by combination of an inorganic white core with either hard or soft magnetic properties and a white light emitting MOF. The key towards this achievement is the supraparticulate character constituted by a magnetic core, of either magnetite or alpha-Fe, surrounded by titania and silica nanoparticles of a certain size in a loose structural shell-arrangement as white components and finally the white light emitting metal-organic framework (MOF) EuTb@IFP-1 as building blocks of a core-shell structure. The supraparticles are created by forced assembly of the inorganic compounds and by combining spray-drying and postsynthetic modification by solvothermal chemistry. Thereby, the gap is bridged that homogenous compounds are either strongly magnetic, white in appearance or white light emitting. The composites presented herein inherit these properties intrinsically as electronic properties. The white characteristics are based on all optical properties that enable white: light reflection, refraction, and light emission. This work shifts the paradigm that strong magnetic materials are always expected to be intrinsically dark.
The present work focuses on the preparation and characterisation of various nanoplastic reference material candidates. Nanoplastics are plastic particles in a size range of 1 − 1000 nm. The term has emerged in recent years as a distinction from the larger microplastic (1 − 1000 μm). Since the properties of the two plastic particles differ significantly due to their size, it is important to have nanoplastic reference material. This was produced for the polymer types polypropylene (PP) and polyethylene (PE) as well as poly(lactic acid) (PLA).
A top-down method was used to produce the nanoplastic for the polyolefins PP and PE (Section 3.1). The material was crushed in acetone using an Ultra-Turrax disperser and then transferred to water. This process produces reproducible results when repeated, making it suitable for the production of a reference material candidate. The resulting dispersions were investigated using dynamic and electrophoretic light scattering. The dispersion of PP particles gave a mean hydrodynamic diameter Dh = 180.5±5.8 nm with a PDI = 0.08±0.02 and a zeta potential ζ = −43.0 ± 2.0 mV. For the PE particles, a diameter Dh = 344.5 ± 34.6 nm, with a PDI = 0.39 ± 0.04 and a zeta potential of ζ = −40.0 ± 4.2 mV was measured. This means that both dispersions are nanoplastics, as the particles are < 1000 nm. Furthermore, the starting material of these polyolefin particles was mixed with a gold salt and thereby the nanoplastic production was repeated in order to obtain nanoplastic particles doped with gold, which should simplify the detection of the particles.
In addition to the top-down approach, a bottom-up method was chosen for the PLA (Section 3.2). Here, the polymer was first dissolved in THF and stabilised with a surfactant. Then water was added and THF evaporated, leaving an aqueous PLA dispersion. This experiment was also investigated using dynamic light scattering and, when repeated, yielded reproducible results, i. e. an average hydrodynamic diameter of Dh = 89.2 ± 3.0 nm. Since the mass concentration of PLA in the dispersion is known due to the production method, a Python notebook was tested for these samples to calculate the number and mass concentration of nano(plastic) particles using the MALS results. Similar to the plastic produced in Section 3.1, gold was also incorporated into the particle, which was achieved by adding a dispersion of gold clusters with a diameter of D = 1.15 nm in an ionic liquid (IL) in the production process. Here, the preparation of the gold clusters in the ionic liquid 1-ethyl-3-methylimidazolium dicyanamide ([Emim][DCA]) represented the first use of an IL both as a reducing agent for gold and as a solvent for the gold clusters. Two volumes of gold cluster dispersion were added during the PLA particle synthesis. The addition of the gold clusters leads to much larger particles. The nanoPLA with 0.8% Au has a diameter of Dh = 198.0 ± 10.8 nm and the nanoPLA with 4.9% Au has a diameter of Dh = 259.1 ± 23.7 nm. First investigations by TEM imaging show that the nanoPLA particles form hollow spheres when gold clusters are added. However, the mechanism leading to these structures remains unclear.
By adding hyaluronic acid (HA) to dioctyl sodium sulfosuccinate (AOT)-stabilized gold nanotriangles (AuNTs) with an average thickness of 7.5 +/- 1 nm and an edge length of about 175 +/- 17 nm, the AOT bilayer is replaced by a polymeric HA-layer leading to biocompatible nanoplatelets. The subsequent reduction process of tetrachloroauric acid in the HA-shell surrounding the AuNTs leads to the formation of spherical gold nanoparticles on the platelet surface. With increasing tetrachloroauric acid concentration, the decoration with gold nanoparticles can be tuned. SAXS measurements reveal an increase of the platelet thickness up to around 14.5 nm, twice the initial value of bare AuNTs. HRTEM micrographs show welding phenomena between densely packed particles on the platelet surface, leading to a crumble formation while preserving the original crystal structure. Crumbles crystallized on top of the platelets enhance the Raman signal by a factor of around 20, and intensify the plasmon-driven dimerization of 4-nitrothiophenol (4-NTP) to 4,4 '-dimercaptoazobenzene in a yield of up to 50 %. The resulting crumbled nanotriangles, with a biopolymer shell and the absorption maximum in the second window for in vivo imaging, are promising candidates for biomedical sensing.
Zanthoxylum leprieurii Guill. and Perr. (Rutaceae) stem bark is used locally in Uganda for treating tuberculosis (TB) and cough-related infections. Lupeol (1), sesamin (2), trans-fagaramide (3), arnottianamide (4), (S)-marmesinin (5), and hesperidin (6) were isolated from the chloroform/methanol (1:1) extract of Z. leprieurii stem bark. Their structures were elucidated using spectroscopic techniques and by comparison with literature data. Furthermore, the extract and isolated compounds were subjected to antimycobacterial activity. The extract exhibited moderate activity against the susceptible (H(37)Rv) TB strain, but weak activity against the multidrug resistant (MDR)-TB strain with minimum inhibitory concentrations (MICs) of 586.0 and 1172.0 mu g/mL, respectively. Compound 3 (trans-fagaramide) showed significant antimycobacterial activity against the susceptible (H(37)Rv) TB strain (MIC 6 mu g/mL), but moderate activity against the MDR-TB strain (MIC 12.2 mu g/mL). Compounds 2, 5, 6, and 1 showed moderate activities against the susceptible (H(37)Rv) strain (MIC 12.2-98.0 mu g/mL) and moderate to weak activities against the MDR-TB strain (MIC 24.4-195.0 mu g/mL). This study reports for the first time the isolation of compounds 1 to 6 from the stem bark of Z leprieurii. trans-Fagaramide (3) may present a vital template in pursuit of novel and highly effective TB drugs.
Objective Due to multiple light scattering that occurs inside and between cells, quantitative optical spectroscopy in turbid biological suspensions is still a major challenge. This includes also optical inline determination of biomass in bioprocessing. Photon Density Wave (PDW) spectroscopy, a technique based on multiple light scattering, enables the independent and absolute determination of optical key parameters of concentrated cell suspensions, which allow to determine biomass during cultivation. Results A unique reactor type, called "mesh ultra-thin layer photobioreactor" was used to create a highly concentrated algal suspension. PDW spectroscopy measurements were carried out continuously in the reactor without any need of sampling or sample preparation, over 3 weeks, and with 10-min time resolution. Conventional dry matter content and coulter counter measurements have been employed as established offline reference analysis. The PBR allowed peak cell dry weight (CDW) of 33.4 g L-1. It is shown that the reduced scattering coefficient determined by PDW spectroscopy is strongly correlated with the biomass concentration in suspension and is thus suitable for process understanding. The reactor in combination with the fiber-optical measurement approach will lead to a better process management.
