Microwave Crystallization of Lithium Aluminum Germanium Phosphate Solid-State Electrolyte.

Lithium aluminum germanium phosphate (LAGP) glass-ceramics are considered as promising solid-state electrolytes for Li-ion batteries. LAGP glass was prepared via the regular conventional melt-quenching method. Thermal, chemical analyses and X-ray diffraction (XRD) were performed to characterize the prepared glass. The crystallization of the prepared LAGP glass was done using conventional heating and high frequency microwave (MW) processing. Thirty GHz microwave (MW) processing setup were used to convert the prepared LAGP glass into glass-ceramics and compared with the conventionally crystallized LAGP glass-ceramics that were heat-treated in an electric conventional furnace. The ionic conductivities of the LAGP samples obtained from the two different routes were measured using impedance spectroscopy. These samples were also characterized using XRD and scanning electron microscopy (SEM). Microwave processing was successfully used to crystallize LAGP glass into glass-ceramic without the aid of susceptors. The MW treated sample showed higher total, grains and grain boundary ionic conductivities values, lower activation energy and relatively larger-grained microstructure with less porosity compared to the corresponding conventionally treated sample at the same optimized heat-treatment conditions. The enhanced total, grains and grain boundary ionic conductivities values along with the reduced activation energy that were observed in the MW treated sample was considered as an experimental evidence for the existence of the microwave effect in LAGP crystallization process. MW processing is a promising candidate technology for the production of solid-state electrolytes for Li-ion battery.

Electrolyte Mixtures Based on Ethylene Carbonate and Dimethyl Sulfone for Li-Ion Batteries with Improved Safety Characteristics.

In this study, novel electrolyte mixtures for Li-ion cells are presented with highly improved safety features. The electrolyte formulations are composed of ethylene carbonate/dimethyl sulfone (80:20 wt/wt) as the solvent mixture and LiBF4 , lithium bis(trifluoromethanesulfonyl)azanide, and lithium bis(oxalato)borate as the conducting salts. Initially, the electrolytes are characterized with regard to their physical properties, their lithium transport properties, and their electrochemical stability. The key advantages of the electrolytes are high flash points of >140 °C, which enhance significantly the intrinsic safety of Li-ion cells containing these electrolytes. This has been quantified by measurements in an accelerating rate calorimeter. By using the newly developed electrolytes, which are liquid down to T=-10 °C, it is possible to achieve C-rates of up to 1.5 C with >80 % of the initial specific capacity. During 100 cycles in cell tests (graphite||LiNi1/3 Co1/3 Mn1/3 O2 ), it is proven that the retention of the specific capacity is >98 % of the third discharge cycle with dependence on the conducting salt. The best electrolyte mixture yields a capacity retention of >96 % after 200 cycles in coin cells.

Sputter deposition of nanocrystalline beta-SiC films and molecular dynamics simulations of the sputter process.

Thin nanocrystalline films of silicon carbide (SiC) have been deposited on Si substrates by rf magnetron sputtering in pure Ar atmosphere. Simultaneously classical molecular dynamics (MD) simulations of sputtering of beta-SiC by Ar atoms were performed using IMD and Materials Explorer software with a combination of the Tersoff and the Ziegler-Biersack-Littmark (ZBL) potential in order to get more insight into the sputter process. In experiments the bias voltage (0 to -40 V) has been varied at constant substrate temperature of 900 degrees C to investigate the influence on the composition, the constitution and the mechanical properties of crystalline beta-SiC films. At second the substrate temperature has been varied between 900 degrees C and 100 degrees C to find the minimum substrate temperature that is needed to get nanocrystalline beta-SiC under the applied sputter conditions (ceramic SiC target, 300 W rf power, 18 cm target-substrate distance, 50 sccm Ar gas flow, 0.26 Pa total gas pressure). The films have been characterized by electron probe micro-analysis (EPMA), X-ray diffraction (XRD), Raman spectroscopy and atomic force microscopy (AFM). Hardness and residual stress have been investigated by nanoindentation and wafer bending. In the MD simulations the sputter yield was determined as a function of the energy of the incident Ar atoms (in the interesting range for sputter deposition, i.e., 50-1000 eV). To our knowledge this is the first time that the sputter yield of a SiC target was determined as a function of the energy of the incident Ar atoms in the low energy range by using MD simulations and compared with experimental results.