Silane doped lithium titanium phosphate two-component surface modified ferric fluoride anode material and preparation method
A technology of lithium titanium phosphate and surface modification, which is applied in the direction of battery electrodes, electrochemical generators, electrical components, etc., can solve the problems of high reaction activation energy, high conversion reaction, poor economy, etc., to overcome the ion conductivity Extremely low, the effect of improving electrochemical performance
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Embodiment 1
[0019] Embodiment 1: Al 2 o 3 : SiO 2 :TiO 2 : NH 4 h 2 PO 4 : Li 2 CO 3 Mix evenly in a ratio of 0.05: 0.1: 1.9: 2.9: 0.6 (molar ratio), add 3% of 95% ethanol, and ball mill in a ball mill at a speed of 100 rpm for 10 hours. After the ball milling, the pressure is 10Pa at 60°C Dry in a vacuum oven for 2 hours, take it out and re-grind it in an agate mortar for 10 minutes. The ground powder is heated to 600°C at a rate of 5°C / min and kept for 5 hours to make Li 1.2 Al 0.1 Ti 1.9 Si 0.1 P 2.9 o 12 Solid electrolyte powder. Fe(NO 3 ) 3 9H 2 O and ammonium fluoride (1.0:3.0 molar ratio) with 3 wt% Li 1.2 Al 0.1 Ti 1.9 Si 0.1 P 2.9 o 12 The solid electrolyte powder, 0.5% by weight of Tween-80 and 0.5% by weight of anilinomethyltriethoxysilane were ball-milled at room temperature for 5 hours under the protection of high-purity nitrogen in a high-energy ball mill, and then the materials were taken out. Under the protection of the mixed gas of % hydrogen and 95...
Embodiment 2
[0020] Embodiment 2: Al 2 o 3 : SiO 2 :TiO 2 : NH 4 h 2 PO 4 : Li 2 CO 3 Mix evenly in a ratio of 0.05: 0.1: 1.9: 2.9: 0.6 (molar ratio), add 8% 95% ethanol, and ball mill for 45 hours at a speed of 450 rpm in a ball mill. After the ball mill finishes, the pressure is 90Pa at 75°C Dry in a vacuum oven for 8 hours, take it out and re-grind it in an agate mortar for 25 minutes. The ground powder is heated to 900°C at a rate of 25°C / min and kept for 15 hours to make Li 1.2 Al 0.1 Ti 1.9 Si 0.1 P 2.9 o 12 Solid electrolyte powder. FeCl 3 ·6H 2 O and ammonium fluoride (1.0:3.6 in molar ratio) with 13% by weight Li 1.2 Al 0.1 Ti 1.9 Si 0.1 P 2.9 o 12 Solid electrolyte powder, 2.8% by weight of span-60 and 3.0% by weight of N-β(aminoethyl)-γ-aminopropyltrimethoxysilane were ball milled in a high-energy ball mill under the protection of high-purity nitrogen at room temperature for 20 After 1 hour, the material was taken out, heated to 450 degrees under the protec...
Embodiment 3
[0021] Embodiment 3: Al 2 o 3 : SiO 2 :TiO 2 : NH 4 h 2 PO 4 : Li 2 CO 3 Mix evenly in a ratio of 0.05: 0.1: 1.9: 2.9: 0.6 (molar ratio), add 5% 95% ethanol, and ball mill in a ball mill at a speed of 200 rpm for 25 hours. After the ball milling, the pressure is 60Pa at 70°C Dry in a vacuum oven for 7 hours, take it out, and re-grind it in an agate mortar for 20 minutes. The ground powder is heated to 700°C at a rate of 20°C / min and kept for 12 hours to make Li 1.2 Al 0.1 Ti 1.9 Si 0.1 P 2.9 o 12 Solid electrolyte powder. Will Fe 2 (SO 4 ) 3 9H 2 O and ammonium fluoride (1.0:3.5 molar ratio) with 7 wt% Li 1.2 Al 0.1 Ti 1.9 Si 0.1 P 2.9 o 12 The solid electrolyte powder, the tx-10 with a weight percentage of 2.0% and the hexamethylenediaminomethyltriethoxysilane with a weight percentage of 2.1% were ball milled at room temperature for 15 hours under the protection of high-purity nitrogen in a high-energy ball mill, and then the materials were taken out an...
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