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- ItemIn-situ nanodiamond to carbon onion transformation in metal matrix composites(Amsterdam : Elsevier, 2018) Suarez, Sebastian; Reinert, Leander; Zeiger, Marco; Miska, Patrice; Grandthyll, Samuel; Müller, Frank; Presser, Volker; Mücklich, FrankIn the present study, nickel matrix composites reinforced with a fine distribution of nanodiamonds (6.5 vol%) as reinforcement phase are annealed in vacuum at different temperatures ranging from 750 °C to 1300 °C. This is carried out to evaluate the in-situ transformation of nanodiamonds to carbon onions within a previously densified composite. The resulting materials are thoroughly analyzed by complementary analytical methods, including Raman spectroscopy, transmission electron microscopy, scanning electron microscopy, energy dispersive X-ray spectroscopy and X-ray photoelectron spectroscopy. The proposed in-situ transformation method presents two main benefits. On one hand, since the particle distribution of a nanodiamond-reinforced composite is significantly more homogenous than in case of the carbon onions, it is expected that the transformed particles will preserve the initial distribution features of nanodiamonds. On the other hand, the proposed process allows for the tuning of the sp3/sp2 carbon ratio by applying a single straightforward post-processing step.
- ItemVacuum or flowing argon: What is the best synthesis atmosphere for nanodiamond-derived carbon onions for supercapacitor electrodes?(Amsterdam : Elsevier, 2015) Zeiger, Marco; Jäckel, Nicolas; Weingarth, Daniel; Presser, VolkerWe present a comprehensive study on the influence of the synthesis atmosphere on the structure and properties of nanodiamond-derived carbon onions. Carbon onions were synthesized at 1300 and 1700 °C in high vacuum or argon flow, using rapid dynamic heating and cooling. High vacuum annealing yielded carbon onions with nearly perfect spherical shape. An increase in surface area was caused by a decrease in particle density when transitioning from sp3 to sp2 hybridization and negligible amounts of disordered carbon were produced. In contrast, carbon onions from annealing nanodiamonds in flowing argon are highly interconnected by few-layer graphene nanoribbons. The presence of the latter improves the electrical conductivity, which is reflected by an enhanced power handling ability of supercapacitor electrodes operated in an organic electrolyte (1 M tetraethylammonium tetrafluoroborate in acetonitrile). Carbon onions synthesized in argon flow at 1700 °C show a specific capacitance of 20 F/g at 20 A/g current density and 2.7 V cell voltage which is an improvement of more than 40% compared to vacuum annealing. The same effect was measured for a synthesis temperature of 1300 °C, with a 140% higher capacitance at 20 A/g for argon flow compared to vacuum annealing.
- ItemQuinone-decorated onion-like carbon/carbon fiber hybrid electrodes for high-rate supercapacitor applications(Hoboken, NJ : Wiley, 2015) Zeiger, Marco; Weingarth, Daniel; Presser, VolkerThe energy performance of carbon onions can be significantly enhanced by introducing pseudocapacitive materials, but this is commonly at the cost of power handling. In this study, a novel synergistic electrode preparation method was developed by using carbon-fiber substrates loaded with quinone-decorated carbon onions. The electrodes are free standing, binder free, extremely conductive, and the interfiber space filling overcomes the severely low apparent density commonly found for electrospun fibers. Electrochemical measurements were performed in organic and aqueous electrolytes. For both systems, a high electrochemical stability after 10 000 cycles was measured, as well as a long-term voltage floating test for the organic electrolyte. The capacitance in 1 M H2SO4 was 288 F g^−1 for the highest loading of quinones, which is similar to literature values, but with a very high power handling, showing more than 100 F g^−1 at a scan rate of 2 Vs^−1.
