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- ItemGold Aerogels: Three-Dimensional Assembly of Nanoparticles and Their Use as Electrocatalytic Interfaces(Washington, DC : Soc., 2016) Wen, Dan; Liu, Wei; Haubold, Danny; Zhu, Chengzhou; Oschatz, Martin; Holzschuh, Matthias; Wolf, André; Simon, Frank; Kaskel, Stefan; Eychmüller, AlexanderThree-dimensional (3D) porous metal nanostructures have been a long sought-after class of materials due to their collective properties and widespread applications. In this study, we report on a facile and versatile strategy for the formation of Au hydrogel networks involving the dopamine-induced 3D assembly of Au nanoparticles. Following supercritical drying, the resulting Au aerogels exhibit high surface areas and porosity. They are all composed of porous nanowire networks reflecting in their diameters those of the original particles (5–6 nm) via electron microscopy. Furthermore, electrocatalytic tests were carried out in the oxidation of some small molecules with Au aerogels tailored by different functional groups. The beta-cyclodextrin-modified Au aerogel, with a host–guest effect, represents a unique class of porous metal materials of considerable interest and promising applications for electrocatalysis.
- ItemNickel cobalt oxide hollow nanosponges as advanced electrocatalysts for the oxygen evolution reaction(Cambridge : Soc., 2015) Zhu, Chengzhou; Wen, Dan; Leubner, Susanne; Oschatz, Martin; Liu, Wei; Holzschuh, Matthias; Simon, Frank; Kaskel, Stefan; Eychmüller, AlexanderA class of novel nickel cobalt oxide hollow nanosponges were synthesized through a sodium borohydride reduction strategy. Due to their porous and hollow nanostructures, and synergetic effects between their components, the optimized nickel cobalt oxide nanosponges exhibited excellent catalytic activity towards oxygen evolution reaction.
- ItemElectrolytic Surface Treatment for Improved Adhesion between Carbon Fibre and Polycarbonate(Basel : MDPI, 2018) Kamps, Jan Henk; Henderson, Luke C.; Scheffler, Christina; Van der Heijden, Ruud; Simon, Frank; Bonizzi, Teena; Verghese, NikhilTo achieve good mechanical properties of carbon fibre-reinforced polycarbonate composites, the fibre-matrix adhesion must be dialled to an optimum level. The electrolytic surface treatment of carbon fibres during their production is one of the possible means of adapting the surface characteristics of the fibres. The production of a range of tailored fibres with varying surface treatments (adjusting the current, potential, and conductivity) was followed by contact angle, inverse gas chromatography and X-ray photoelectron spectroscopy measurements, which revealed a significant increase in polarity and hydroxyl, carboxyl, and nitrile groups on the fibre surface. Accordingly, an increase in the fibre-matrix interaction indicated by a higher interfacial shear strength was observed with the single fibre pull-out force-displacement curves. The statistical analysis identified the correlation between the process settings, fibre surface characteristics, and the performance of the fibres during single fibre pull-out testing.
- ItemSurface Treatment of Carbon Fibers by Oxy-Fluorination(Basel : MDPI, 2019) Kruppke, Iris; Scheffler, Christina; Simon, Frank; Hund, Rolf-Dieter; Cherif, ChokriIn this paper, the oxy-fluorination process and the influence of different concentrations of fluorine and oxygen in the gas phase on the physicochemical properties of polyacrylonitrile(PAN)-based carbon fibers are described. The properties of the treated carbon structures are determined by zeta potential and tensiometry measurements. In addition, changes in surface composition and morphology are investigated by X-ray photoelectron spectroscopy (XPS) and scanning electron microscopy (SEM). Adhesion properties are characterized by the single fiber pull-out (SFPO) test. Furthermore, changes in intrinsic properties are described by means of tensile and density measurements. After a primary desizing effect by oxy-fluorination, an increased number of oxygen-containing surface functional groups could be detected, which led to more debonding work in SFPOs with an epoxy-based matrix. It was also shown that the polar surface energy grows with rising fluorine concentration in the reaction gas mixture. In addition, a minor increase of ~10% in the maximum strength of PAN-based carbon fibers is detected by single fiber tensile measurements after oxy-fluorination with a fluorine content of 5% in the reaction mixture.
