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- ItemVanadia–titania multilayer nanodecoration of carbon onions via atomic layer deposition for high performance electrochemical energy storage(Cambridge : Royal Society of Chemistry, 2016) Fleischamann, Simon; Tolosa, Aura; Zieger, Marco; Krüner, Benjamin; Peter, Nicolas J.; Grobelsek, Ingrid; Quade, Antje; Kruth, Angela; Presser, VolkerAtomic layer deposition has proven to be a particularly attractive approach for ecorating mesoporous carbon substrates with redox active metal oxides for lectrochemical energy storage. This study, for the first time, capitalizes on the cyclic character of atomic layer deposition to obtain highly conformal and atomically controlled decoration of carbon onions with alternating stacks of vanadia and titania. The addition of 25 mass% TiO2 leads to expansion of the VO2 unit cell, thus greatly enhancing lithium intercalation capacity and kinetics. Electrochemical characterization revealed an ultrahigh discharge capacity of up to 382 mA h g^-1 of the composite electrode (554 mA h g^-1 per metal oxide) with an impressive capacity retention of 82 mA h g^-1 (120 mA h g^-1 per metal oxide) at a high discharge rate of 20 A g^-1 or 52C. Stability benchmarking showed stability over 3000 cycles when discharging to a reduced potential of ^-1.8 V vs. carbon. These capacity values are among the highest reported for any metal oxide system, while in addition, upercapacitor-like power performance and longevity are achieved. At a device level, high specific energy and power of up to 110 W h kg^-1 and 6 kW kg^-1, respectively, were achieved when employing the hybrid material as anode versus activated carbon cathode.
- ItemNiobium carbide nanofibers as a versatile precursor for high power supercapacitor and high energy battery electrodes(London [u.a.] : RSC, 2016) Tolosa, Aura; Krüner, Benjamin; Fleischmann, Simon; Jäckel, Nicolas; Zeiger, Marco; Aslan, Mesut; Grobelsek, Ingrid; Presser, VolkerThis study presents electrospun niobium carbide/carbon (NbC/C) hybrid nanofibers, with an average diameter of 69 ± 30 nm, as a facile precursor to derive either highly nanoporous niobium carbide-derived carbon (NbC–CDC) fibers for supercapacitor applications or niobium pentoxide/carbon (Nb2O5/C) hybrid fibers for battery-like energy storage. In all cases, the electrodes consist of binder-free and free-standing nanofiber mats that can be used without further conductive additives. Chlorine gas treatment conformally transforms NbC nanofiber mats into NbC–CDC fibers with a specific surface area of 1508 m2 g−1. These nanofibers show a maximum specific energy of 19.5 W h kg−1 at low power and 7.6 W h kg−1 at a high specific power of 30 kW kg−1 in an organic electrolyte. CO2 treatment transforms NbC into T-Nb2O5/C hybrid nanofiber mats that provide a maximum capacity of 156 mA h g−1. The presence of graphitic carbon in the hybrid nanofibers enabled high power handling, maintaining 50% of the initial energy storage capacity at a high rate of 10 A g−1 (64 C-rate). When benchmarked for an asymmetric full-cell, a maximum specific energy of 86 W h kg−1 was obtained. The high specific power for both systems, NbC–CDC and T-Nb2O5/C, resulted from the excellent charge propagation in the continuous nanofiber network and the high graphitization of the carbon structure.
- ItemEnhanced capacitance of nitrogen-doped hierarchically porous carbide-derived carbon in matched ionic liquids(Cambridge : Royal Society of Chemistry, 2015) Ewert, Julia K.; Weingarth, Daniel; Denner, Christine; Friedrich, Martin; Zeiger, Marco; Schreiber, Anna; Jäckel, Nicolas; Presser, Volker; Kempe, RhettSupercapacitors combine efficient electrical energy storage and performance stability based on fast electrosorption of electrolyte ions at charged interfaces. They are a central element of existing and emerging energy concepts. A better understanding of capacitance enhancement options is essential to exploit the full potential of supercapacitors. Here, we report a novel hierarchically structured N-doped carbon material and a significant capacitance enhancement for a specific ionic liquid. Our studies indicate that matching of the electrode material and the ionic liquid specifically leads to a constant normalized resistance of the electrode material (voltage window up to ±1 V vs. carbon) and a significant enhancement of the specific capacitance. Such effects are not seen for standard organic electrolytes, non-matched ionic liquids, or non-N-doped carbons. A higher N-doping of the electrode material improves the symmetric full cell capacitance of the match and considerably increases its long-term stability at +3 V cell voltage. This novel observance of enhanced specific capacitance for N-doped carbons with matched ionic liquid may enable a new platform for developing supercapacitors with enhanced energy storage capacity.