Surface-enhanced Raman scattering (SERS) is an effective and widely used technique to study chemical reactions induced or catalyzed by plasmonic substrates, since the experimental setup allows us to trigger and track the reaction simultaneously and identify the products. However, on substrates with plasmonic hotspots, the total signal mainly originates from these nanoscopic volumes with high reactivity and the information about the overall consumption remains obscure in SERS measurements. This has important implications; for example, the apparent reaction order in SERS measurements does not correlate with the real reaction order, whereas the apparent reaction rates are proportional to the real reaction rates as demonstrated by finite-difference time-domain (FDTD) simulations. We determined the electric field enhancement distribution of a gold nanoparticle (AuNP) monolayer and calculated the SERS intensities in light-driven reactions in an adsorbed self-assembled molecular monolayer on the AuNP surface. Accordingly, even if a high conversion is observed in SERS due to the high reactivity in the hotspots, most of the adsorbed molecules on the AuNP surface remain unreacted. The theoretical findings are compared with the hot-electron-induced dehalogenation of 4-bromothiophenol, indicating a time dependency of the hot-carrier concentration in plasmon-mediated reactions. To fit the kinetics of plasmon-mediated reactions in plasmonic hotspots, fractal-like kinetics are well suited to account for the inhomogeneity of reactive sites on the substrates, whereas also modified standard kinetics model allows equally well fits. The outcomes of this study are on the one hand essential to derive a mechanistic understanding of reactions on plasmonic substrates by SERS measurements and on the other hand to drive plasmonic reactions with high local precision and facilitate the engineering of chemistry on a nanoscale.
The base pairing property and the "melting" behavior of oligonucleotides can take advantage to develop new smart thermoresponsive and programmable materials. Complementary cytidine- (C) and guanosine- (G) based monomers were blockcopolymerized using RAFT polymerization technique with poly-(N-(2-hydroxypropyl) methacrylamide) (pHPMA) as the hydrophilic macro chain transfer agent (macro-CTA). C-C, G-G and C-G hydrogen bond interactions of blockcopolymers with respectively C and G moieties have been investigated using SEM, DLS and UV-Vis. Mixing and heating both complementary copolymers resulted in reforming new aggregates. Due to the ribose moiety of the isolated nucleoside-bearing blockcopolymers, the polarity is increased for better solubility. Self-assembly investigations of these bioinspired compounds are the crucial basis for the development of potential future drug delivery systems.
The compound [Nb6Cl14(pyrazine)(4)]center dot 2CH(2)Cl(2) (1) was investigated for its suitability as a starting compound for new ligand-supported hexanuclear niobium cluster compounds. The synthesis, stability to air and increased temperature, solubility and usability for subsequent reactions of 1, and purification and separation of the reaction products are discussed. The compounds with cluster units [Nb6Cl14L4], where L = iso-quinoline N-oxides (2), 1,1-dimethylethylenediamines (3), or thiazoles (4), and [Nb6Cl14(PEt3)(3.76)(Et3PO)(0.24)]-[Nb6Cl14(MeCN)(4)]center dot 4MeCN (5) are presented as follow-up products. The crystal structures of compounds 1-5 are analyzed, and the structures are discussed with respect to their intraand intermolecular bonding situations and crystal packing. In addition to hydrogen bonds and pi-pi interactions, the appearance of chalcogen and halogen bonds and lone pair-pi interactions between Nb-6 cluster units was observed for the first time.
Hallo Zukunft!
(2022)
Gedruckte Elektronik ist nicht nur ein aufstrebendes Forschungsfeld, sie wird in naher Zukunft auch eine wesentliche Rolle in unserem Alltag spielen. Gedruckte, elektronische Bauteile können sehr dünn und flexibel sein und somit vielfältig eingesetzt werden. Für die Implementation in der (Hoch-)Schule haben die Autoren eine flexible, lichtemittierende Folie entwickelt, die mit einfachen Materialien und Methoden manuell gedruckt werden kann.
Molecular excitons play a central role in processes of solar energy conversion, both natural and artificial. It is therefore no wonder that numerous experimental and theoretical investigations in the last decade, employing state-of-the-art spectroscopic techniques and computational methods, have been driven by the common aim to unravel exciton dynamics in multichromophoric systems. Theoretically, exciton (de)localization and transfer dynamics are most often modelled using either mixed quantum-classical approaches (e.g., trajectory surface hopping) or fully quantum mechanical treatments (either using model diabatic Hamiltonians or direct dynamics). Yet, the terms such as "exciton localization" or "exciton transfer" may bear different meanings in different works depending on the method in use (quantum-classical vs. fully quantum). Here, we relate different views on exciton (de)localization. For this purpose, we perform molecular surface hopping simulations on several tetracene dimers differing by a magnitude of exciton coupling and carry out quantum dynamical as well as surface hopping calculations on a relevant model system. The molecular surface hopping simulations are done using efficient long-range corrected time-dependent density functional tight binding electronic structure method, allowing us to gain insight into different regimes of exciton dynamics in the studied systems.
It has been experimentally demonstrated that reaction rates for molecules embedded in microfluidic optical cavities are altered when compared to rates observed under "ordinary" reaction conditions. However, precise mechanisms of how strong coupling of an optical cavity mode to molecular vibrations affects the reactivity and how resonance behavior emerges are still under dispute. In the present work, we approach these mechanistic issues from the perspective of a thermal model reaction, the inversion of ammonia along the umbrella mode, in the presence of a single-cavity mode of varying frequency and coupling strength. A topological analysis of the related cavity Born-Oppenheimer potential energy surface in combination with quantum mechanical and transition state theory rate calculations reveals two quantum effects, leading to decelerated reaction rates in qualitative agreement with experiments: the stiffening of quantized modes perpendicular to the reaction path at the transition state, which reduces the number of thermally accessible reaction channels, and the broadening of the barrier region, which attenuates tunneling. We find these two effects to be very robust in a fluctuating environment, causing statistical variations of potential parameters, such as the barrier height. Furthermore, by solving the time-dependent Schrodinger equation in the vibrational strong coupling regime, we identify a resonance behavior, in qualitative agreement with experimental and earlier theoretical work. The latter manifests as reduced reaction probability when the cavity frequency omega(c) is tuned resonant to a molecular reactant frequency. We find this effect to be based on the dynamical localization of the vibro-polaritonic wavepacket in the reactant well.
