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Lithium iron fluorophosphate composite material as well as preparation method and application thereof

A technology of lithium iron phosphate fluorophosphate and lithium iron phosphate, which is applied in the field of lithium iron phosphate fluorophosphate composite materials and its preparation, can solve problems such as uneven doping of fluorine elements, achieve simple process schemes, suppress irreversible phase transitions, The effect of the rate and cycle performance improvement

Pending Publication Date: 2022-01-28
陕西创普斯新能源科技有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

[0018] The purpose of the present invention is to overcome defects such as uneven doping of fluorine elements in the prior art, and provide a lithium iron phosphate fluorophosphate composite material and its preparation method

Method used

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  • Lithium iron fluorophosphate composite material as well as preparation method and application thereof
  • Lithium iron fluorophosphate composite material as well as preparation method and application thereof

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0056] In this example, the positive electrode material of lithium iron phosphate fluorophosphate was prepared according to the following steps:

[0057] The specific molecular formula of the cathode material described in this embodiment is Li 1.06 Fe 0.97 PO 3.97 f 0.06 @C.

[0058]According to the molar ratio of lithium element: iron element: phosphate ion: fluorine element = 1.06:0.97:3.97:0.06, 8.83kg of iron phosphate, 2.18kg of lithium carbonate, and 0.13kg of LiF were weighed respectively, and 1.35kg of glucose was used for carbon coating. Use 0.27 kg of citric acid as a research aid, prepare a slurry solution with a solid content of 35%, and carry out water-based grinding in a 1L sand mill. Second fine grinding to 300nm. The particle size D50 of the spray-dried powder was 8 microns, and the water content was 1.5%. Then carry out graphite saggar filling treatment, and finally carry out high-temperature sintering at 700°C for 8 hours in a box-type atmosphere furnac...

Embodiment 2

[0062] In this example, the positive electrode material of lithium iron phosphate fluorophosphate was prepared according to the following steps:

[0063] The specific molecular formula of the cathode material described in this embodiment is LiFeP O3.9 f 0.2 @C.

[0064] Weigh respectively 59.1kg of iron phosphate, 35.7kg of ferrous oxalate, 23.0kg of lithium phosphate, FeF 2 0.26kg, 3.8kg of glucose was used for carbon coating, polyethylene glycol 1.59kg was selected as the research aid, a slurry solution with a solid content of 30% was prepared, and water system grinding was carried out in a 10L sand mill, wherein the water system grinding included coarse Grinding and secondary fine grinding, coarse grinding to 0.7μm, secondary fine grinding to 200nm. The particle size D50 of the spray-dried powder was 10 microns, and the water content was 1.5%. Then carry out graphite saggar filling treatment, and finally carry out high-temperature sintering at 750°C for 10 hours in a bo...

Embodiment 3

[0068] In this example, the positive electrode material of lithium iron phosphate fluorophosphate was prepared according to the following steps:

[0069] The specific molecular formula of the positive electrode material described in this embodiment is Li 1.4 Fe 0.8 PO 3.6 f 0.8 @C.

[0070] According to the molar ratio of lithium element: iron element: phosphate ion: fluorine element = 1.4:0.8:3.6:0.8, respectively weigh 1000kg of ferric phosphate, 95.5kg of ferrous oxalate, 22.0kg of lithium hydroxide, 76.8kg of phosphoric acid, and 208.4kg of lithium carbonate. kg, HF5kg, 139.8kg of glucose was used for carbon coating, 14.7kg of oxalic acid was selected as the research aid, a slurry solution with a solid content of 40% was prepared, and water-based grinding was carried out in a 10L sand mill. The water-based grinding included rough grinding and Secondary fine grinding, coarse grinding to 0.9μm, secondary fine grinding to 100nm. The particle size D50 of the spray-dried p...

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Abstract

The invention belongs to the technical field of preparation of electrode materials, and particularly discloses a lithium iron fluorophosphate composite material and a preparation method thereof. The lithium ion battery positive electrode material comprises in-situ doped lithium iron fluorophosphate, the general formula of the lithium iron fluorophosphate positive electrode material is Li1 + 2xFe1-xPO4-y / 2Fy, x is more than or equal to 0 and less than or equal to 0.2, and y is more than 0 and less than or equal to 1. According to the invention, through raw material optimization and new reaction process design, the fluorine element forms bond valence binding with main elements such as lithium, iron and phosphorus in advance, so that the distribution uniformity of the doped fluorine element in the material crystal is ensured indeed. The prepared composite material shows excellent plateau voltage stability and rate capability.

Description

technical field [0001] The invention belongs to the technical field of electrode material preparation, and in particular relates to a lithium iron phosphate fluorophosphate composite material and a preparation method and application thereof. Background technique [0002] Lithium iron phosphate has the advantages of high capacity, low manufacturing cost, and environmental protection, and is widely used as a cathode material for ion batteries. It is recognized in the industry as the preferred cathode material for power and energy storage batteries. [0003] There are two conventional methods for synthesizing fluorine-doped lithium iron phosphate: 1) Ammonium dihydrogen phosphate + ferrous oxalate + lithium carbonate process is used to prepare the finished product through sintering, and then ammonium fluoride is added to form a fluorine surface gradient Miscellaneous; 2) The lithium carbonate + iron phosphate process is used to prepare the finished product through sintering, a...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): H01M4/36H01M4/58H01M10/0525
CPCH01M4/366H01M4/5825H01M4/582H01M10/0525H01M2004/028Y02E60/10
Inventor 王昊彭工厂谢正伟梁小惠
Owner 陕西创普斯新能源科技有限公司
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