- ItemAntioxidant and hydrophilic poly(lactic acid) fibers obtained through their modification with amines and ferulic acid(New York, NY [u.a.] : Wiley, 2017) Wojciechowska, Dorota; Herczyńska, Lucyna; Simon, Frank; Puchalski, Michał; Stawski, DawidThe ferulic acid (FA) is a natural antioxidant, abundantly present in plants, which acts as the plant's immune system. In order to take advantage of its properties, a method has been developed, which combines antioxidant FA with bio-based biodegradable poly(lactic acid) fibers and biocompatible hydrophilic polyallylamine, enabling the production of versatile base material that could be used for active anti-inflammatory wound dressings. The fibers are first subjected to aminolysis in order to obtain amino moieties on the surface, able to react with the molecules of FA. Next, the FA was attached to the aminolyzed fibers surface with use of 1-ethyl-3–(3-dimethylaminopropyl) carbodiimide and N-hydroxysuccinimide. The anti-inflammatory properties of the modified fibers were assessed using 2,2-diphenyl-1-picrylhydrazyl radical scavenging assay. Presence of FA on the fibers’ surface was investigated through X-ray photoelectron spectroscopy analysis and Folin–Ciocalteu (total phenolic content) test.
- ItemCVD-Grown CNTs on Basalt Fiber Surfaces for Multifunctional Composite Interphases(Basel : MDPI, 2016) Förster, Theresa; Hao, Bin; Mäder, Edith; Simon, Frank; Wölfel, Enrico; Ma, Peng-ChengChemical vapor deposition (CVD) is used as a method for the synthesis of carbon nanotubes (CNT) on substrates, most commonly pre-treated by a metal-catalyst. In this work, the capability of basalt fiber surfaces was investigated in order to stimulate catalyst-free growth of carbon nanotubes. We have carried out CVD experiments on unsized, sized, and NaOH-treated basalt fibers modified by growth temperature and a process gas mixture. Subsequently, we investigated the fiber surfaces by SEM, AFM, XPS and carried out single fiber tensile tests. Growth temperatures of 700 °C as well as 800 °C may induce CNT growth, but depending on the basalt fiber surface, the growth process was differently affected. The XPS results suggest surficial iron is not crucial for the CNT growth. We demonstrate that the formation of a corrosion shell is able to support CNT networks. However, our investigations do not expose distinctively the mechanisms by which unsized basalt fibers sometimes induce vertically aligned CNT carpets, isotropically arranged CNTs or no CNT growth. Considering data from the literature and our AFM results, it is assumed that the nano-roughness of surfaces could be a critical parameter for CNT growth. These findings will motivate the design of future experiments to discover the role of surface roughness as well as surface defects on the formation of hierarchical interphases.
- ItemElucidating the chemistry behind the reduction of graphene oxide using a green approach with polydopamine(Basel : MDPI, 2019) Silva, Cláudia; Simon, Frank; Friedel, Peter; Pötschke, Petra; Zimmerer, CordeliaA new approach using X-ray photoelectron spectroscopy (XPS) was employed to give insight into the reduction of graphene oxide (GO) using a green approach with polydopamine (PDA). In this approach, the number of carbon atoms bonded to OH and to nitrogen in PDA is considered and compared to the total intensity of the signal resulting from OH groups in polydopamine-reduced graphene oxide (PDA-GO) to show the reduction. For this purpose, GO and PDA-GO with different times of reduction were prepared and characterized by Raman Spectroscopy and XPS. The PDA layer was removed to prepare reduced graphene oxide (RGO) and the effect of all chemical treatments on the thermal and electrical properties of the materials was studied. The results show that the complete reduction of the OH groups in GO occurred after 180 min of reaction. It was also concluded that Raman spectroscopy is not well suited to determine if the reduction and restoration of the sp2 structure occurred. Moreover, a significant change in the thermal stability was not observed with the chemical treatments. Finally, the electrical powder conductivity decreased after reduction with PDA, increasing again after its removal. © 2019 by the authors. Licensee MDPI, Basel, Switzerland.
