Lithium iron carbonate material prepared by vacuum carbon reduction and method
A lithium iron phosphate, vacuum technology, applied in chemical instruments and methods, phosphorus compounds, inorganic chemistry, etc., can solve the problems of low bulk density, poor electrical conductivity, increased production cost, etc., to simplify the synthesis process, shorten the reaction time, The effect of improving production efficiency
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Embodiment 1
[0029] In the first step, iron phosphate, lithium hydroxide and aluminum dihydrogen phosphate are mixed at a molar ratio of P:Fe:Li:Al of 1:1:1:0.05;
[0030] In the second step, the above mixture is placed in a vacuum high-energy ball milling tank and evacuated to 10 -2 Pa, ball milling for 12 hours;
[0031] In the third step, the carbon reducing agent activated carbon is added to the above-mentioned ball-milled mixture at the ratio of Fe:C molar ratio 1:0.8, and the vacuum is reduced to 10 -2 Pa, continue ball milling for 6 hours to obtain reaction precursors;
[0032] The fourth step is to transfer the precursors of the above-mentioned reactants to a vacuum reactor, bubbling in high-purity nitrogen for 5 minutes, and then evacuating to 10 -2 Pa, heating, controlling the temperature at 450°C, keeping the furnace temperature constant for 24 hours, bubbling in high-purity nitrogen for 45 minutes, sealing and cooling to room temperature to obtain carbon-coated metal aluminum doped lit...
Embodiment 2
[0035] The first step is to combine ferrous phosphate with lithium phosphate, doped metal compounds aluminum dihydrogen phosphate, zinc oxide, magnesium oxide, and cobalt oxide according to P: Fe: Li: M (M means doping metal, Al: Zn: Mg: Co The molar ratio is 1:1:1:0.5) and the molar ratio is 1:1:1:0.03;
[0036] In the second step, the above mixture is placed in a vacuum high-energy ball milling tank and evacuated to 10 -3 Pa, ball milling for 10 hours;
[0037] In the third step, the carbon reducing agent acetylene black and graphite (ratio 1:1) are added to the above-mentioned processed mixture at the ratio of Fe:C molar ratio 1:1, and the vacuum is reduced to 10 -3 Pa, continue ball milling for 8 hours to obtain reaction precursors;
[0038] The fourth step is to transfer the above-mentioned reactant precursors to a vacuum reactor, and pass high-purity nitrogen for 30 minutes, and then evacuate to 10 -3 Pa, heating, controlling the temperature at 650°C, keeping the furnace temper...
Embodiment 3
[0041] In the first step, ferrous phosphate is mixed with lithium phosphate and zinc oxide at a molar ratio of P:Fe:Li:Zn of 1:1:1:0.02;
[0042] In the second step, the above mixture is placed in a vacuum high-energy ball milling tank and evacuated to 10 -2 Pa, ball milling for 11 hours;
[0043] In the third step, the carbon reducing agent graphite is added to the above-mentioned ball-milled mixture at the ratio of Fe:C molar ratio 1:1.4, and the vacuum is reduced to 10 -2 Pa, continue ball milling for 9 hours to obtain reaction precursors;
[0044] The fourth step is to transfer the precursors of the above-mentioned reactants to a vacuum reactor, bubbling in high-purity nitrogen for 5 minutes, and then evacuating to 10 -2 Pa, heating, controlling the temperature at 550°C, keeping the furnace temperature constant for 20 hours, blowing in high-purity nitrogen for 45 minutes, sealing and cooling to room temperature, to obtain carbon-coated metal aluminum doped lithium iron phosphate p...
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