A cationic surfactant containing a spiropyrane unit is prepared exhibiting a dual-responsive adjustability of its surface-active characteristics. The switching mechanism of the system relies on the reversible conversion of the non-ionic spiropyrane (SP) to a zwitterionic merocyanine (MC) and can be controlled by adjusting the pH value and via light, resulting in a pH-dependent photoactivity: While the compound possesses a pronounced difference in surface activity between both forms under acidic conditions, this behavior is suppressed at a neutral pH level. The underlying switching processes are investigated in detail, and a thermodynamic explanation based on a combination of theoretical and experimental results is provided. This complex stimuli-responsive behavior enables remote-control of colloidal systems. To demonstrate its applicability, the surfactant is utilized for the pH-dependent manipulation of oil-in-water emulsions.
Quantum dynamics of the photoinduced charge separation in a symmetric donor-acceptor-donor triad
(2022)
The photoinduced charge separation in a symmetric donor-acceptor-donor (D-A-D) triad is studied quantum mechanically using a realistic diabatic vibronic coupling model. The model includes a locally excited DA*D state and two charge-transfer states D(+)A(-)D and DA(-)D(+) and is constructed according to a procedure generally applicable to semirigid D-A-D structures and based on energies, forces, and force constants obtained by quantum chemical calculations. In this case, the electronic structure is described by time-dependent density functional theory, and the corrected linear response is used in conjunction with the polarizable continuum model to account for state-specific solvent effects. The multimode dynamics following the photoexcitation to the locally excited state are simulated by the hybrid Gaussian-multiconfigurational time-dependent Hartree method, and temperature effects are included using thermo field theory. The dynamics are connected to the transient absorption spectrum obtained in recent experiments, which is simulated and fully assigned from first principles. It is found that the charge separation is mediated by symmetry-breaking vibrations of relatively low frequency, which implies that temperature should be accounted for to obtain reliable estimates of the charge transfer rate.
Bio-interactive hydrogel formation in situ requires sensory capabilities toward physiologically relevant stimuli. Here, we report on pH-controlled in situ hydrogel formation relying on latent cross-linkers, which transform from pH sensors to reactive molecules. In particular, thiopeptolide/thio-depsipeptides were capable of pH-sensitive thiol-thioester exchange reactions to yield a,co-dithiols, which react with maleimide-functionalized multi-arm polyethylene glycol to polymer networks. Their water solubility and diffusibility qualify thiol/thioester-containing peptide mimetics as sensory precursors to drive in situ localized hydrogel formation with potential applications in tissue regeneration such as treatment of inflamed tissues of the urinary tract.
Numerous nanostructured materials have been reported as efficient sulfur hosts to suppress the problematic "shuttling" of lithium polysulfides (LiPSs) in lithium-sulfur (Li-S) batteries. However, direct comparison of these materials in their efficiency of suppressing LiPSs shuttling is challenging, owing to the structural and morphological differences between individual materials. This study introduces a simple route to synthesize a series of sulfur host materials with the same yolk-shell nanospindle morphology but tunable compositions (Fe3O4, FeS, or FeS2), which allows for a systematic investigation into the specific effect of chemical composition on the electrochemical performances of Li-S batteries. Among them, the S/FeS2-C electrode exhibits the best performance and delivers an initial capacity of 877.6 mAh g(-1) at 0.5 C with a retention ratio of 86.7 % after 350 cycles. This approach can also be extended to the optimization of materials for other functionalities and applications.
Sorption measurements of water vapor on an isoreticular series of Imidazolate Frameworks Potsdam (IFP), based on penta-coordinated metal centers with secondary building units (SBUs) connected by multidentate amido-imidate-imidazolate linkers, have been carried out at 303.15 K. The isotherm shapes were analyzed in order to gain insight into material properties and compared to sorption experiments with nitrogen at 77.4 K and carbon dioxide at 273.15 K. Results show that water vapor sorption measurements are strongly influenced by the pore size distribution while having a distinct hysteresis loop between the adsorption and desorption branch in common. Thus, IFP-4 and -8, which solely contain micropores, exhibit H4 (type I) isotherm shapes, while those of IFP-1, -2 and -5, which also contain mesopores, are of H3 (type IV) shape with three inflection points. The choice of the used linker substituents and transition metals employed in the framework has a tremendous effect on the material properties and functionality. The water uptake capacities of the examined IFPs are ranging 0.48 mmol g(-1) (IFP-4) to 6.99 mmol g(-1) (IFP-5) and comparable to those documented for ZIFs. The water vapor stability of IFPs is high, with the exception of IFP-8.
Shape-memory polymer micronetworks (MN) are micrometer-sized objects that can switch their outer shape upon external command.This study aims to scale MN sizes to the low micrometer range at very narrow size distributions. In a two-step microfluidic strategy, the specific design of coaxial class capillary devices allowed stabilizing the thread of the dispersed phase to efficiently produce precursor particles in the tip-streaming regime at rates up to similar to 170 kHz and final sizes down to 4 mu m. In a subsequent melt-based microfluidic photocrosslinking of the methacrylate-functionalized oligo(epsilon-caprolactone) precursor material, MN could be produced without particle aggregation. A comprehensive analysis of MN properties illustrated successful crosslinking, semi-crystalline morphology, and a shape-switching functionality for all investigated MN sizes (4, 6, 9, 12, 22 mu m). Such functional micronetworks tailored to and below the dimension of cells can enable future applications in technology and medicine like controlling cell interaction.
Reactive eutectic media based on ammonium formate for the valorization of bio-sourced materials
(2023)
In the last several decades eutectic mixtures of different compositions were successfully used as solvents for vast amount of chemical processes, and only relatively recently they were discovered to be widely spread in nature. As such they are discussed as a third liquid media of the living cell, that is composed of common cell metabolites. Such media may also incorporate water as a eutectic component in order to regulate properties such as enzyme activity or viscosity. Taking inspiration form such sophisticated use of eutectic mixtures, this thesis will explore the use of reactive eutectic media (REM) for organic synthesis. Such unconventional media are characterized by the reactivity of their components, which means that mixture may assume the role of the solvent as well as the reactant itself.
The thesis focuses on novel REM based on ammonium formate and investigates their potential for the valorization of bio-sourced materials. The use of REM allows the performance of a number of solvent-free reactions, which entails the benefits of a superior atom and energy economy, higher yields and faster rates compared to reactions in solution. This is evident for the Maillard reaction between ammonium formate and various monosaccharides for the synthesis of substituted pyrazines as well as for a Leuckart type reaction between ammonium formate and levulinic acid for the synthesis of 5-methyl-2-pyrrolidone. Furthermore, reaction of ammonium formate with citric acid for the synthesis of yet undiscovered fluorophores, shows that synthesis in REM can open up unexpected reaction pathways.
Another focus of the thesis is the study of water as a third component in the REM. As a result, the concept of two different dilution regimes (tertiary REM and in REM in solvent) appears useful for understanding the influence of water. It is shown that small amounts of water can be of great benefit for the reaction, by reducing viscosity and at the same time increasing reaction yields.
REM based on ammonium formate and organic acids are employed for lignocellulosic biomass treatment. The thesis thereby introduces an alternative approach towards lignocellulosic biomass fractionation that promises a considerable process intensification by the simultaneous generation of cellulose and lignin as well as the production of value-added chemicals from REM components. The thesis investigates the generated cellulose and the pathway to nanocellulose generation and also includes the structural analysis of extracted lignin.