- ItemPolyethenetetrathiolate or polytetrathiooxalate? Improved synthesis, a comparative analysis of a prominent thermoelectric polymer and implications to the charge transport mechanism(Cambridge : RSC Publ., 2018) Tkachov, Roman; Stepien, Lukas; Grafe, Robert; Guskova, Olga; Kiriy, Anton; Simon, Frank; Reith, Heiko; Nielsch, Kornelius; Schierning, Gabi; Kasinathan, Deepa; Leyens, Christoph1,1,2,2-Ethenetetrathiolate (ett4-) coordination polymers, such as poly[Kx(Ni-ett)], have been known for decades for their excellent thermoelectric properties. However in reality, ett4- is neither a "true" comonomer which participates in the polymerization, nor represents a "true" repeat unit of the target polymer. Indeed, poly[K2(Ni-ett)], which is formally the product of Ni-induced polymerization of ett4-, has a poor conductivity and needs to be oxidized to show attractive thermoelectric characteristics. The polymerization and oxidation processes are poorly controllable which causes irreproducibility of the polymer properties. To improve the synthesis reproducibility, we studied polymerization of potassium tetrathiooxalate (K2tto), the convenient synthesis of which was developed in our recent work. Because K2tto is the "true monomer", and not its precursor, a high quality product is reproducibly formed simply by mixing K2tto with NiCl2 at room temperature. The procedure does not require additional components (bases), or special conditions (prolonged heating), which are usually needed for the preparation of this polymer from the monomer precursor 1,3,4,6-tetrathiapentalene-2,5-dione (TPD). Furthermore, as tto2- is formally the product of two-electron oxidation of ett4-, the poorly controllable oxidation process is avoided and poly[Ni-tto] almost free from K is directly formed upon the complexation of Ni2+ and tto2-. Thus-obtained poly[Ni-tto] possesses conductivity in the range of 27-47 S cm-1 and a Seebeck coefficient in the range of -38 to -55 μV K-1, which are superior thermoelectric properties compared to poly[Kx(Ni-ett)] samples obtained by the previously reported methods. Redox and structural properties of poly[Ni-tto] were compared with those of poly[Kx(Ni-ett)] obtained by the reported methods. Furthermore, DFT calculations were performed to shed more light on generally promising properties of this class of materials. Particularly, possible packing models have been predicted for polymers, and the molecular dynamics simulations have been used to simulate the molecular arrangements under ambient conditions.
- ItemBiowaste chicken eggshell powder as a potential cure modifier for epoxy/anhydride systems: competitiveness with terpolymer-modified calcium carbonate at low loading levels(London : RSC Publishing, 2017) Saeb, Mohammad Reza; Ghaffari, Mehdi; Rastin, Hadi; Khonakdar, Hossein Ali; Simon, Frank; Najafi, Farhood; Goodarzi, Vahabodin; Vijayan P., Poornima; Puglia, Debora; Asl, Farzaneh Hassanpour; Formela, KrzysztofBiowaste chicken eggshell (ES) powder was applied as a potential cure modifier in epoxy/anhydride systems. Cure behaviour and kinetics of composites filled with very low content (0.1 wt% based on epoxy resin) of ES, calcium carbonate (CaCO3), and terpolymer-modified fillers, mES and mCaCO3, were discussed comparatively. Surface analysis was performed by X-ray photoelectron spectroscopy. Cure kinetics was investigated by differential (Friedman) and integral (Ozawa and Kissinger-Akahira-Sunose) isoconversional methods using dynamic differential scanning calorimetry (DSC) data. Overall, protein precursors naturally existing in the structure of pristine ES facilitated crosslinking of epoxy and hardener of anhydride with functional groups resulting from terpolymer attachment to CaCO3 particles. Accelerated/hindered cure was observed depending on the filler type and surface characteristics, as investigated via the autocatalytic/non-catalytic nature of reactions and comparison of activation energy values of four types of composites. An enhanced cure was identified for composites containing untreated ES, which could be inferred on account of the lower competitive cure of carboxyl groups in the terpolymer backbone with epoxy compared to peptide groups existing in microporous pristine ES. On the other hand, mCaCO3 revealed low values of activation energy compared to pristine CaCO3, but still of the same order as ground biowaste ES.