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- ItemDirectly Anodized Sulfur-Doped TiO2 Nanotubes as Improved Anodes for Li-ion Batteries(Basel : MDPI, 2020) Sabaghi, Davood; Madian, Mahmoud; Omar, Ahmad; Oswald, Steffen; Uhlemann, Margitta; Maghrebi, Morteza; Baniadam, Majid; Mikhailova, DariaTiO2 represents one of the promising anode materials for lithium ion batteries due to its high thermal and chemical stability, relatively high theoretical specific capacity and low cost. However, the electrochemical performance, particularly for mesoporous TiO2, is limited and must be further developed. Elemental doping is a viable route to enhance rate capability and discharge capacity of TiO2 anodes in Li-ion batteries. Usually, elemental doping requires elevated temperatures, which represents a challenge, particularly for sulfur as a dopant. In this work, S-doped TiO2 nanotubes were successfully synthesized in situ during the electrochemical anodization of a titanium substrate at room temperature. The electrochemical anodization bath represented an ethylene glycol-based solution containing NH4F along with Na2S2O5 as the sulfur source. The S-doped TiO2 anodes demonstrated a higher areal discharge capacity of 95 µAh·cm−2 at a current rate of 100 µA·cm−2 after 100 cycles, as compared to the pure TiO2 nanotubes (60 µAh·cm−2). S-TiO2 also exhibited a significantly improved rate capability up to 2500 µA·cm−2 as compared to undoped TiO2. The improved electrochemical performance, as compared to pure TiO2 nanotubes, is attributed to a lower impedance in S-doped TiO2 nanotubes (STNTs). Thus, the direct S-doping during the anodization process is a promising and cost-effective route towards improved TiO2 anodes for Li-ion batteries.
- ItemFlux Growth and Characterization of Bulk InVO4 Crystals(Basel : MDPI, 2023) Voloshyna, Olesia; Gorbunov, Mikhail V.; Mikhailova, Daria; Maljuk, Andrey; Seiro, Silvia; Büchner, BerndThe flux growth of InVO4 bulk single crystals has been explored for the first time. The reported eutectic composition at a ratio of V2O5:InVO4 = 1:1 could not be used as a self-flux since no sign of melting was observed up to 1100 °C. Crystals of InVO4 of typical size 0.5 × 1 × 7 mm3 were obtained using copper pyrovanadate (Cu2V2O7) as a flux, using Pt crucibles. X-ray powder diffraction confirmed the orthorhombic Cmcm structure. Rests of the flux material were observed on the sample surface, with occasional traces of Pt indicating some level of reaction with the crucible. X-ray absorption spectroscopy showed that oxidation states of indium and vanadium ions are +3 and +5, respectively. The size and high quality of the obtained InVO4 crystals makes them excellent candidates for further study of their physical properties.
- ItemSodium-Vanadium Bronze Na9V14O35: An Electrode Material for Na-Ion Batteries(Basel : MDPI, 2021) Kirsanova, Maria A.; Akmaev, Alexey S.; Gorbunov, Mikhail V.; Mikhailova, Daria; Abakumov, Artem M.Na9V14O35 (η-NaxV2O5) has been synthesized via solid-state reaction in an evacuated sealed silica ampoule and tested as electroactive material for Na-ion batteries. According to powder X-ray diffraction, electron diffraction and atomic resolution scanning transmission electron microscopy, Na9V14O35 adopts a monoclinic structure consisting of layers of corner- and edge-sharing VO5 tetragonal pyramids and VO4 tetrahedra with Na cations positioned between the layers, and can be considered as sodium vanadium(IV,V) oxovanadate Na9V104.1+O19(V5+O4)4. Behavior of Na9V14O35 as a positive and negative electrode in Na half-cells was investigated by galvanostatic cycling against metallic Na, synchrotron powder X-ray diffraction and electron energy loss spectroscopy. Being charged to 4.6 V vs. Na+/Na, almost 3 Na can be extracted per Na9V14O35 formula, resulting in electrochemical capacity of ~60 mAh g−1. Upon discharge below 1 V, Na9V14O35 uptakes sodium up to Na:V = 1:1 ratio that is accompanied by drastic elongation of the separation between the layers of the VO4 tetrahedra and VO5 tetragonal pyramids and volume increase of about 31%. Below 0.25 V, the ordered layered Na9V14O35 structure transforms into a rock-salt type disordered structure and ultimately into amorphous products of a conversion reaction at 0.1 V. The discharge capacity of 490 mAh g−1 delivered at first cycle due to the conversion reaction fades with the number of charge-discharge cycles.