Finally, the thesis investigates the potential of microwave heating to run chemical reactions in REM and describes the synergy between these two approaches. Microwave heating for chemical reactions and the use of eutectic mixtures as alternative reaction media are two research fields that are often described in the scope of green chemistry. The thesis will therefore also contain a closer inspection of this terminology and its greater goal of sustainability.
Soft-template strategy enables the fabrication of composite nanomaterials with desired functionalities and structures. In this thesis, soft templates, including poly(ionic liquid) nanovesicles (PIL NVs), self-assembled polystyrene-b-poly(2-vinylpyridine) (PS-b-P2VP) particles, and glycopeptide (GP) biomolecules have been applied for the synthesis of versatile composite particles of PILs/Cu, molybdenum disulfide/carbon (MoS2/C), and GP-carbon nanotubes-metal (GP-CNTs-metal) composites, respectively. Subsequently, their possible applications as efficient catalysts in two representative reactions, i.e. CO2 electroreduction (CO2ER) and reduction of 4-nitrophenol (4-NP), have been studied, respectively.
In the first work, PIL NVs with a tunable particle size of 50 to 120 nm and a shell thickness of 15 to 60 nm have been prepared via one-step free radical polymerization. By increasing monomer concentration for polymerization, their nanoscopic morphology can evolve from hollow NVs to dense spheres, and finally to directional worms, in which a multi-lamellar packing of PIL chains occurred in all samples. The obtained PIL NVs with varied shell thickness have been in situ functionalized with ultra-small Cu nanoparticles (Cu NPs, 1-3 nm) and subsequently employed as the electrocatalysts for CO2ER. The hollow PILs/Cu composite catalysts exhibit a 2.5-fold enhancement in selectivity towards C1 products compared to the pristine Cu NPs. This enhancement is primarily attributed to the strong electronic interactions between the Cu NPs and the surface functionalities of PIL NVs. This study casts new aspects on using nanostructured PILs as novel electrocatalyst supports in efficient CO2 conversion.
In the second work, a novel approach towards fast degradation of 4-NP has been developed using porous MoS2/C particles as catalysts, which integrate the intrinsically catalytic property of MoS2 with its photothermal conversion capability. Various MoS2/C composite particles have been prepared using assembled PS-b-P2VP block copolymer particles as sacrificed soft templates. Intriguingly, the MoS2/C particles exhibit tailored morphologies including pomegranate-like, hollow, and open porous structures. Subsequently, the photothermal conversion performance of these featured particles has been compared under near infrared (NIR) light irradiation. When employing the open porous MoS2/C particles as the catalyst for the reduction of 4-NP, the reaction rate constant has increased by 1.5-fold under light illumination. This catalytic enhancement mainly results from the open porous architecture and photothermal conversion performance of the MoS2 particles. This proposed strategy offers new opportunities for efficient photothermal-assisted catalysis.
In the third work, a facile and green approach towards the fabrication of GP-CNTs-metal composites has been proposed, which utilizes a versatile GP biomolecule both as a stabilizer for CNTs in water and as a reducing agent for noble metal ions. The abundant hydrogen bonds in GP molecules bestow the formed GP-CNTs with excellent plasticity, enabling the availability of polymorphic CNTs species ranging from dispersion to viscous paste, gel, and even dough by increasing their concentration. The GP molecules can reduce metal precursors at room temperature without additional reducing agents, enabling the in situ immobilization of metal NPs (e.g. Au, Ag, and Pd) on the CNTs surface. The combination of excellent catalytic property of Pd NPs with photothermal conversion capability of CNTs makes the GP-CNTs-Pd composite a promising catalyst for the efficient degradation of 4-NP. The obtained composite displays a 1.6-fold increase in conversion under NIR light illumination in the reduction of 4-NP, mainly owing to the strong light-to-heat conversion effect of CNTs. Overall, the proposed method opens a new avenue for the synthesis of CNTs composite as a sustainable and versatile catalyst platform.
The results presented in the current thesis demonstrate the significance of using soft templates for the synthesis of versatile composites with tailored nanostructure and functionalities. The investigation of these composite nanomaterials in the catalytic reactions reveals their potential in the development of desired catalysts for emerging catalytic processes, e.g. photothermal-assisted catalysis and electrocatalysis.
The kinetics of water transfer between the lower critical solution temperature (LCST) and upper critical solution temperature (UCST) thermoresponsive blocks in about 10 nm thin films of a diblock copolymer is monitored by in situ neutron reflectivity. The UCST-exhibiting block in the copolymer consists of the zwitterionic poly(4((3-methacrylamidopropyl)dimethylammonio)butane-1-sulfonate), abbreviated as PSBP. The LCST-exhibiting block consists of the nonionic poly(N-isopropylacrylamide), abbreviated as PNIPAM. The as-prepared PSBP80-b-PNIPAM(400) films feature a three-layer structure, i.e., PNIPAM, mixed PNIPAM and PSBP, and PSBP. Both blocks have similar transition temperatures (TTs), namely around 32 degrees C for PNIPAM, and around 35 degrees C for PSBP, and with a two-step heating protocol (20 degrees C to 40 degrees C and 40 degrees C to 80 degrees C), both TTs are passed. The response to such a thermal stimulus turns out to be complex. Besides a three-step process (shrinkage, rearrangement, and reswelling), a continuous transfer of D2O from the PNIPAM to the PSBP block is observed. Due to the existence of both, LCST and UCST blocks in the PSBP80-b-PNIPAM(400 )film, the water transfer from the contracting PNIPAM, and mixed layers to the expanding PSBP layer occurs. Thus, the hydration kinetics and thermal response differ markedly from a thermoresponsive polymer film with a single LCST transition.
Special issue
(2020)
The structure, formation and dynamics of both animate and inanimate matter on the nanoscale are a highly interdisciplinary field of rapidly emerging research engaging a broad community encompassing experimentalists, theorists, and technologists. It is relevant for a large variety of molecular and nanosystems of different origin and composition and concerns numerous phenomena originating from physics, chemistry, biology, or materials science. This Topical Issue presents a collection of original research papers devoted to different aspects of structure and dynamics on the nanoscale. Some of the contributions discuss specific applications of the research results in several modern technologies and in next generation medicine. Most of the works of this topical issue were reported at the Fifth International Conference on Dynamics of Systems on the Nanoscale (DySoN) - the premier forum for the presentation of cutting-edge research in this field that was held in Potsdam, Germany in October of 2018.