- ItemElectrospinning and electrospraying of silicon oxycarbide-derived nanoporous carbon for supercapacitor electrodes(Amsterdam : Elsevier, 2016) Tolosa, Aura; Krüner, Benjamin; Jäckel, Nicolas; Aslan, Mesut; Vakifahmetoglu, Cekdar; Presser, VolkerIn this study, carbide-derived carbon fibers from silicon oxycarbide precursor were synthesized by electrospinning of a commercially available silicone resin without adding a carrier polymer for the electrospinning process. The electrospun fibers were pyrolyzed yielding SiOC. Modifying the synthesis procedure, we were able to obtain electrosprayed SiOC beads instead of fibers. After chlorine treatment, nanoporous carbon with a specific surface area of up to 2394 m2·g-1 was obtained (3089 m2·g-1 BET). Electrochemical characterization of the SiOC-CDC either as free-standing fiber mat electrodes or polymer-bound bead films was performed in 1 M tetraethylammonium tetrafluoroborate in acetonitrile (TEA-BF4 in ACN). The electrospun fibers presented a high gravimetric capacitance of 135 F·g-1 at 10 mV·s-1 and a very high power handling, maintaining 63 % of the capacitance at 100 A·g-1. Comparative data of SiOC-CDC beads and fibers show enhanced power handling for fiber mats only when the fiber network is intact, that is, a lowered performance was observed when using crushed mats that employ polymer binder.
- ItemReview: Carbon onions for electrochemical energy storage(Cambridge : Royal Society of Chemistry, 2016) Zeiger, Marco; Jäckel, Nicolas; Mochalin, Vadym N.; Presser, VolkerCarbon onions are a relatively new member of the carbon nanomaterials family. They consist of multiple concentric fullerene-like carbon shells which are highly defective and disordered. Due to their small size of typically below 10 nm, the large external surface area, and high conductivity they are used for supercapacitor applications. As electrode materials, carbon onions provide fast charge/discharge rates resulting in high specific power but present comparatively low specific energy. They improve the performance of activated carbon electrodes as conductive additives and show suitable properties as substrates for redox-active materials. This review provides a critical discussion of the electrochemical properties of different types of carbon onions as electrode materials. It also compares the general advantages and disadvantages of different carbon onion synthesis methods. The physical and chemical properties of carbon onions, in particular nanodiamond-derived carbon onions, are described with emphasis on those parameters especially important for electrochemical energy storage systems, including the structure, conductivity, and porosity. Although the primary focus of current research is on electrode materials for supercapacitors, the use of carbon onions as conductive additives and for redox-active species is also discussed.
- ItemSub-micron novolac-derived carbon beads for high performance supercapacitors and redox electrolyte energy storage(Washington D.C. : American Chemical Society, 2016) Krüner, Benjamin; Lee, Juhan; Jäckel, Nicolas; Tolosa, Aura; Presser, VolkerCarbon beads with sub-micrometer diameter were produced with a self-emulsifying novolac–ethanol–water system. A physical activation with CO2 was carried out to create a high microporosity with a specific surface area varying from 771 (DFT) to 2237 m2/g (DFT) and a total pore volume from 0.28 to 1.71 cm3/g. The carbon particles conserve their spherical shape after the thermal treatments. The controllable porosity of the carbon spheres is attractive for the application in electrochemical double layer capacitors. The electrochemical characterization was carried out in aqueous 1 M Na2SO4 (127 F/g) and organic 1 M tetraethylammonium tetrafluoroborate in propylene carbonate (123 F/g). Furthermore, an aqueous redox electrolyte (6 M KI) was tested with the highly porous carbon and a specific energy of 33 W·h/kg (equivalent to 493 F/g) was obtained. In addition to a high specific capacitance, the carbon beads also provide an excellent rate performance at high current and potential in all tested electrolytes, which leads to a high specific power (>11 kW/kg) with an electrode thickness of ca. 200 μm.
