Method for preparing lithium iron phosphate in batch-type high-vacuum dynamic sintering mode
A lithium iron phosphate, high vacuum technology, applied in chemical instruments and methods, phosphorus compounds, structural parts, etc., can solve the problems of increasing uncontrollable factors, slow cooling speed, uneven heating, etc., to shorten the sintering time and reduce sintering. temperature, the effect of preventing oxidation
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[0037] Embodiment 1: In this embodiment, according to the stoichiometric ratio Fe:Li:P=1:1:1, iron phosphate, lithium carbonate and organic carbon source (in this embodiment, the weight percent of organic carbon source accounts for all precursors) 1%~5% of the body) as the raw material to prepare the precursor, the lithium iron phosphate precursor is sent into the rotary furnace body, and the furnace head and the rotating place are sealed with a gasket and high temperature vacuum grease to ensure the furnace head, rotation Then adjust the level of the furnace body, turn on the multi-stage vacuum pump to extract the air remaining in the furnace body, then fill in the inert gas, turn on the power of the rotary furnace after repeated many times, and adjust the rotation speed of the furnace body to 0.5 rev / min, material at 10 2 ~10 -2 The temperature is raised to 700 °C under high vacuum and calcined dynamically for 8 hours, the vacuum pump is turned off, and the inert gas is fil...
Example Embodiment
[0039] Example 2: In this example, ferrous oxalate, lithium carbonate, and ammonium dihydrogen phosphate with a stoichiometric ratio of Fe:Li:P=1:1:1 are used as raw materials. The 1%~5% organic carbon source of all the precursors is obtained by sanding and drying to obtain the lithium iron phosphate precursor, and then the precursor is sent into the rotary furnace body, and the furnace head and rotating Seal the furnace to ensure the air tightness of the furnace head, the rotating part and the outlet of the gas outlet, then adjust the furnace body level, turn on the secondary vacuum pump to extract the residual air in the furnace body, then fill it with nitrogen, and open it back after repeated many times. Converter power supply, adjust the rotation speed of the furnace body to 5 rpm, and the material is 10 2 ~10 -2 The temperature is raised to 600 °C under high vacuum and calcined dynamically for 15 hours, the vacuum pump is turned off, and then the inert gas is charged to ...
Example Embodiment
[0041] Example 3: In this example, iron oxide, lithium carbonate and phosphoric acid with a stoichiometric ratio of Fe:Li:P=1:1:1 are used as raw materials. 1%~5% organic carbon source is obtained by ball milling and spray drying to obtain lithium iron phosphate precursor, and then the precursor is sent into the rotary furnace body, and the furnace head and the rotating part are sealed with sealing gasket and high temperature vacuum grease , to ensure the air tightness of the furnace head, the rotating place and the outlet of the gas outlet, then adjust the furnace body level, turn on the four-stage vacuum pump to extract the residual air in the furnace body, and then fill it with argon gas, and turn on the power of the rotary furnace after repeated many times. Adjust the rotation speed of the furnace body to 1 rev / min, and the material to be at 10 2 ~10 -2 The temperature is raised to 800 °C under high vacuum and calcined dynamically for 8 hours. The vacuum pump is turned of...
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