Carbon nanodots revised
(2020)
Luminescent compounds obtained from the thermal reaction of citric acid and urea have been studied and utilized in different applications in the past few years. The identified reaction products range from carbon nitrides over graphitic carbon to distinct molecular fluorophores. On the other hand, the solid, non-fluorescent reaction product produced at higher temperatures has been found to be a valuable precursor for the CO2-laser-assisted carbonization reaction in carbon laser-patterning. This work addresses the question of structural identification of both, the fluorescent and non-fluorescent reaction products obtained in the thermal reaction of citric acid and urea. The reaction products produced during autoclave-microwave reactions in the melt were thoroughly investigated as a function of the reaction temperature and the reaction products were subsequently separated by a series of solvent extractions and column chromatography. The evolution of a green molecular fluorophore, namely HPPT, was confirmed and a full characterization study on its structure and photophysical properties was conducted. The additional blue fluorescence is attributed to oligomeric ureas, which was confirmed by complementary optical and structural characterization. These two components form strong hydrogen-bond networks which eventually react to form solid, semi-crystalline particles with a size of similar to 7 nm and an elemental composition of 46% C, 22% N, and 29% O. The structural features and properties of all three main components were investigated in a comprehensive characterization study.
Separation of enantiomers is an everlasting challenge in chemistry, catalysis, and synthesis of pharmaceuticals. The design and fabrication of chiral adsorbent materials is a promising way to increase the surface area of chiral information, as well as to maximize the available surface for the adsorption of one enantiomer. Porous materials such as silica or metal-organic-frameworks are established compounds in this field, due to their well-defined surface structure and ease of functionalization with chiral groups. As another class of porous materials, carbons provide the advantages of high thermal and chemical stability, resistance against moisture, electrical conductivity, and widely tunable pore size. Although they are well established in many adsorption-related applications, carbons received far less attention in enantioselective adsorption processes because the controlled functionalization of their surface is rather difficult due to the chemically heterogeneous atoms in the network. A suitable approach to overcome this limitation is the synthesis of chiral carbons directly from chiral precursors. So far, chiral carbons synthesized from chiral precursors used salt-templating as a way of introducing porosity, which resulted in mainly microporous materials or materials with broad pore size distribution. In the present study, the possibility of combining nanocasting as an alternative templating approach with chiral ionic liquids as a carbon precursor is demonstrated. Chiral recognition is measured in the gas phase, by adsorption of chiral gas, as well as in the solution, by using isothermal titration calorimetry. (C) 2020 Elsevier Ltd. All rights reserved.
An easy-to-do synthesis for the hexanuclear niobium cluster compound [Nb6Cl12(CH3OH)(4)(OCH3)(2)] . DABCO . 1.66 CH2Cl2 has been developed. An one-pot reaction between the cluster precursor [Nb6Cl14(H2O)(4)] . 4H(2)O and methanol with the addition of DABCO leads to the crystallization of the title compound in high yield within a few minutes. The single-crystal X-ray structure of this cluster compound has been determined. Very strong, nearly symmetric intercluster hydrogen bonds Nb-6-MeO...H...OMe-Nb-6 are present between the cluster units. A bridging co-crystalline DABCO molecule is also involved in a three-dimensional hydrogen-bonding network.
Modern laser technology and ultrafast spectroscopies have pushed the timescales for detecting and manipulating dynamical processes in molecules from the picosecond over femtosecond domains, to the attosecond regime (1 as = 10(-18) s). This way, real-time dynamics of electrons after their photoexcitation can be probed and manipulated. In particular, experiments are moving more and more from atomic and solid state systems to molecules, opening the fields of "molecular electron dynamics" and "attosecond chemistry." Also on the theory side, powerful quantum dynamical tools have been developed to rationalize experiments on ultrafast electron dynamics in molecular species. <br /> In this contribution, we concentrate on theoretical aspects of ultrafast electron dynamics in molecules, mostly driven by lasers. The dynamics will be described with the help of wavefunction-based ab initio methods such as time-dependent configuration interaction (TD-CI) or the multiconfigurational time-dependent Hartree-Fock (MCTDHF) methods. Besides a survey of the methods and their extensions toward, e.g., treatment of ionization, laser pulse optimization, and open quantum systems, two specific examples of applications will be considered: The creation and/or dynamical fate of electronic wavepackets, and the nonlinear optical response to laser pulse excitation in molecules by high harmonic generation (HHG).
A series of biomass-derived levoglucosenyl alkyl ethers (alkyl = methyl, ethyl, n-propyl, isopropyl, and n-butyl) were synthesized and polymerized by ring-opening olefin metathesis polymerization using the Grubbs catalyst C793 at room temperature. Polymerizations were successfully performed in conventional solvents such as 1,4-dioxane and dichloromethane as well as in polar aprotic "green" solvents such as 2-methyltetrahydrofuran, dihydrolevoglucosenone (Cyrene), and ethyl acetate. The prepared polyacetals with degrees of polymerization of similar to 100 exhibit Schulz-Flory-type molar mass distributions and are thermoplastic materials with rather low glass transition temperatures in the range of 43-0 degrees C depending on the length of the alkyl substituent. Kinetic studies revealed that the polymerization proceeded rapidly to a steady state with a certain minimum monomer concentration threshold. When the steady state was reached, just about half of the [Ru] catalyst had been effective to initiate the polymerization, indicating that the initiation step was a slow process. The remaining catalyst was still active and did no longer react with monomers but with in-chain double bonds, cutting the formed polymer chains into shorter fragments. In the long term, all catalyst was consumed and propagating [Ru] chain ends were deactivated by the elimination of [Ru] from the chain ends to form inactive chains with terminal aldehyde groups.
Oligodepsipeptides (ODPs) attract increasing attention as degradable materials in controlled drug delivery or as building blocks for nano-carriers. Their strong intermolecular interactions provide high stability. Tailoring the side groups of the amino acid repeating units to achieve a strong affinity to particular drugs allows a high drug-loading capacity. Here we describe synthesis and characterization of dihydroxy terminated teroligodepsipeptides (ter-ODPs) by ring-opening copolymerization (ROP) of three different morpholine-2,5-diones (MDs) in bulk in order to provide a set of teroligomers with structural variation for drug release or transfection. Ter-ODPs with equivalent co-monomer feed ratios were prepared as well as ter-ODPs, in which the co-monomer feed ratio was varied between 9 mol% and 78 mol%. Ter-ODPs were synthesized by ROP using 1,1,10,10-tetra-n-butyl-1,10-distanna-2,9,11,18-tetraoxa-5,6,14,15-tetrasulfur-cyclodecane (tin(IV) alkoxide) that was obtained by the reaction of dibutyl tin(II) oxide with 2-hydroxyethyl disulfide. The number average molecular weight (M-n) of ter-ODPs, determined by H-1 NMR and gel permeation chromatography (GPC), ranged between 4000 g center dot mol(-1) and 8600 g center dot mol(-1). Co-monomer compositions in ter-ODPs could be controlled by changing the feed ratio of co-monomers as observed by H-1 NMR spectroscopy and matrix-assisted laser desorption/ionization time-of-flight mass spectrometry (MALDI-TOF-MS). The amount of remaining monomers as determined by H-1 NMR could be kept below 1 wt%. Macrocycles as main sources of byproducts as determined from MALDI-TOF-MS measurements were significantly lower as compared to polymerization by Sn(Oct)(2). Glass-transition temperature (T-g) of ter-ODPs ranged between 59 degrees C and 70 degrees C.
