Method for preparing lithium iron phosphate cathode material by three-stage high-temperature solid phase calcination

A positive electrode material, lithium iron phosphate technology, applied in chemical instruments and methods, phosphorus compounds, battery electrodes, etc., can solve problems such as high price, cycle life, poor thermal stability and high temperature performance, and potential safety hazards, and achieve safety And the effect of good stability, superior electrochemical performance, easy control and operation

Inactive Publication Date: 2008-10-08
TIANJIN UNIV
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  • Summary
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  • Claims
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Problems solved by technology

At present, lithium cobalt oxide (LiCoO) is widely used as anode material in small lithium-ion batteries. 2 ), but due to the small reserves of cobalt in lithium cobaltate in nature, the price is relatively expensive and has certain toxicity, and in the process of charging, lithium cobaltate becomes CoO due to the deintercalation of metal lithium 2 ,Co 4+ Strong oxidizing property, easy to cause fire, explosion and other safety accidents
Therefore, for the development of high-power, large-capacity power batteries that require multiple single cells in series and parallel, there is a huge safety hazard in the use of lithium cobalt oxide
Lithium nickel oxide and lithium manganese oxide, which were once hoped for, have not made major breakthroughs so far. LiNiO 2 Although it has a high capacity, it has great difficulties in preparation, it is difficult to synthesize pure phase substances, and there are also certain safety problems.
LiMn 2 o 4 Although the price is cheap and the safety performance is good, its theoretical capacity is not high, and its cycle life, thermal stability and high temperature performance are poor
Therefore, these materials are still difficult to replace lithium cobalt oxide

Method used

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  • Method for preparing lithium iron phosphate cathode material by three-stage high-temperature solid phase calcination
  • Method for preparing lithium iron phosphate cathode material by three-stage high-temperature solid phase calcination
  • Method for preparing lithium iron phosphate cathode material by three-stage high-temperature solid phase calcination

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Embodiment 1

[0019] Will Li 2 CO 3 , FeC 2 o 4 2H 2 O and NH 4 h 2 PO 4 Weighing according to the stoichiometric ratio of 0.5:1:1, a total of 332 grams (of which Li 2 CO 3 : 37 g; FeC 2 o 4 2H 2 O: 180 g; NH 4 h 2 PO 4 : 115 grams), and add 13 grams of glucose relative to the raw material weight 4%, grind 5h in the wet method agitation type ball mill. Dry and granulate the suspension obtained above, transfer the obtained spherical particles to a rotary sintering furnace, raise the temperature to 300°C for pre-decomposition for 5 hours under a nitrogen protective atmosphere, then raise the temperature to 750°C, keep it warm for 12 hours, and then drop to room temperature with the furnace temperature , the obtained sample was added with 2% glucose relative to the weight of the raw material, and after ball milling for 12 hours, the temperature was raised to 750° C., kept for 6 hours and then lowered to room temperature with the furnace temperature, and the final lithium iron pho...

Embodiment 2

[0023] Will Li 2 CO 3 , FeC 2 o 4 2H 2 O and (NH 4 ) 2 HPO 4 Weighing according to the stoichiometric ratio of 0.5:1:1, a total of 332 grams (of which Li 2 CO 3 : 37 g; FeC 2 o 4 2H 2 O: 180 g; NH 4 h 2 PO 4 : 115 grams), and add 6.5 grams of glucose relative to raw material weight 2%, grind 5h in the wet-type stirring ball mill. Dry and granulate the suspension obtained above, transfer the obtained spherical particles to a rotary sintering furnace, raise the temperature to 300°C for pre-decomposition for 5 hours under a nitrogen protective atmosphere, then raise the temperature to 700°C, keep it warm for 12 hours, and then drop to room temperature with the furnace temperature 13 grams of glucose 4% relative to the weight of the raw material was added to the obtained sample, and after ball milling for 12 hours, the temperature was raised to 700°C, kept for 6 hours and then lowered to room temperature with the furnace temperature, and the final lithium iron phosph...

Embodiment 3

[0026] LiOH·H 2 O, FeC 2 o 4 2H 2 O and (NH 4 ) 2 HPO 4 Weighing according to the stoichiometric ratio of 1:1:1, a total of 337 grams (of which LiOH·H 2 O: 42 g; FeC 2 o 4 2H 2 O: 180 g; NH 4 h 2 PO 4 : 115 grams), ground 5h in a wet stirring ball mill. Dry the above-obtained suspension and granulate it. Transfer the obtained spherical particles to a rotary sintering furnace, raise the temperature to 300°C for pre-decomposition for 5 hours under a nitrogen protective atmosphere, then raise the temperature to 650°C, keep it warm for 12 hours, and then drop to room temperature with the furnace temperature , add 20 grams of glucose 6% relative to the weight of the raw material to the obtained sample, after ball milling for 12 hours, then raise the temperature to 650°C, keep warm for 6 hours and then drop to room temperature with the furnace temperature, and get the final lithium iron phosphate-carbon coating material after ball milling for 12 hours . The average par...

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Abstract

The invention discloses a method for preparing lithium iron phosphate anode material by three-step high temperature solid state sintering and pertains to the technique of chemical power source anode material. The process of the preparation method is that lithium salt, Fe<2+> compound, phosphate and carbon source are mixed according to certain ratio, ground and granulated; particles obtained are transferred in a rotary sintering furnace and carried out predecomposition for 3-10 hours when the temperature is increased to 300-500 DEG C under the protection of nitrogen; the temperature raises to 650-850 DEG C and the heat is preserved for 6-15 hours and then the temperature is dropped to room temperature with furnace temperature; the material obtained is added with carbon source in different amount and is carried out ball milling, the temperature raises to 650-850 DEG C and the heat is preserved for 6-15 hours and then the temperature is dropped to room temperature with furnace temperature, and the lithium iron phosphate anode material is obtained after ball milling. The method of the invention is characterized by simple process, being easy to realize industrial scale production, wide sources of raw materials, low cost, complete crystal form of anode material, regular product pattern, excellent electrochemical performance and high tap density which reaches 1.36g cm<-3>.

Description

technical field [0001] The invention relates to a method for preparing a lithium iron phosphate cathode material by three-step high-temperature solid-phase calcination, and belongs to the technical field of cathode materials for chemical power sources. Background technique [0002] Energy is closely related to the survival and development of human society. With the growth of the global population and the rapid development of the economy, a large amount of energy is consumed and serious environmental pollution is caused. In order to achieve sustainable development, the natural environment and natural resources on which human beings depend must be protected. This is a serious challenge that human beings face in the 21st century. [0003] A chemical power source is a device that converts chemical energy into electrical energy. Since R.G.Plante invented lead-acid batteries in 1859 and G.Leclance made zinc-manganese dry batteries in 1868, chemical power sources have experienced...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C01B25/45H01M4/58
CPCY02E60/10
Inventor 唐致远高飞
Owner TIANJIN UNIV
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