Towards enhanced sodium storage of anatase TiO2via a dual-modification approach of Mo doping combined with AlF3 coating.

Recent studies on anatase TiO2 have demonstrated its capability of performing as an anode material for sodium-ion batteries (SIBs) even though, due to poor conductivity, realistic applications have not yet been foreseen. In order to try to address this issue, herein, we shall introduce a cost effective and facile route based on the co-precipitation method for the synthesis of Mo-doped anatase TiO2 nanoparticles with AlF3 surface coating. The electrochemical measurements demonstrate that the Mo-doped anatase TiO2 nanoparticles deliver an ∼40% enhanced reversible capacity compared to pristine TiO2 (139.8 vs. 100.7 mA h g-1 at 0.1 C after 50 cycles) due to an improved electronic/ionic conductivity. Furthermore, upon AlF3 coating, the overall system can deliver a much higher reversible capacity of 178.9 mA h g-1 (∼80% increase with respect to pristine TiO2) with good cycling stability and excellent rate capabilities of up to 10 C. The experimental results indicate that the AlF3 surface coating could indeed effectively reduce the solid electrolyte interfacial resistance, enhance the electrochemical reactivity at the surface/interface region, and lower the polarization during cycling. The improved performance achieved using a cost-effective fabrication approach makes the dually modified anatase TiO2 a promising anode material for high-performance SIBs.

Evolution of 3D Printing Methods and Materials for Electrochemical Energy Storage.

Additive manufacturing has revolutionized the building of materials, and 3D-printing has become a useful tool for complex electrode assembly for batteries and supercapacitors. The field initially grew from extrusion-based methods and quickly evolved to photopolymerization printing, while supercapacitor technologies less sensitive to solvents more often involved material jetting processes. The need to develop higher-resolution multimaterial printers is borne out in the performance data of recent 3D printed electrochemical energy storage devices. Underpinning every part of a 3D-printable battery are the printing method and the feed material. These influence material purity, printing fidelity, accuracy, complexity, and the ability to form conductive, ceramic, or solvent-stable materials. The future of 3D-printable batteries and electrochemical energy storage devices is reliant on materials and printing methods that are co-operatively informed by device design. Herein, the material and method requirements in 3D-printable batteries and supercapacitors are addressed and requirements for the future of the field are outlined by linking existing performance limitations to requirements for printable energy-storage materials, casings, and direct printing of electrodes and electrolytes. A guide to materials and printing method choice best suited for alternative-form-factor energy-storage devices to be designed and integrated into the devices they power is thus provided.

Facile Synthesis of Highly Graphitized Carbon via Reaction of CaC2 with Sulfur and Its Application for Lithium/Sodium-Ion Batteries.

In the present work, we report, for the first time, a novel one-step approach to prepare highly graphitized carbon (HGC) material by selectively etching calcium from calcium carbide (CaC2) using a sulfur-based thermo-chemical etching technique. Comprehensive analysis using X-ray diffraction, Raman spectroscopy, X-ray photoelectron spectroscopy, and N2 adsorption-desorption isotherms reveals a highly graphitized mesoporous structure for the CaC2-derived carbon with a specific surface area of 159.5 m2 g-1. Microscopic analysis displays micron-scale mesoporous frameworks (4-20 µm) with a distinct layered structure along with agglomerates of highly graphitized nanosheets (about 10 nm in thickness and 1-10 µm lateral size). The as-prepared HGC is investigated for the role of an anode material for lithium- and sodium-ion batteries. We found that HGC exhibits good lithium storage performance in the 0.01-1.5 V range (reversible capacity of 272.4 mA h g-1 at 50 mA g-1 after 100 cycles and 214.2 mA h g-1 at 500 mA g-1 after 500 cycles), whereas, when sodium is considered, we observed a drop in the overall electrochemical performance owing to the high graphitization degree. More importantly, the present study provides a perspective approach to fabricate HGC via a simple, cost-effective, and efficient synthetic route using CaC2 and sulfur as reactants.