This paper presents shape-memory foams that can be temporarily fixed in their compressed state and be expanded on demand. Highly porous, nanocomposite foams were prepared from a solution of polyetherurethane with suspended nanoparticles (mean aggregate size 90 nm) which have an iron(III) oxide core with a silica shell. The polymer solution with suspended nanoparticles was cooled down to -20 degrees C in a two-stage process, which was followed by freeze-drying. The average pore size increases with decreasing concentration of nanoparticles from 158 mu m to 230 mu m while the foam porosity remained constant. After fixation of a temporary form of the nanocomposite foams, shape recovery can be triggered either by heat or by exposure to an alternating magnetic field. Compressed foams showed a recovery rate of up to 76 +/- 4% in a thermochamber at 80 degrees C, and a slightly lower recovery rate of up to 65 +/- 4% in a magnetic field.
CO oxidation on Ru(0001) is a long-standing example of a reaction that, being thermally forbidden in ultrahigh vacuum, can be activated by femtosecond laser pulses. In spite of its relevance, the precise dynamics of the photoinduced oxidation process as well as the reasons behind the dominant role of the competing CO photodesorption remain unclear. Here we use ab initio molecular dynamics with electronic friction that account for the highly excited and nonequilibrated system created by the laser to investigate both reactions. Our simulations successfully reproduce the main experimental findings: the existence of photoinduced oxidation and desorption, the large desorption to oxidation branching ratio, and the changes in the O K-edge X-ray absorption spectra attributed to the initial stage of the oxidation process. Now, we are able to monitor in detail the ultrafast CO desorption and CO oxidation occurring in the highly excited system and to disentangle what causes the unexpected inertness to the otherwise energetically favored oxidation.
Hybrid nanomaterials offer the combination of individual properties of different types of nanoparticles. Some strategies for the development of new nanostructures in larger scale rely on the self-assembly of nanoparticles as a bottom-up approach. The use of templates provides ordered assemblies in defined patterns. In a typical soft-template, nanoparticles and other surface-active agents are incorporated into non-miscible liquids. The resulting self-organized dispersions will mediate nanoparticle interactions to control the subsequent self-assembly. Especially interactions between nanoparticles of very different dispersibility and functionality can be directed at a liquid-liquid interface.
In this project, water-in-oil microemulsions were formulated from quasi-ternary mixtures with Aerosol-OT as surfactant. Oleyl-capped superparamagnetic iron oxide and/or silver nanoparticles were incorporated in the continuous organic phase, while polyethyleneimine-stabilized gold nanoparticles were confined in the dispersed water droplets. Each type of nanoparticle can modulate the surfactant film and the inter-droplet interactions in diverse ways, and their combination causes synergistic effects. Interfacial assemblies of nanoparticles resulted after phase-separation. On one hand, from a biphasic Winsor type II system at low surfactant concentration, drop-casting of the upper phase afforded thin films of ordered nanoparticles in filament-like networks. Detailed characterization proved that this templated assembly over a surface is based on the controlled clustering of nanoparticles and the elongation of the microemulsion droplets. This process offers versatility to use different nanoparticle compositions by keeping the surface functionalization, in different solvents and over different surfaces. On the other hand, a magnetic heterocoagulate was formed at higher surfactant concentration, whose phase-transfer from oleic acid to water was possible with another auxiliary surfactant in ethanol-water mixture. When the original components were initially mixed under heating, defined oil-in-water, magnetic-responsive nanostructures were obtained, consisting on water-dispersible nanoparticle domains embedded by a matrix-shell of oil-dispersible nanoparticles.
Herein, two different approaches were demonstrated to form diverse hybrid nanostructures from reverse microemulsions as self-organized dispersions of the same components. This shows that microemulsions are versatile soft-templates not only for the synthesis of nanoparticles, but also for their self-assembly, which suggest new approaches towards the production of new sophisticated nanomaterials in larger scale.
Many physicochemical processes depend on the diffusion of small molecules through solid materials. While crystallinity in polymers is advantageous with respect to structure performance, diffusion in such materials is difficult to predict. Here, we investigate the impact of crystal morphology and organization on the diffusion of small molecules using a lattice Monte Carlo approach. Interestingly, diffusion determined with this model does not depend on the internal morphology of the semi-crystalline regions. The obtained insight is highly valuable for developing predictive models for all processes in semi-crystalline polymers involving mass transport, like polymer degradation or drug release, and provide design criteria for the time-dependent functional behavior of multifunctional polymer systems.
Programmable oils feature tunable viscosity and therefore possess potential for technical improvements and innovative solutions in many lubricated applications. Herein, we describe the first assessment of the variability of rheological properties of light-programmable 9-anthracene ester-terminated polydimethylsiloxanes (PDMS-As), including implications that arise with UV-light as an external trigger. We applied a modified rheometer setup that enables the monitoring of dynamic moduli during exposure to UV-light. The reversible dimerization of anthracene esters is used to either link PDMS chains by UV-A radiation (365 nm) or cleave chains by UV-C radiation (254 nm) or at elevated temperatures (>130 degrees C). Thermal cleavage fully restores the initial material properties, while the photochemical cleavage of dimers occurs only to a limited extent. Prolonged UV radiation causes material damage and in turn reduces the range of programmable rheological properties. The incomplete cleavage contributes to a gradual buildup of viscosity over a course of several switching cycles, which we suggest to result from chain length-dependent reaction kinetics. Material property gradients induced during radiation due to attenuation of the light beam upon its passing through the oil layer have to be considered, emphasizing the need for proper mixing protocols during the programming step. The material in focus shows integrated photorheology and is suggested to improve the performance of silicone oils in friction systems.
The macroscale function of multicomponent polymeric materials is dependent on their phase-morphology. Here, we investigate the morphological structure of a multiblock copolymer consisting of poly(L-lactide) and poly(epsilon-caprolactone) segments (PLLA-PCL), physically cross-linked by stereocomplexation with a low molecular weight poly(D-lactide) oligomer (PDLA). The effects of blend composition and PLLA-PCL molecular structure on the morphology are elucidated by AFM, TEM and SAXS. We identify the formation of a lattice pattern, composed of PLA domains within a PCL matrix, with an average domain spacing d0 = 12 - 19 nm. The size of the PLA domains were found to be proportional to the block length of the PCL segment of the copolymer and inversely proportional to the PDLA content of the blend. Changing the PLLA-PCL / PDLA ratio caused a shift in the melt transition Tm attributed to the PLA stereocomplex crystallites, indicating partial amorphous phase dilution of the PLA and PCL components within the semicrystalline material. By elucidating the phase structure and thermal character of multifunctional PLLA-PCL / PDLA blends, we illustrate how composition affects the internal structure and thermal properties of multicomponent polymeric materials. This study should facilitate the more effective incorporation of a variety of polymeric structural units capable of stimuli responsive phase transitions, where an understanding the phase-morphology of each component will enable the production of multifunctional soft-actuators with enhanced performance.
