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Titanium dioxide high aspect ratio nanoparticle hydrothermal synthesis optimization

100%
Półrolniczak P., Walkowiak M.
Open Chemistry
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2015
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vol. 13
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issue 1
EN
TiO2-B (bronze) nanowires were synthesized via simple hydrothermal treatment of commercial titanium dioxide nanopowder in aqueous NaOH. The reaction temperature, calcination temperature, reaction time, NaOH concentration, autoclave filing fraction and precursor were systematically varied to optimize the nanowire morphology. The crystal structure, morphology and particle size were investigated by XRD, SEM and TEM. The morphology and structure are sensitive to experimental conditions. A reaction temperature of at least 150°C and NaOH concentration at least 10 M are essential, but reaction time from 24 to 72 h makes little difference. Nanowires obtained at 150°C were 60-180 nm wide and 2-4 μm long, while those after treatment at 200°C were thinner (40-100 nm) and longer (2-6 μm). The relationship between reaction conditions and morphology is discussed and practical guidelines for titanium dioxide nanowire synthesis are suggested
2
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Synthesis and characterization of a new hybrid TiO2/SiO2 filler for lithium conducting gel electrolytes

81%
Walkowiak M., Osińska M., Jesionowski T., Siwińska-Stefańska K.
Open Chemistry
|
2010
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vol. 8
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issue 6
1311-1317
EN
This paper describes the synthesis and properties of a new type of ceramic fillers for composite polymer gel electrolytes. Hybrid TiO2-SiO2 ceramic powders have been obtained by co-precipitation from titanium(IV) sulfate solution using sodium silicate as the precipitating agent. The resulting submicron-size powders have been applied as fillers for composite polymer gel electrolytes for Li-ion batteries based on poly(vinylidene fluoride-co-hexafluoropropylene) (PVdF/HFP) copolymeric membranes. The powders, dry membranes and gel electrolytes have been examined structurally and electrochemically, showing favorable properties in terms of electrolyte uptake and electrochemical characteristics in Li-ion cells.
3
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Impact of selected supramolecular additives on the initial electrochemical lithium intercalation into graphite in propylene carbonate

81%
Walkowiak M., Waszak D., Gierczyk B., Schroeder G.
Open Chemistry
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2008
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vol. 6
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issue 4
600-606
EN
Impact of silicon tripodand-type electrolyte additives and graphite pre-treatment agents on the electrochemical intercalation of lithium cations into graphite was investigated. Addition of Si-tripodand-type silanes to propylene carbonate-based electrolytes was found to suppress detrimental solvent co-intercalation and graphite exfoliation. Similar effects were observed for graphite pre-treated with the reported silane agents. It was observed that the presented supramolecular additives allow for the formation of effective passive layers on graphite during first charging, and thus can be considered as novel low-cost film-forming components for rechargeable lithium batteries. [...]
4
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Graphene oxide-assisted synthesis of LiMn2O4nanopowder

71%
Majchrzycki Ł., Michalska M., Walkowiak M., Wiliński Z., Lipińska L.
Polish Journal of Chemical Technology
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2013
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vol. 15
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issue 3
15-19
EN
The article reports sol-gel synthesis of nanosized spinel-type lithium manganese oxide LiMn2O4 (LMO) carried out in the presence of graphene oxide (GO) and its electrochemical lithium insertion ability. The synthesis was performed in an aqueous environment with lithium acetate and manganese acetate used as precursors and citric acid as a chelating agent. The material was characterized by X-ray diffraction, SEM microscopy, Raman spectroscopy and cyclic voltammetry. The calcination step totally eliminated graphene from the final product, nevertheless its presence during the synthesis was found to affect the resulting LiMn2O4 morphology by markedly reducing the size of grains. Moreover, potentials of electrochemical lithium insertion/deinsertion reactions have been shifted, as observed in the cyclic voltammetry measurements. Along with the diminished grain size the voltammetric curves of the graphene oxide-modified material exhibit higher oxidation and lower reduction peak currents. The study demonstrates that GO mediation/assistance during the sol-gel synthesis fosters more nanostructured powder and changes the electrochemical characteristics of the product
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