Nitrogen-Doped Single-Walled Carbon Nanohorns as a Cost-Effective Carbon Host toward High-Performance Lithium-Sulfur Batteries.

Nitrogen-doped single-walled carbon nanohorns (N-SWCNHs) are porous carbon material characterized by unique horn-shape structures with high surface areas and good conductivity. Moreover, they can be mass-produced (tons/year) using a novel proprietary process technology making them an attractive material for various industrial applications. One of the applications is the encapsulation of sulfur, which turns them as promising conductive host materials for lithium-sulfur batteries. Therefore, we explore for the first time the electrochemical performance of industrially produced N-SWCNHs as a sulfur-encapsulating conductive material. Fabrication of lithium-sulfur cells based on N-SWCNHs with sulfur composite could achieve a remarkable initial gravimetric capacity of 1650 mA h g-1, namely equal to 98.5% of the theoretical capacity (1675 mA h g-1), with an exceptional sulfur content as high as 80% in weight. Using cyclic chronopotentiometry and impedance spectroscopy, we also explored the dissolution mechanism of polysulfides inside the electrolyte.

Effective separation and simultaneous analysis of anabolic androgenic steroids (AAS) in their pharmaceutical formulations by a validated TLC-densitometry method.

BACKGROUND: Anabolic androgenic steroids (AAS) are widely misused for the enhancement of performance in sports. Several drugs are available that contain different combinations or individual steroids in different dosage form. This paper describes a TLC densitometric method for simultaneous determination of four AAS of testosterone derivatives including testosterone propionate (TP), testosterone phenyl propionate (TPP), testosterone isocaproate (TI) and testosterone deaconate (TD) in their pharmaceutical products. RESULTS: Separation was carried out on Al based TLC plates, pre-coated with silica gel 60F-254 using hexane and ethyl acetate (8.5:1.5, v/v). Spots at Rf 0.31 ± 0.01, 0.34 ± 0.01, 0.40 ± 0.01 and 0.45 ± 0.02 were recognized as TPP, TP, TI and TD, respectively. Quantitative analysis was done by densitometric measurements at λmax 251 nm for all derivatives. The developed method was validated as per ICH guidelines. Method was found linear over the concentration range of 200-1200 ng/spot with the correlation coefficient of 0.995, 0.993, 0.995 and 0.996 for TP, TPP, TI, TD, respectively. Limit of detection for all derivatives were in the range of 16.7-22.3 ng/spot while limit of quantitation were found to be in the range of 55.7-70.9 ng/spot. CONCLUSIONS: The developed TLC method can be applied for the simultaneous routine analysis of testosterone derivatives in their individual and combined pharmaceutical formulations.

Effective separation and analysis of E- and Z-guggulsterones in Commiphora mukul resin, guggulipid and their pharmaceutical product by high performance thin-layer chromatography-densitometric method.

A high performance thin-layer chromatographic (HPTLC) method for the simultaneous determination of the hypolipidemic agents, E- and Z-isomers of guggulsterone in Commiphora mukul resin, guggulipid (ethyl acetate extract of resin), and its pharmaceutical formulation, was developed. The developed system was efficient enough to separate both isomers from their conger, 17,20-dihydroguggulsterone. HPTLC glass plates, pre-coated with silica gel 60F-254, were used as a stationary phase. The mobile phase consisted of toluene:acetone (9.3:0.7, v/v) which gave well resolved spots for E- and Z-guggulsterones (R(f): 0.52±0.01, and 0.67±0.01, respectively) following double development of chromatoplate with the same mobile phase under unsaturated conditions. The analyte stability towards the developed chromatographic procedure was also investigated by two-dimensional (2D) HPTLC analysis. 17,20-Dihydroguggulsterone (3) was identified by the electrospray ionization quadrupole time-of-flight tandem mass spectrometry (ESI-QTOF-MS/MS) analysis.