Fibrous shape-memory polymer (SMP) scaffolds were investigated considering the fiber as basic microstructural feature. By reduction of the fiber diameter in randomly oriented electrospun polyetherurethane (PEU) meshes from the micro-to the nano-scale, we observed changes in the molecular orientation within the fibers and its impact on the structural and shape-memory performance. It was assumed that a spatial restriction by reduction of the fiber diameter increases molecular orientation along the orientation of the fiber. The stress-strain relation of random PEU scaffolds is initially determined by the 3D arrangement of the fibers and thus is independent of the molecular orientation. Increasing the molecular orientation with decreasing single fiber diameter in scaffolds composed of randomly arranged fibers did not alter the initial stiffness and peak stress but strongly influenced the elongation at break and the stress increase above the Yield point. Reduction of the single fiber diameter also distinctly improved the shape-memory performance of the scaffolds. Fibers with nanoscale diameters (< 100 nm) possessed an almost complete shape recovery, high recovery stresses and fast relaxation kinetics, while the shape fixity was found to decrease with decreasing fiber diameter. Hence, the fiber diameter is a relevant design parameter for SMP.
Quantum mechanical tunnelling describes transmission of matter waves through a barrier with height larger than the energy of the wave(1). Tunnelling becomes important when the de Broglie wavelength of the particle exceeds the barrier thickness; because wavelength increases with decreasing mass, lighter particles tunnel more efficiently than heavier ones. However, there exist examples in condensed-phase chemistry where increasing mass leads to increased tunnelling rates(2). In contrast to the textbook approach, which considers transitions between continuum states, condensed-phase reactions involve transitions between bound states of reactants and products. Here this conceptual distinction is highlighted by experimental measurements of isotopologue-specific tunnelling rates for CO rotational isomerization at an NaCl surface(3,4), showing nonmonotonic mass dependence. A quantum rate theory of isomerization is developed wherein transitions between sub-barrier reactant and product states occur through interaction with the environment. Tunnelling is fastest for specific pairs of states (gateways), the quantum mechanical details of which lead to enhanced cross-barrier coupling; the energies of these gateways arise nonsystematically, giving an erratic mass dependence. Gateways also accelerate ground-state isomerization, acting as leaky holes through the reaction barrier. This simple model provides a way to account for tunnelling in condensed-phase chemistry, and indicates that heavy-atom tunnelling may be more important than typically assumed.
The imagination of clearly separated core-shell structures is already outdated by the fact, that the nanoparticle core-shell structures remain in terms of efficiency behind their respective bulk material due to intermixing between core and shell dopant ions. In order to optimize the photoluminescence of core-shell UCNP the intermixing should be as small as possible and therefore, key parameters of this process need to be identified. In the present work the Ln(III) ion migration in the host lattices NaYF4 and NaGdF4 was monitored. These investigations have been performed by laser spectroscopy with help of lanthanide resonance energy transfer (LRET) between Eu(III) as donor and Pr(III) or Nd(III) as acceptor. The LRET is evaluated based on the Forster theory. The findings corroborate the literature and point out the migration of ions in the host lattices. Based on the introduced LRET model, the acceptor concentration in the surrounding of one donor depends clearly on the design of the applied core-shell-shell nanoparticles. In general, thinner intermediate insulating shells lead to higher acceptor concentration, stronger quenching of the Eu(III) donor and subsequently stronger sensitization of the Pr(III) or the Nd(III) acceptors. The choice of the host lattice as well as of the synthesis temperature are parameters to be considered for the intermixing process.
Microbially produced polyhydroxyalkanoates (PHAs) are polyesters that are degradable by naturally occurring enzymes. Albeit PHAs degrade slowly when implanted in animal models, their disintegration is faster compared to abiotic hydrolysis under simulated physiological environments. Ultrathin Langmuir-Blodgett (LB) films are used as models for fast in vitro degradation testing, to predict enzymatically catalyzed hydrolysis of PHAs in vivo. The activity of mammalian enzymes secreted by pancreas and liver, potentially involved in biomaterials degradation, along with microbial hydrolases is tested toward LB-films of two model PHAs, poly(3-R-hydroxybutyrate) (PHB) and poly[(3-R-hydroxyoctanoate)-co-(3-R-hydroxyhexanoate)] (PHOHHx). A specific PHA depolymerase fromStreptomyces exfoliatus, used as a positive control, is shown to hydrolyze LB-films of both polymers regardless of their side-chain-length and phase morphology. From amorphous PHB and PHOHHx, approximate to 80% is eroded in few hours, while mass loss for semicrystalline PHB is 25%. Surface potential and interfacial rheology measurements show that material dissolution is consistent with a random-chain-scission mechanism. Degradation-induced crystallization of semicrystalline PHB LB-films is also observed. Meanwhile, the surface and the mechanical properties of both LB-films remain intact throughout the experiments with lipases and other microbial hydrolases, suggesting that non-enzymatic hydrolysis could be the predominant factor for acceleration of PHAs degradation in vivo.
The chemical nature, the number length of integrated building blocks, as well as their sequence structure impact the phase morphology of multiblock copolymers (MBC) consisting of two non-miscible block types. It is hypothesized that a strictly alternating sequence should impact phase segregation. A library of well-defined MBC obtained by coupling oligo(epsilon-caprolactone) (OCL) of different molecular weights (2, 4, and 8 kDa) with oligotetrahydrofuran (OTHF, 2.9 kDa) via Steglich esterification results in strictly alternating (MBCalt) or random (MBCran) MBC. The three different series has a weight average molecular weight (M-w) of 65 000, 165 000, and 168 000 g mol(-1) for MBCalt and 80 500, 100 000, and 147 600 g mol(-1) for MBCran. When the chain length of OCL building blocks is increased, the tendency for phase segregation is facilitated, which is attributed to the decrease in chain mobility within the MBC. Furthermore, it is found that the phase segregation disturbs the crystallization by causing heterogeneities in the semi-crystalline alignment, which is attributed to an increase of the disorder of the OCL semi-crystalline alignment.
Natural gas hydrate occurrences contain predominantly methane; however, there are increasing reports of complex mixed gas hydrates and coexisting hydrate phases. Changes in the feed gas composition due to the preferred incorporation of certain components into the hydrate phase and an inadequate gas supply is often assumed to be the cause of coexisting hydrate phases. This could also be the case for the gas hydrate system in Qilian Mountain permafrost (QMP), which is mainly controlled by pores and fractures with complex gas compositions. This study is dedicated to the experimental investigations on the formation process of mixed gas hydrates based on the reservoir conditions in QMP. Hydrates were synthesized from water and a gas mixture under different gas supply conditions to study the effects on the hydrate formation process. In situ Raman spectroscopic measurements and microscopic observations were applied to record changes in both gas and hydrate phase over the whole formation process. The results demonstrated the effects of gas flow on the composition of the resulting hydrate phase, indicating a competitive enclathration of guest molecules into the hydrate lattice depending on their properties. Another observation was that despite significant changes in the gas composition, no coexisting hydrate phases were formed.
