Parstat mc potentiostat

The as-prepared nanocrystalline Li[In_xLi_y]Br₄ was pressed into a cylindrical pellet (d = 8 mm, h = 1.51 mm) under uniaxial pressure (0.3 GPa). Pt electrodes were applied on both sides via sputtering. Due to its hygroscopic character, the pellet with this electrode sandwich configuration was mounted in an air-tight Swagelok-type cell. We prepared the pellet and the cell in a glovebox (O₂, H₂O < 0.1 ppm) and subsequently placed the cell in a drying oven at 60°C. The cell was then connected to a Parstat MC potentiostat (Princeton Applied Research), which is equipped with a low-current option. We applied a constant voltage U of 300 mV and measured the change of current I(t) over time.

For all-solid-state cyclic voltammetry measurements approximately 120 mg of the sample powder were pressed into cylindrical pellets with a diameter of 8 mm. After uni-axial pressing (0.4 t) the thickness of the pellets ranged from 0.9 to 1 mm. As reference and counter electrode (CE) different materials of high purity (Au, Ag, Cu, Pt, Ni) were sputtered on one complete side of the pellets. We studied pellets equipped with sputtered working electrodes (Leica, EM SCD050) of the following diameters d: 2.5, 4, 6 and 8 mm. Again, all preparation steps were carried out in a glovebox filled with Ar (H ${}_2$ O, O ${}_2$ < 0.5 ppm). The sample chamber of the sputter device was purged with Ar 5.0 for five times before the sputter process was started to avoid any contamination with moisture or O ${}_2$ . Cyclic voltammetry was performed with a Parstat MC potentiostat (Princeton Applied Research) equipped with a low-current option. We carried out all measurements at a temperature of 200 ${}^{\circ }$ C in a cell, which was continuously purged with N ${}_2$ . Scanning rates ranged from 0.002 to 0.1 V/s whereby the voltage was varied from −1 V to 4 V. A schematic drawing of the cell set-up is shown in Figure A1.