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- ItemMechanochemistry-assisted synthesis of hierarchical porous carbons applied as supercapacitors(Frankfurt, M. : Beilstein-Institut zur Förderung der Chemischen Wissenschaften, 2017) Leistenschneider, Desirée; Jäckel, Nicolas; Hippauf, Felix; Presser, Volker; Borchardt, LarsA solvent-free synthesis of hierarchical porous carbons is conducted by a facile and fast mechanochemical reaction in a ball mill. By means of a mechanochemical ball-milling approach, we obtained titanium(IV) citrate-based polymers, which have been processed via high temperature chlorine treatment to hierarchical porous carbons with a high specific surface area of up to 1814 m2 g−1 and well-defined pore structures. The carbons are applied as electrode materials in electric double-layer capacitors showing high specific capacitances with 98 F g−1 in organic and 138 F g−1 in an ionic liquid electrolyte as well as good rate capabilities, maintaining 87% of the initial capacitance with 1 M TEA-BF4 in acetonitrile (ACN) and 81% at 10 A g−1 in EMIM-BF4.
- ItemMechanically reinforced catechol-containing hydrogels with improved tissue gluing performance(Basel : MDPI, 2017) Feng, Jun; Ton, Xuan-Anh; Zhao, Shifang; Paez, Julieta I.; del Campo, AránzazuIn situ forming hydrogels with catechol groups as tissue reactive functionalities are interesting bioinspired materials for tissue adhesion. Poly(ethylene glycol) (PEG)–catechol tissue glues have been intensively investigated for this purpose. Different cross-linking mechanisms (oxidative or metal complexation) and cross-linking conditions (pH, oxidant concentration, etc.) have been studied in order to optimize the curing kinetics and final cross-linking degree of the system. However, reported systems still show limited mechanical stability, as expected from a PEG network, and this fact limits their potential application to load bearing tissues. Here, we describe mechanically reinforced PEG–catechol adhesives showing excellent and tunable cohesive properties and adhesive performance to tissue in the presence of blood. We used collagen/PEG mixtures, eventually filled with hydroxyapatite nanoparticles. The composite hydrogels show far better mechanical performance than the individual components. It is noteworthy that the adhesion strength measured on skin covered with blood was >40 kPa, largely surpassing (>6 fold) the performance of cyanoacrylate, fibrin, and PEG–catechol systems. Moreover, the mechanical and interfacial properties could be easily tuned by slight changes in the composition of the glue to adapt them to the particular properties of the tissue. The reported adhesive compositions can tune and improve cohesive and adhesive properties of PEG–catechol-based tissue glues for load-bearing surgery applications.
- ItemBright fluorescent silica-nanoparticle probes for high-resolution STED and confocal microscopy(Frankfurt am Main : Beilstein-Institut, 2017) Tavernaro, Isabella; Cavelius, Christian; Peuschel, Henrike; Kraegeloh, AnnetteIn recent years, fluorescent nanomaterials have gained high relevance in biological applications as probes for various fluorescencebased spectroscopy and imaging techniques. Among these materials, dye-doped silica nanoparticles have demonstrated a high potential to overcome the limitations presented by conventional organic dyes such as high photobleaching, low stability and limited fluorescence intensity. In the present work we describe an effective approach for the preparation of fluorescent silica nanoparticles in the size range between 15 and 80 nm based on L-arginine-controlled hydrolysis of tetraethoxysilane in a biphasic cyclohexane–water system. Commercially available far-red fluorescent dyes (Atto647N, Abberior STAR 635, Dy-647, Dy-648 and Dy-649) were embedded covalently into the particle matrix, which was achieved by aminosilane coupling. The physical particle attributes (particle size, dispersion, degree of agglomeration and stability) and the fluorescence properties of the obtained particles were compared to particles from commonly known synthesis methods. As a result, the spectroscopic characteristics of the presented monodisperse dye-doped silica nanoparticles were similar to those of the free uncoupled dyes, but indicate a much higher photostability and brightness. As revealed by dynamic light scattering and ζ-potential measurements, all particle suspensions were stable in water and cell culture medium. In addition, uptake studies on A549 cells were performed, using confocal and stimulated emission depletion (STED) microscopy. Our approach allows for a step-by-step formation of dye-doped silica nanoparticles in the form of dye-incorporated spheres, which can be used as versatile fluorescent probes in confocal and STED imaging.