- ItemNuclear magnetic resonance study of ion adsorption on microporous carbide-derived carbon(Cambridge : Royal Society of Chemistry, 2013) Presser, Volker; Forse, Alexander C.; Griffin, John M.; Wang, Hao; Trease, Nicole M.; Gogotsi, Yuri; Simon, Patrice; Grey, Clare P.A detailed understanding of ion adsorption within porous carbon is key to the design and improvement of electric double-layer capacitors, more commonly known as supercapacitors. In this work nuclear magnetic resonance (NMR) spectroscopy is used to study ion adsorption in porous carbide-derived carbons. These predominantly microporous materials have a tuneable pore size which enables a systematic study of the effect of pore size on ion adsorption. Multinuclear NMR experiments performed on the electrolyte anions and cations reveal two main environments inside the carbon. In-pore ions (observed at low frequencies) are adsorbed inside the pores, whilst ex-pore ions (observed at higher frequencies) are not adsorbed and are in large reservoirs of electrolyte between carbon particles. All our experiments were carried out in the absence of an applied electrical potential in order to assess the mechanisms related to ion adsorption without the contribution of electrosorption. Our results indicate similar adsorption behaviour for anions and cations. Furthermore, we probe the effect of sample orientation, which is shown to have a marked effect on the NMR spectra. Finally, we show that a 13C → 1H cross polarisation experiment enables magnetisation transfer from the carbon architecture to the adsorbed species, allowing selective observation of the adsorbed ions and confirming our spectral assignments.
- ItemUpcycling spent petroleum cracking catalyst: pulsed laser deposition of single-wall carbon nanotubes and silica nanowires(Cambridge : Royal Society of Chemistry, 2016) Souza, Nicolas; Lasserre, Féderico; Blickley, Adam; Suárez, Sebastian; Duarte, Martín; Presser, Volker; Mücklich, FrankFluid catalytic cracking (FCC), which currently accounts for half of the worldwide petroleum refining efforts, relies on catalytic, aluminosilicate zeolite particles which slowly deactivate. As of yet, this FCC catalyst residue (FC3R) has no commercial outlet, resulting in abundant amounts of landfill-destined refuse. However, this overlooked waste has the right ingredients for the synthesis of some of today's emerging nanomaterials. High-carbon FC3R, sourced from a Uruguayan refinery, was identified as faujasite particles encased in graphitic carbon shells. We show that pulsed laser ablation of raw FC3R produces simultaneous deposition of single-wall carbon nanotubes and silica nanowires through vapour/solid–liquid–solid self-assembly in distinct zones of an oven-laser apparatus. This is an extreme revalorisation and provides a new untapped resource for research and applications in C- and Si-based nanomaterials and mesoscopic physics.
- ItemThermal conductivity and temperature profiles in carbon electrodes for supercapacitors(Amsterdam : Elsevier, 2014) Burheim, Odne S.; Aslan, Mesut; Atchison, Jennifer S.; Presser, VolkerThe thermal conductivity of supercapacitor film electrodes composed of activated carbon (AC), AC with 15 mass% multi-walled carbon nanotubes (MWCNTs), AC with 15 mass% onion-like carbon (OLC), and only OLC, all mixed with polymer binder (polytetrafluoroethylene), has been measured. This was done for dry electrodes and after the electrodes have been saturated with an organic electrolyte (1 M tetraethylammonium-tetrafluoroborate in acetonitrile, TEA-BF4). The thermal conductivity data was implemented in a simple model of generation and transport of heat in a cylindrical cell supercapacitor systems. Dry electrodes showed a thermal conductivity in the range of 0.09-0.19 W K-1 m-1 and the electrodes soaked with an organic electrolyte yielded values for the thermal conductivity between 0.42 and 0.47 W K-1 m-1. It was seen that the values related strongly to the porosity of the carbon electrode materials. Modeling of the internal temperature profiles of a supercapacitor under conditions corresponding to extreme cycling demonstrated that only a moderate temperature gradient of several degrees Celsius can be expected and which depends on the ohmic resistance of the cell as well as the wetting of the electrode materials.
