Bandar seri begawan lithium-iron-phosphate batteries lfp
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(a) Schematic diagrams of the continuous hydrothermal flow synthesis reactor system. FeSO4 = Iron sulphate, VOSO4 = vanadium oxide sulphate hydrate and H3PO4 = phosphoric acid; P = pump; LiOH = Lithium hydroxide. (b) Outlines the mixing head, the central component of the apparatus where the reagents are combined.
The particles were recovered by centrifugation and washed with deionised water. The observed yield was 0.50 kg from 90 L of product suspension. The wet powder was freeze-dried and then subsequently heat-treated at 700 °C for 3 hours (under flowing argon) to graphitize the carbon coating on the surface of the particles. The carbon content of the carbon-coated V-LFP was calculated to be 6.7 wt % C from carbon-hydrogen-nitrogen (CHN) analysis. The material was ball-milled for 1 h at 400 rpm using a Retsch planetary ball mill PM-200 using a 1:1 w/w ratio of LFP and N-methyl pyrrolidone (NMP) with 4 mm zirconia balls. The particle size distribution as a result reduced from a D90 particle size of 650 μm to 22 μm.
Silicon electrodes were prepared in multiple steps as outlined below. The composite electrodes were based on a combination of Si (purity > 99%, Elkem Bremanger): PAA polymer (Sigma Aldrich, MWT = 450 k, purity ≥ 99.5%) and conductive additives acetylene black (Alfa Aesar, purity 99.9%, S.A. 75 m2 g−1 and FLG (XG Sciences M Grade, purity > 99.9%, specific surface area specified in the range 120–150 m2 g−1).
A conductive additive mixture was formulated using 10.0 g FLG, 5.0 g acetylene black, 136.4 g deionised water and 1.0 g of 12 w/w % PAA solution to give a C loading of 11.7 wt %. This suspension was stirred at 500 rpm using a Primix Homodisperser (Model 2.5), followed by static ultrasonication using a Hielscher sonic probe (Model UP400S) using 0.5 cycles and an amplitude of 60% for two 7 min sonication steps.
Following degassing of the solution, anode coatings were cast onto 10 μm thick Cu foil (Oak Mitsui, electrodeposited), using a laboratory scale RK Instruments K Coating Proofer machine with a micrometer-assisted doctor blade coated. Electrodes were dried on a hot plate at 80 °C, followed by vacuum drying (7 mBar) for 12 hours at 70 °C. The above formulation resulted in electrodes with a dry mass % composition of 70:14:16 (Silicon: Na-PAA: carbon additives).
A cathode formulation of 80:10:10 wt % (V-LFP: PVdF: CB) was generated by mixing the V-LiFePO4 with carbon black (Timcal C65, Purity 99.9%, specific surface area 65 m2 g−1) and NMP (Sigma Aldrich). It is important to note that 6.64 wt% of the V-LFP material was carbon from the sucrose carbonization process, occurring from heat treatment of the V-LFP. The cathode was processed using the following steps:
A solution of polyvinylidene difluoride (PVdF) grade 5130 (Solvay) was formulated by dissolving 80 g PVdF powder in 920 g NMP. This was performed using a T2F Turbula mixing apparatus (WAB, Germany) for 12 hours until the PVdF is completely dissolved to produce a binder concentration of 8 wt %.
144 g V-LFP and 16.6 g acetylene black were dry mixed in a HIVIS high torque mixer at 10 rpm for 10 min.
208.1 g of the 8 wt % PVdF 5130 solution was added and the slurry was mixed for 30 min at 15 rpm.
50 g of NMP was added to reduce the viscosity of the solution, with further mixing for 35 min at 15 rpm followed by 30 min at 100 rpm.
70 g NMP was added prior to the final stage of high torque mixing under static vacuum for 90 min at 100 rpm.
The contents were transferred to a FilmixTM Model 56–50 Disperser for 0.5 mins at a lineal speed of 8 m s−1. The resulting solid content of the electrode formulation was 35 wt %.
Cathode coating on Al foil was carried out on a Reel-to-reel Coater (MEGTEC) using a comma bar set an incrementally increasing blade gaps in the range 50–240 μm to produce areal coating densities in the range 24–95 g m−2. The coating speed was fixed at 0.75 m min−1 using temperatures in three successive drying zones of 100, 120 and 110 °C respectively.
The graphene-containing cathode was made in a smaller-scale formulation using an 80:10:5:5 wt % ratio (V-LFP: PVdF: CB: FLG), and was processed using the following steps:
20 g V-LFP, 1.25 g acetylene black and 1.25 g FLG were combined with 31.25 g of the 8 wt % PVdF 5130 solution and stirred with a Primix Homodisper Model 2.5 for 30 min, whilst continually adding 15.69 g of NMP to give a solid content of 36 wt %.
The mixture was transferred to a FilmixTM Thin-film Disperser Model 40–60 and dispersed at a lineal speed of 5 m/s for 0.5 min, 10 m s−1 for 0.5 min and 15 m s−1 for 15 sec.
Cathode coating on Al foil was carried out on using a draw-down coater (RK Instruments) to incrementally increasing blade gaps of 50–200 μm.
Coin cells for Si vs. Li/Li+ half-cells incorporated a Celgard separator (2325 grade) which is a porous polyolefin film. The electrolyte used was EC: EMC (3:7), with 15 wt % FEC and 3 wt % VC. The cycling voltage range for Si electrodes in a half cell configuration was 0.005 to 1.0 V. The first (formation) cycle used a relatively low current (±C/25), followed by higher currents on subsequent cycles (±C/5). For some tests, the lithiation step was limited by capacity rather than voltage. In these tests, the capacity limit on the first cycle was higher than on subsequent cycles. Differential plots of dQ/dV were calculated directly from the data.
All cell components were dried in a vacuum oven at 50 °C overnight prior to assembly. Three-electrode cells were fabricated using stainless steel Swagelok® hardware and perfluoroalkoxy (PFA) ferrules – as shown in Fig. 2. 60 μL of LP30 electrolyte was used (containing 1 M LiPF6), with EC: DMC 1:1, with 10% FEC and 5% VC. Connections to the three-electrode cell were made using connectors suited to a Biologic VMP3 potentiostat.
Electrochemical test cells used for evaluation of electrochemical performance of battery electrodes.
(a) 3-electrode Swagelok cell with a reference Li electrode. (b) Schematic of the components within a 2032-type coin cell.
The three-electrode cell was charged (silicon lithiation) at a constant C/20 rate followed by subsequent cycling at C/5. The charging was limited by a cathode voltage of 3.95 V vs. Li/Li+. Discharge (delithiation of silicon) was limited by an anode voltage of 1.50 V vs. Li/Li+. Coin cell characterisation was performed using a Maccor cycling unit, with all cells housed in Votsch VT-3050 environmental chambers maintained at 25 °C.
Upon examination of the microstructure of the Si-FLG electrodes it can be seen in Figure S2b that the dispersion of the carbon additives was reasonably uniform, which would be expected to provide effective connectivity between the active materials and the additives down to the current collector. Beyond reducing and controlling the particle size and degree of polydispersity, all of the major developments to enhance the high rate performance of LFP electrodes have historically been the result of electrode-scale improvements27. Both electrode materials appear to be uniformly dispersed, reducing the likelihood of charging and discharging inhomogeneities resulting from poor ionic (Li+ availability) and electronic connectivity throughout the electrode microstructure.
C rate vs. capacity for the V-LFP cathode vs. Li/Li+.
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