A new cell design has been developed using a standard Swagelok cell for Li-ion battery material characterisation, which has been modified by replacing one of the electrode cylindrical plungers with an adaptor to a pressure sensor. By simplifying the cell design (no valves or unnecessary connectors have been included), the cell headspace volume is kept at a minimum (ca. 1.9 ml for a one-inch-diameter cell) which produces a dramatic increase in sensitivity of the measurements with respect to conventional set-ups. Changes in pressure induced by Li-ion battery materials processes (gas evolution, structural changes in volume of the battery material due to Li-ion insertion/extraction) are monitored with unprecedented sensitivity. Here we illustrate the application of this novel cell design for the operando pressure measurements of LiFePO4 and graphite in Li half-cell configurations, and detailed procedures of cell calibration, protocols for cell preparation and assembly and technical drawings of the cell parts are provided to facilitate the adoption of this technique for testing new battery materials. We also demonstrate the high sensitivity of this new set-up to study the corrosion of cell materials in contact with LiPF6-containing electrolytes, which had not been explored before with operando pressure measurements.
Dye-sensitised Schottky junction cells were fabricated on stainless steel using TiO2 and silver nanowires. A titania sol was synthesised by a sol-gel process and was deposited on the substrate by dip coating, followed by sintering at 350°C for grade 304 stainless steel. Silver nanowires were drop cast from suspension and annealed. The current-voltage characteristics were measured and fit to the diode equation. The average I0 value for a typical batch of anatase devices was 4.9 × 10-6 A cm-2. The devices showed a UV response after treatment with tartaric acid and showed EQEs of 7.0 % in the UV at single wavelengths. It was possible to measure a small visible photocurrent for these devices following functionalisation with a ruthenium dye.
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