Solar photocatalysis is the one of leading concepts of research in the current paradigm of sustainable chemical industry. For actual practical implementation of sunlight-driven catalytic processes in organic synthesis, a cheap, efficient, versatile and robust heterogeneous catalyst is necessary. Carbon nitrides are a class of organic semiconductors who are known to fulfill these requirements.
First, current state of solar photocatalysis in economy, industry and lab research is overviewed, outlining EU project funding, prospective synthetic and reforming bulk processes, small scale solar organic chemistry, and existing reactor designs and prototypes, concluding feasibility of the approach.
Then, the photocatalytic aerobic cleavage of oximes to corresponding aldehydes and ketones by anionic poly(heptazine imide) carbon nitride is discussed. The reaction provides a feasible method of deprotection and formation of carbonyl compounds from nitrosation products and serves as a convenient model to study chromoselectivity and photophysics of energy transfer in heterogeneous photocatalysis.
Afterwards, the ability of mesoporous graphitic carbon nitride to conduct proton-coupled electron transfer was utilized for the direct oxygenation of 1,3-oxazolidin-2-ones to corresponding 1,3-oxazlidine-2,4-diones. This reaction provides an easier access to a key scaffold of diverse types of drugs and agrochemicals.
Finally, a series of novel carbon nitrides based on poly(triazine imide) and poly(heptazine imide) structure was synthesized from cyanamide and potassium rhodizonate. These catalysts demonstrated a good performance in a set of photocatalytic benchmark reactions, including aerobic oxidation, dual nickel photoredox catalysis, hydrogen peroxide evolution and chromoselective transformation of organosulfur precursors.
Concluding, the scope of carbon nitride utilization for net-oxidative and net-neutral photocatalytic processes was expanded, and a new tunable platform for catalyst synthesis was discovered.
Hazelnuts are rarely cultivated in Germany, although they are a valuable source for macro- and micronutrients and can thus contribute to a healthy diet. Near the present, 15 varieties were cultivated in Thuringia, Germany, as a pilot study for further research. The aim of our study was to evaluate the micro- and macronutrient composition of representative, randomly mixed samples of the 15 different hazelnut cultivars. Protein, fat, and fiber contents were determined using established methods. Fatty acids, tocopherols, minerals, trace elements, and ultra-trace elements were analyzed using gas chromatography, high-performance liquid chromatography, and inductively coupled plasma triple quadrupole mass-spectrometry, respectively. We found that the different hazelnut varieties contained valuable amounts of fat, protein, dietary fiber, minerals, trace elements, and alpha-tocopherol, however, in different quantities. The variations in nutrient composition were independent of growth conditions, which were identical for all hazelnut varieties. Therefore, each hazelnut cultivar has its specific nutrient profile.
In this paper, we propose a consistent mechanism of protein microcapsule formation upon ultrasound treatment. Aqueous suspensions of bovine serum albumin (BSA) microcapsules filled with toluene are prepared by use of high-intensity ultrasound following a reported method. Stabilization of the oil-in-water emulsion by the adsorption of the protein molecules at the interface of the emulsion droplets is accompanied by the creation of the cross-linked capsule shell due to formation of intermolecular disulfide bonds caused by highly reactive species like superoxide radicals generated sonochemically. The evidence for this mechanism, which until now remained elusive and was not proven properly, is presented based on experimental data from SDS-PAGE, Raman spectroscopy and dynamic light scattering.
The present thesis focuses on the synthesis of nanostructured iron-based compounds by using β-FeOOH nanospindles and poly(ionic liquid)s (PILs) vesicles as hard and soft templates, respectively, to suppress the shuttle effect of lithium polysulfides (LiPSs) in Li-S batteries. Three types of composites with different nanostructures (mesoporous nanospindle, yolk-shell nanospindle, and nanocapsule) have been synthesized and applied as sulfur host material for Li-S batteries. Their interactions with LiPSs and effects on the electrochemical performance of Li-S batteries have been systematically studied.
In the first part of the thesis, carbon-coated mesoporous Fe3O4 (C@M-Fe3O4) nanospindles have been synthesized to suppress the shuttle effect of LiPSs. First, β-FeOOH nanospindles have been synthesized via the hydrolysis of iron (III) chloride in aqueous solution and after silica coating and subsequent calcination, mesoporous Fe2O3 (M-Fe2O3) have been obtained inside the confined silica layer through pyrolysis of β-FeOOH. After the removal of the silica layer, electron tomography (ET) has been applied to rebuild the 3D structure of the M-Fe2O3 nanospindles. After coating a thin layer of polydopamine (PDA) as carbon source, the PDA-coated M-Fe2O3 particles have been calcinated to synthesize C@M-Fe3O4 nanospindles. With the chemisorption of Fe3O4 and confinement of mesoporous structure to anchor LiPSs, the composite C@M-Fe3O4/S electrode delivers a remaining capacity of 507.7 mAh g-1 at 1 C after 600 cycles.
In the second part of the thesis, a series of iron-based compounds (Fe3O4, FeS2, and FeS) with the same yolk-shell nanospindle morphology have been synthesized, which allows for the direct comparison of the effects of compositions on the electrochemical performance of Li-S batteries. The Fe3O4-carbon yolk-shell nanospindles have been synthesized by using the β-FeOOH nanospindles as hard template. Afterwards, Fe3O4-carbon yolk-shell nanospindles have been used as precursors to obtain iron sulfides (FeS and FeS2)-carbon yolk-shell nanospindles through sulfidation at different temperatures. Using the three types of yolk-shell nanospindles as sulfur host, the effects of compositions on interactions with LiPSs and electrochemical performance in Li-S batteries have been systematically investigated and compared. Benefiting from the chemisorption and catalytic effect of FeS2 particles and the physical confinement of the carbon shell, the FeS2-C/S electrode exhibits the best electrochemical performance with an initial specific discharge capacity of 877.6 mAh g-1 at 0.5 C and a retention ratio of 86.7% after 350 cycles.
In the third part, PILs vesicles have been used as soft template to synthesize carbon nanocapsules embedded with iron nitride particles to immobilize and catalyze LiPSs in Li-S batteries. First, 3-n-decyl-1-vinylimidazolium bromide has been used as monomer to synthesize PILs nanovesicles by free radical polymerization. Assisted by PDA coating route and ion exchange, PIL nanovesicles have been successfully applied as soft template in morphology-maintaining carbonization to prepare carbon nanocapsules embedded with iron nitride nanoparticles (FexN@C). The well-dispersed iron nitride nanoparticles effectively catalyze the conversion of LiPSs to Li2S, owing to their high electrical conductivity and strong chemical binding to LiPSs. The constructed FexN@C/S cathode demonstrates a high initial discharge capacity of 1085.0 mAh g-1 at 0.5 C with a remaining value of 930.0 mAh g-1 after 200 cycles.
The results in the present thesis demonstrate the facile synthetic routes of nanostructured iron-based compounds with controllable morphologies and compositions using soft and hard colloidal templates, which can be applied as sulfur host to suppress the shuttle behavior of LiPSs. The synthesis approaches developed in this thesis are also applicable to fabricating other transition metal-based compounds with porous nanostructures for other applications.