- ItemInfluence of carbon substrate on the electrochemical performance of carbon/manganese oxide hybrids in aqueous and organic electrolytes(Cambridge : Royal Society of Chemistry, 2016) Zeiger, Marco; Fleischmann, Simon; Krüner, Benjamin; Tolosa, Aura; Bechtel, Stephan; Baltes, Mathias; Schreiber, Anna; Moroni, Riko; Vierrath, Severin; Thiele, Simon; Presser, VolkerManganese oxide presents very promising electrochemical properties as an electrode material in supercapacitors, but there remain important open questions to guide further development of the complex manganese oxide/carbon/electrolyte system. Our work addresses specifically the influence of carbon ordering and the difference between outer and inner porosity of carbon particles for the application in aqueous 1 M Na2SO4 and 1 M LiClO4 in acetonitrile. Birnessite-type manganese oxide was hydrothermally hybridized on two kinds of carbon onions with only outer surface area and different electrical conductivity, and conventional activated carbon with a high inner porosity. Carbon onions with a high degree of carbon ordering, high conductivity, and high outer surface area were identified as the most promising material, yielding 179 F g−1. Pore blocking in activated carbon yields unfavorable electrochemical performances. The highest specific energy of 16.4 W h kg−1 was measured for a symmetric full-cell arrangement of manganese oxide coated high temperature carbon onions in the organic electrolyte. High stability during 10 000 cycles was achieved for asymmetric full-cells, which proved as a facile way to enhance the electrochemical performance stability.
- ItemCarbon onion–sulfur hybrid cathodes for lithium–sulfur batteries(Cambridge : Royal Society of Chemistry, 2017) Choudhury, Soumyadip; Zeiger, Marco; Massuti-Ballester, Pau; Fleischmann, Simon; Formanek, Petr; Borchardt, Lars; Presser, VolkerIn this study, we explore carbon onions (diameter below 10 nm), for the first time, as a substrate material for lithium sulfur cathodes. We introduce several scalable synthesis routes to fabricate carbon onion–sulfur hybrids by adopting in situ and melt diffusion strategies with sulfur fractions up to 68 mass%. The conducting skeleton of agglomerated carbon onions proved to be responsible for keeping active sulfur always in close vicinity to the conducting matrix. Therefore, the hybrids are found to be efficient cathodes for Li–S batteries, yielding 97–98% Coulombic efficiency over 150 cycles with a slow fading of the specific capacity (ca. 660 mA h g−1 after 150 cycles) in long term cycle test and rate capability experiments.
- ItemReview on the science and technology of water desalination by capacitive deionization(Amsterdam : Elsevier, 2013) Presser, Volker; Porada, S.; Zhao, R.; van der Wal, A.; Biesheuvel, P.M.Porous carbon electrodes have significant potential for energy-efficient water desalination using a promising technology called Capacitive Deionization (CDI). In CDI, salt ions are removed from brackish water upon applying an electrical voltage difference between two porous electrodes, in which the ions will be temporarily immobilized. These electrodes are made of porous carbons optimized for salt storage capacity and ion and electron transport. We review the science and technology of CDI and describe the range of possible electrode materials and the various approaches to the testing of materials and devices. We summarize the range of options for CDI-designs and possible operational modes, and describe the various theoretical–conceptual approaches to understand the phenomenon of CDI.
- ItemCarbon onion / sulfur hybrid cathodes via inverse vulcanization for lithium sulfur batteries(Cambridge : Royal Society of Chemistry, 2017) Choudhury, Soumyadip; Srimuk, Pattarachai; Raju, Kumar; Tolosa, Aura; Fleischmann, Simon; Zeiger, Marco; Ozoemena, Kenneth I.; Borchardt, Lars; Presser, VolkerA sulfur–1,3-diisopropenylbenzene copolymer was synthesized by ring-opening radical polymerization and hybridized with carbon onions at different loading levels. The carbon onion mixing was assisted by shear in a two-roll mill to capitalize on the softened state of the copolymer. The sulfur copolymer and the hybrids were thoroughly characterized in structure and chemical composition, and finally tested by electrochemical benchmarking. An enhancement of specific capacity was observed over 140 cycles at higher content of carbon onions in the hybrid electrodes. The copolymer hybrids demonstrate a maximum initial specific capacity of 1150 mA h gsulfur−1 (850 mA h gelectrode−1) and a low decay of capacity to reach 790 mA h gsulfur−1 (585 mA h gelectrode−1) after 140 charge/discharge cycles. All carbon onion/sulfur copolymer hybrid electrodes yielded high chemical stability, stable electrochemical performance superior to conventional melt-infiltrated reference samples having similar sulfur and carbon onion content. The amount of carbon onions embedded in the sulfur copolymer has a strong influence on the specific capacity, as they effectively stabilize the sulfur copolymer and sterically hinder the recombination of sulfur species to the S8 configuration.