- ItemStructural and Electrochemical Properties of Layered P2-Na0.8Co0.8Ti0.2O2 Cathode in Sodium-Ion Batteries(Basel : MDPI, 2022) Pohle, Björn; Gorbunov, Mikhail V.; Lu, Qiongqiong; Bahrami, Amin; Nielsch, Kornelius; Mikhailova, DariaLayered Na0.8Co0.8Ti0.2O2 oxide crystallizes in the β-RbScO2 structure type (P2 modification) with Co(III) and Ti(IV) cations sharing the same crystallographic site in the metal-oxygen layers. It was synthesized as a single-phase material and characterized as a cathode in Na- and Na-ion batteries. A reversible capacity of about 110 mA h g−1 was obtained during cycling between 4.2 and 1.8 V vs. Na+/Na with a 0.1 C current density. This potential window corresponds to minor structural changes during (de)sodiation, evaluated from operando XRD analysis. This finding is in contrast to Ti-free NaxCoO2 materials showing a multi-step reaction mechanism, thus identifying Ti as a structure stabilizer, similar to other layered O3- and P2-NaxCo1−yTiyO2 oxides. However, charging the battery with the Na0.8Co0.8Ti0.2O2 cathode above 4.2 V results in the reversible formation of a O2-phase, while discharging below 1.5 V leads to the appearance of a second P2-layered phase with a larger unit cell, which disappears completely during subsequent battery charge. Extension of the potential window to higher or lower potentials beyond the 4.2–1.8 V range leads to a faster deterioration of the electrochemical performance. After 100 charging-discharging cycles between 4.2 and 1.8 V, the battery showed a capacity loss of about 20% in a conventional carbonate-based electrolyte. In order to improve the cycling stability, different approaches including protective coatings or layers of the cathodic and anodic surface were applied and compared with each other.
- ItemA Facile Chemical Method Enabling Uniform Zn Deposition for Improved Aqueous Zn-Ion Batteries(Basel : MDPI, 2021) Liu, Congcong; Lu, Qiongqiong; Omar, Ahmad; Mikhailova, DariaRechargeable aqueous Zn-ion batteries (ZIBs) have gained great attention due to their high safety and the natural abundance of Zn. Unfortunately, the Zn metal anode suffers from dendrite growth due to nonuniform deposition during the plating/stripping process, leading to a sudden failure of the batteries. Herein, Cu coated Zn (Cu–Zn) was prepared by a facile pretreatment method using CuSO4 aqueous solution. The Cu coating transformed into an alloy interfacial layer with a high affinity for Zn, which acted as a nucleation site to guide the uniform Zn nucleation and plating. As a result, Cu–Zn demonstrated a cycling life of up to 1600 h in the symmetric cells and endowed a stable cycling performance with a capacity of 207 mAh g−1 even after 1000 cycles in the full cells coupled with a V2O5-based cathode. This work provides a simple and effective strategy to enable uniform Zn deposition for improved ZIBs.