- ItemFunnel-shaped microstructures for strong reversible adhesion(Hoboken, NJ : Wiley, 2017) Fischer, Sarah C.L.; Groß, Katja; Abad, Oscar Torrents; Becker, MIchael M.; Park, Euiyoung; Hensel, René; Arzt, EduardThe potential of a new design of adhesive microstructures in the micrometer range for enhanced dry adhesion is investigated. Using a two-photon lithography system, complex 3D master structures of funnel-shaped microstructures are fabricated for replication into poly(ethylene glycol) dimethacrylate polymer. The diameter, the flap thickness, and the opening angle of the structures are varied systematically. The adhesion of single structures is characterized using a triboindenter system equipped with a flat diamond punch. The pull-off stresses obtained reaches values up to 5.6 MPa, which is higher than any values reported in literature for artificial dry adhesives. Experimental and numerical results suggest a characteristic attachment mechanism that leads to intimate contact formation from the edges toward the center of the structures. van der Waals interactions most likely dominate the adhesion, while contributions by suction or capillarity play only a minor role. Funnel-shaped microstructures are a promising concept for strong and reversible adhesives, applicable in novel pick and place handling systems or wall-walking robots.
- ItemTemperature-dependent size effects on the strength of Ta and W micropillars(Amsterdam : Elsevier, 2016) Torrents Abad, Oscar; Wheeler, Jeffrey M.; Michler, Johann; Schneider, Andreas S.; Arzt, EduardThe strength of metals increases with decreasing sample size, a trend known as the size effect. In particular, focused ion beam-milled body-centered cubic (BCC) micropillars exhibit a size effect known to scale with the ratio of the test temperature to the critical temperature (Tc) of the BCC metal, a measure of how much the yield stress is governed by the lattice resistance. In this paper, this effect is systematically studied by performing high-temperature compression tests on focused ion beam-manufactured Ta and W single crystal pillars ranging in diameter from 500 nm to 5 μm at temperatures up to 400 °C, and discussed in the context of bulk strength and size dependent stresses. Both metals show larger size effects at higher temperatures, reaching values that are in the range of FCC metals at temperatures near Tc. However, it is demonstrated that size effects can be considerably affected by material parameters such as dislocation density and lattice friction, as well as by the yield criterion used. Furthermore, for W, a change from uniform wavy deformation to localized deformation is observed with increasing temperature and pillar size, further indicating that the temperature ratio strongly influences the relative motion of screw and edge dislocations.
- ItemOn the process of co-deformation and phase dissolution in a hard-soft immiscible CuCo alloy system during high-pressure torsion deformation(Amsterdam : Elsevier, 2016) Bachmaier, Andrea; Schmauch, Jörg; Aboulfadl, Hisham; Verch, Andreas; Motz, ChristianIn this study, dual phase Cusingle bondCo composites with a total immiscibility in the solid state and a very different initial phase strength are deformed by severe plastic deformation. Nanocrystalline supersaturated solid solutions are reached in all Cusingle bondCo composites independent of the initial composition. The deformation and mechanical mixing process is studied thoroughly by combining scanning electron microscopy, transmission electron microscopy, three-dimensional atom probe tomography and nanoindentation. The indentation hardness of the Cu and Co phase and its evolution as a function of the applied strain is linked to deformation and mechanical mixing process to gain a better understanding how the phase strength mismatch of the Cu and Co phase effects the amount of co-deformation and deformation-induced mixing. Our results show that co-deformation is not a necessary requirement to achieve mechanical mixing.
- ItemComposite pillars with a tunable interface for adhesion to rough substrates(Washington D.C. : American Chemical Society, 2017) Fischer, Sarah C.L.; Arzt, Eduard; Hensel, RenéThe benefits of synthetic fibrillar dry adhesives for temporary and reversible attachment to hard objects with smooth surfaces have been successfully demonstrated in previous studies. However, surface roughness induces a dramatic reduction in pull-off stresses and necessarily requires revised design concepts. Toward this aim, we introduce cylindrical two-phase single pillars, which are composed of a mechanically stiff stalk and a soft tip layer. Adhesion to smooth and rough substrates is shown to exceed that of conventional pillar structures. The adhesion characteristics can be tuned by varying the thickness of the soft tip layer, the ratio of the Young’s moduli and the curvature of the interface between the two phases. For rough substrates, adhesion values similar to those obtained on smooth substrates were achieved. Our concept of composite pillars overcomes current practical limitations caused by surface roughness and opens up fields of application where roughness is omnipresent.
