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Preparation method of high-density lithium iron phosphate positive material

A technology of lithium iron phosphate and positive electrode material, applied in electrode manufacturing, battery electrodes, electrical components and other directions, can solve the problems of high production cost, difficult to realize industrialization, etc., achieve the improvement of tap density, realize large-scale industrial production, method Simple and easy effects

Inactive Publication Date: 2011-04-20
YANTAI ZHUONENG BATTERY MATERIAL
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

[0005] The above methods all use the liquid phase method to prepare high-density spherical lithium iron phosphate, but the preparation of lithium iron phosphate materials by the liquid phase method only stays in the laboratory stage, and a large amount of solution needs to be processed in large-scale production, the production cost is high, and it is difficult to realize industrialization

Method used

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  • Preparation method of high-density lithium iron phosphate positive material
  • Preparation method of high-density lithium iron phosphate positive material
  • Preparation method of high-density lithium iron phosphate positive material

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0026] 1. Put 3.700kgLi 2 CO 3 , 16.530kgFe(CH 3 COO) 2 , 11.500kg NH 4 h 2 PO 4 , 0.405kgCr 2 o 3, 0.788kg of sucrose was ball-milled and mixed in a high-energy planetary ball mill for 1 hour, and then roasted in a pusher kiln at a temperature increase rate of 15°C / min from room temperature to 350°C under nitrogen protection, kept for 5 hours, and then lowered to room temperature to obtain a roasted materials;

[0027] 2. Pulverize the roasted material in step 1, with an average particle size of less than 3 microns, add sucrose accounting for 3% of the weight of the primary roasted material, ball mill and mix in a high-energy planetary ball mill for 3 hours again, and under nitrogen protection, in a pusher kiln with The heating rate of 2°C / min was raised from room temperature to 650°C for roasting, kept for 20 hours, and then lowered to room temperature to obtain secondary roasted materials;

[0028] 3. Pulverize the roasted material in step 2, with an average partic...

Embodiment 2

[0032] 1. Put 3.700kgLi 2 CO 3 , 17.625kgFe(C 2 o 4 ) 2 2H 2 O, 11.500kgNH 4 h 2 PO 4 , 0.1686kgMgCO 3 1.689 kg of glucose was mixed in a high-energy planetary ball mill for 2 hours, and then roasted in a pusher kiln at a temperature increase rate of 10 °C / min from room temperature to 300 °C under nitrogen protection, kept for 2 hours, and then lowered to room temperature to obtain a first-time roasting materials;

[0033] 2. Pulverize the roasted material in step 1, the average particle size is less than 3 microns, add glucose accounting for 5% of the weight of the primary roasted material, and mix it again in a high-energy planetary ball mill for 4 hours. The heating rate of °C / min is raised from room temperature to 680 °C for roasting, kept for 18 hours, and then lowered to room temperature to obtain a secondary roasted material;

[0034] 3. Pulverize the roasted material in step 2, the average particle size is less than 3 microns, and again account for 6% of the ...

Embodiment 3

[0037] 1. Combine 2.39kgLiOH, 16.186kgFe(C 2 o 4 ) 2 2H 2 O, 13.200kg (NH 4 ) 2 HPO 4 , 1.230kgZrO 2 1.57kg of glucose was ball milled and mixed in a stirring ball mill for 5 hours. Under the protection of argon, it was roasted in a steel belt kiln at a temperature increase rate of 20°C / min from room temperature to 500°C, kept for 10h, and then lowered to room temperature to obtain primary roasted material;

[0038] 2. Pulverize the roasted material in step 1, with an average particle size of less than 3 microns, add glucose accounting for 5% of the weight of the primary roasted material, and ball mill and mix for 5 hours in a stirring ball mill again. Under the protection of argon, in a steel belt kiln The heating rate of 8°C / min was raised from room temperature to 800°C for roasting, kept for 10 hours, and then lowered to room temperature to obtain the secondary roasted material;

[0039] 3. Pulverize the roasted material in step 2, the average particle size is less ...

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Abstract

The invention discloses a preparation method of a high-density lithium iron phosphate positive material. The preparation method is characterized by weighing a metallic element-doped compound containing lithium, ferrum and phosphorus, and an organic carbon source according to the mol ratio of Li: (Fe+M): P=1:1:1, wherein, the additive quantity of the organic carbon source is 1-10% of the total weight of the raw materials, mixing the materials by ball milling, and carrying out the first roasting at low-and-medium temperature under the protection of inert atmosphere; pulverizing the first roasting material, adding 2-8% of the organic carbon source for ball milling, and performing the second roasting at high temperature in inert atmosphere; and pulverizing the second roasting material, adding2-8% of the organic carbon source for ball milling, carrying out the third roasting at high temperature in inert atmosphere, and then carrying out pulverization grading to obtain the positive material. The lithium iron phosphate prepared by the method has high tap density, small specific surface area, normal distribution of granularity, good processing property, high actual discharge specific capacity, excellent product performances, and simple and easy method, thus easily realizing large-scale industrial production.

Description

Technical field: [0001] The invention relates to a method for preparing a high-density lithium iron phosphate cathode material, in particular to preparing a high-density lithium iron phosphate composite material by three-time roasting and three-time coating carbon technology, which belongs to the field of lithium-ion battery cathode materials. Background technique: [0002] Lithium-ion battery cathode material layered LiCoO 2 It has been widely used in small batteries, but its application in large-capacity batteries is limited due to the lack of cobalt resources, high price, pollution to the environment, and unsafe overcharging. Spinel LiMn 2 o 4 It has the advantages of non-toxic, cheap, and easy to recycle, but its actual specific capacity is low, and its high-temperature cycle performance is poor, which has not been completely solved by surface modification and coating. Although it is partially industrialized, its high-temperature cycle performance still needs to be sol...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): H01M4/04H01M4/58H01M4/62
CPCY02E60/12Y02E60/10
Inventor 杨志宽胡国荣黄文杰都立珍程元胜
Owner YANTAI ZHUONENG BATTERY MATERIAL
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