- ItemPreparation and Application of ZIF-8 Thin Layers(Basel : MDPI, 2021) Schernikau, Martin; Sablowski, Jakob; Gonzalez Martinez, Ignacio Guillermo; Unz, Simon; Kaskel, Stefan; Mikhailova, DariaHerein we compare various preparation methods for thin ZIF-8 layers on a Cu substrate for application as a host material for omniphobic lubricant-infused surfaces. Such omniphobic surfaces can be used in thermal engineering applications, for example to achieve dropwise condensation or anti-fouling and anti-icing surface properties. For these applications, a thin, conformal, homogeneous, mechanically and chemically stable coating is essential. In this study, thin ZIF-8 layers were deposited on a Cu substrate by different routes, such as (i) electrochemical anodic deposition on a Zn-covered Cu substrate, (ii) doctor blade technique for preparation of a composite layer containing PVDF binder and ZIF-8, as well as (iii) doctor blade technique for preparation of a two-layer composite on the Cu substrate containing a PVDF-film and a ZIF-8 layer. The morphology and topography of the coatings were compared by using profilometry, XRD, SEM and TEM techniques. After infusion with a perfluorinated oil, the wettability of the surfaces was assessed by contact angle measurements, and advantages of each preparation method were discussed.
- ItemComparative Study of Onion-like Carbons Prepared from Different Synthesis Routes towards Li-Ion Capacitor Application(Basel : MDPI, 2022) Permana, Antonius Dimas Chandra; Ding, Ling; Gonzalez-Martinez, Ignacio Guillermo; Hantusch, Martin; Nielsch, Kornelius; Mikhailova, Daria; Omar, AhmadLi-ion capacitors (LIC) have emerged as a promising hybrid energy storage system in response to increasing energy demands. However, to achieve excellent LIC performance at high rates, along with cycling stability, an alternative anode to graphite is needed. Porous high-surface-area carbons, such as onion-like carbons (OLCs), have been recently found to hold high potential as high-rate-capable LIC anodes. However, a systematic understanding of their synthesis route and morphology is lacking. In this study, OLCs prepared from self-made metal organic frameworks (MOFs) Fe-BTC and Fe-MIL100 by a simple pyrolysis method were compared to OLCs obtained via high-temperature annealing of nanodiamonds. The LICs with OLCs produced from Fe-BTC achieved a maximum energy density of 243 Wh kg−1 and a power density of 20,149 W kg−1. Furthermore, excellent capacitance retention of 78% after 10,000 cycles was demonstrated. LICs with MOF-derived OLCs surpassed the energy and power density of LICs with nanodiamond-derived OLCs. We determined the impact of the MOF precursor structure and morphology on the resulting OLC properties, as well as on the electrochemical performance. Thus, MOF-derived OLCs offer significant potential toward high-performance anode material for LICs, enabling control over structure and morphology, as well as easy scalability for industrial implementation.
- ItemStructural Behaviour and Charge-Compensation Mechanism in Li2Fe1−xCoxSeO Solid Solutions during Reversible Delithiation(Basel : MDPI, 2024) Gorbunov, Mikhail V.; Mikhailova, DariaThe constantly growing demand for renewable electrical energy keeps the continuation of battery-related research imperative. In spite of significant progress made in the development of Na- and K-ion systems, Li-ion batteries (LIBs) still prevail in the fields of portative devices and electric or hybrid vehicles. Since the amount of lithium on our planet is significantly limited, studies dedicated to the search for and development of novel materials, which would make LIBs more efficient in terms of their specific characteristics and life lengths, are necessary. Investigations of less industry-related systems are also important, as they provide general knowledge which helps in understanding directions and strategies for the improvement of applied materials. The current paper represents a comprehensive study of cubic Li2Fe1−xCoxSeO compounds with an anti-perovskite structure. These solid solutions demonstrate both cationic and anionic electrochemical activity in lithium cells while being applied as cathodes. Cobalt cations remain inactive; however, their amount in the structure defines if the Se0/Se2− or Fe3+/Fe2+ redox couple dominates the charge compensation mechanism upon (de)lithiation. Apart from that, cobalt affects the structural stability of the materials during cycling. These effects were evaluated by means of operando XRD and XAS techniques. The outcomes can be useful for both fundamental and practice-relevant research.