- ItemEnhanced electrochemical energy storage by nanoscopic decoration of endohedral and exohedral carbon with vanadium oxide via atomic layer deposition(Washington D.C. : American Chemical Society, 2016) Fleischmann, Simon; Jäckel, Nicolas; Zeiger, Marco; Krüner, Benjamin; Grobelsek, Ingrid; Formanek, Petr; Choudhury, Soumyadip; Weingarth, Daniel; Presser, VolkerAtomic layer deposition (ALD) is a facile process to decorate carbon surfaces with redox-active nanolayers. This is a particularly attractive route to obtain hybrid electrode materials for high performance electrochemical energy storage applications. Using activated carbon and carbon onions as representatives of substrate materials with large internal or external surface area, respectively, we have studied the enhanced energy storage capacity of vanadium oxide coatings. While the internal porosity of activated carbon readily becomes blocked by obstructing nanopores, carbon onions enable the continued deposition of vanadia within their large interparticle voids. Electrochemical benchmarking in lithium perchlorate in acetonitrile (1 M LiClO4) showed a maximum capacity of 122 mAh/g when using vanadia coated activated carbon and 129 mAh/g for vanadia coated carbon onions. There is an optimum amount of vanadia between 50 and 65 wt % for both substrates that results in an ideal balance between redox-activity and electrical conductivity of the hybrid electrode. Assembling asymmetric (charge balanced) full-cells, a maximum specific energy of 38 Wh/kg and 29 Wh/kg was found for carbon onions and activated carbon, respectively. The stability of both systems is promising, with a capacity retention of ∼85–91% after 7000 cycles for full-cell measurements.
- ItemDatasets from a vapor diffusion mineral precipitation protocol for Dictyostelium stalks(Amsterdam : Elsevier, 2016) Eder, Magdalena; Muth, Christina; Weiss, Ingrid M.Datasets from a slow carbonate vapor diffusion and mineral precipitation protocol for Dictyostelium ECM and cellulose stalks show examples for composite materials obtained by an in vitro approach, which differs substantially from the in vivo approach reported in The Journal of Structural Biology, doi: 10.1016/j.jsb.2016.03.015 [1]. Methods for obtaining the datasets include bright field transmitted light microscopy, fluorescence microscopy, LC-PolScope birefringence microscopy, variable pressure scanning electron microscopy (VP-SEM/ESEM), and Raman imaging spectroscopy.
- ItemGold nanorods with conjugated polymer ligands: sintering-free conductive inks for printed electronics(Cambridge : Royal Society of Chemistry, 2016) Reiser, B.; González-García, L.; Kanelidis, I.; Maurer, J.H.M.; Kraus, T.Metal-based nanoparticle inks for printed electronics usually require sintering to improve the poor electron transport at particle-particle interfaces. The ligands required for colloidal stability act as insulating barriers and must be removed in a post-deposition sintering step. This complicates the fabrication process and makes it incompatible with many flexible substrates. Here, we bind a conjugated, electrically conductive polymer on gold nanorods (AuNRs) as a ligand. The polymer, poly[2-(3-thienyl)-ethyloxy-4-butylsulfonate] (PTEBS), provides colloidal stability and good electron transport properties to stable, sintering-free inks. We confirm that the polymer binds strongly through a multidentate binding motif and provides superior colloidal stability in polar solvents over months by IR and Raman spectrometry and zeta potential measurements. We demonstrate that the developed ligand exchange protocol is directly applicable to other polythiophenes such as poly(3,4-ethylenedioxythiophene):polystyrene sulfonate (PEDOT:PSS). Films of AuNRs coated with above polymers reached conductivities directly after deposition comparable to conventional metal inks after ligand removal and retained their conductivity for at least one year when stored under ambient conditions.