- ItemAn electrochemical in situ study of freezing and thawing of ionic liquids in carbon nanopores(Cambridge : Royal Society of Chemistry, 2014) Weingarth, Daniel; Drumm, Robert; Foelske-Schmitz, Annette; Kotz, Rüdiger; Presser, VolkerRoom temperature ionic liquids (RTILs) are an emerging class of electrolytes enabling high cell voltages and, in return, high energy density of advanced supercapacitors. Yet, the low temperature behavior, including freezing and thawing, is little understood when ions are confined in the narrow space of nanopores. This study shows that RTILs may show a tremendously different thermal behavior when comparing bulk with nanoconfined properties as a result of the increased surface energy of carbon pore walls. In particular, a continuous increase in viscosity is accompanied by slowed-down charge-discharge kinetics as seen with in situ electrochemical characterization. Freezing reversibly collapses the energy storage ability and thawing fully restores the initial energy density of the material. For the first time, a different thermal behavior in positively and negatively polarized electrodes is demonstrated. This leads to different freezing and melting points in the two electrodes. Compared to bulk, RTILs in the confinement of electrically charged nanopores show a high affinity for supercooling; that is, the electrode may freeze during heating.
- ItemHigh performance stability of titania decorated carbon for desalination with capacitive deionization in oxygenated water(London : RSC Publishing, 2016) Srimuk, Pattarachai; Ries, Lucie; Zeiger, Marco; Fleischmann, Simon; Jäckel, Nicolas; Tolosa, Aura; Krüner, Benjamin; Aslan, Mesut; Presser, VolkerPerformance stability in capacitive deionization (CDI) is particularly challenging in systems with a high amount of dissolved oxygen due to rapid oxidation of the carbon anode and peroxide formation. For example, carbon electrodes show a fast performance decay, leading to just 15% of the initial performance after 50 CDI cycles in oxygenated saline solution (5 mM NaCl). We present a novel strategy to overcome this severe limitation by employing nanocarbon particles hybridized with sol–gel-derived titania. In our proof-of-concept study, we demonstrate very stable performance in low molar saline electrolyte (5 mM NaCl) with saturated oxygen for the carbon/metal oxide hybrid (90% of the initial salt adsorption capacity after 100 cycles). The electrochemical analysis using a rotating disk electrode (RDE) confirms the oxygen reduction reaction (ORR) catalytic effect of FW200/TiO2, preventing local peroxide formation by locally modifying the oxygen reduction reaction.
- ItemCarbon aerogels with improved flexibility by sphere templating(Cambridge : Royal Society of Chemistry, 2018) Salihovic, Miralem; Hüsing, Nicola; Bernardi, Johannes; Presser, Volker; Elsaesser, Michael S.Mechanically reversible compressible resorcinol–formaldehyde (RF) aerogels can be converted into mechanically reversible compressible carbon aerogels (CA) by carbonization in an inert atmosphere. By incorporation of polystyrene spheres into the RF gels as a sacrificial template, it is possible to create macropores with controlled size within the carbon framework during carbonization. The resulting templated carbon aerogel shows enhanced mechanical flexibility during compression compared to pristine samples. In addition, the presence of hierarchical porosity provides a porous architecture attractive for energy storage applications, such as supercapacitors.
- ItemMXene as a novel intercalation-type pseudocapacitive cathode and anode for capacitive deionization(London [u.a.] : RSC, 2016) Srimuk, Pattarachai; Kaasik, Friedrich; Krüner, Benjamin; Tolosa, Aura; Fleischmann, Simon; Jäckel, Nicolas; Tekeli, Mehmet C.; Aslan, Mesut; Suss, Matthew E.; Presser, VolkerIn this proof-of-concept study, we introduce and demonstrate MXene as a novel type of intercalation electrode for desalination via capacitive deionization (CDI). Traditional CDI cells employ nanoporous carbon electrodes with significant pore volume to achieve a large desalination capacity via ion electrosorption. By contrast, MXene stores charge by ion intercalation between the sheets of its two-dimensional nanolamellar structure. By this virtue, it behaves as an ideal pseudocapacitor, that is, showing capacitive electric response while intercalating both anions and cations. We synthesized Ti3C2-MXene by the conventional process of etching ternary titanium aluminum carbide i.e., the MAX phase (Ti3AlC2) with hydrofluoric acid. The MXene material was cast directly onto the porous separator of the CDI cell without added binder, and exhibited very stable performance over 30 CDI cycles with an average salt adsorption capacity of 13 ± 2 mg g−1.
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