CN101850957A - Method for preparing nano-lithium iron phosphate of cathode material of lithium ion battery - Google Patents
Method for preparing nano-lithium iron phosphate of cathode material of lithium ion battery Download PDFInfo
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- CN101850957A CN101850957A CN201010179297A CN201010179297A CN101850957A CN 101850957 A CN101850957 A CN 101850957A CN 201010179297 A CN201010179297 A CN 201010179297A CN 201010179297 A CN201010179297 A CN 201010179297A CN 101850957 A CN101850957 A CN 101850957A
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- Prior art keywords
- lithium
- iron phosphate
- ion battery
- cathode material
- lithium iron
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- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
- Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
- Y02E—REDUCTION OF GREENHOUSE GAS [GHG] EMISSIONS, RELATED TO ENERGY GENERATION, TRANSMISSION OR DISTRIBUTION
- Y02E60/00—Enabling technologies; Technologies with a potential or indirect contribution to GHG emissions mitigation
- Y02E60/10—Energy storage using batteries
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Abstract
The invention discloses a method for preparing nano-lithium iron phosphate of a cathode material of a lithium ion battery. The method comprises the following steps of: performing ball-milling on ferrous oxalate, ammonium dihydrogen phosphate, lithium acetate and lauric acid in a high-energy ball mill; tabletting a mixture; and performing solid phase sintering on a tabletted mixture to obtain the cathode material of the lithium ion battery of the nano-lithium iron phosphate with good disperstiveness. In the method, the lauric acid of an organic carbon source is added and a proper solid phase sintering method is utilized, so that the surface conductivity of synthesized lithium iron phosphate nanoparticles is improved; the charge-discharge capacity and the cycle performance of the lithium iron phosphate nanoparticles are improved; and the electrochemical performance of the lithium iron phosphate nanoparticles serving as the cathode material of the lithium ion battery is improved effectively. The method has the characteristics of simple overall reaction process, no toxic substance or environment pollutant and environmental friendliness, belongs to a green chemical preparation method, and can realize large-scale production.
Description
Technical field
The invention belongs to material preparation method, particularly a kind of method for preparing nano-lithium iron phosphate of cathode material of lithium ion battery.
Background technology
The LiFePO 4 LiFePO of olivine structural
4Have theoretical specific capacity height, abundant raw material, have extended cycle life, advantages such as high temperature safety is good, environmental protection, be considered to the most rising anode material for lithium-ion batteries.But, LiFePO
4Low electronic conductivity causes its specific storage to reduce, and the lithium ion spread coefficient is low to make that its cycle performance is bad; These shortcomings have restricted LiFePO
4Industrialized development.Present solution route mainly contains: the one, and by reducing the material granule size to shorten lithium ion at LiFePO
4Migration distance in the charge and discharge process; The 2nd, other element that mixes improves LiFePO
4The electric conductivity of material surface.
About preparation LiFePO
4Method have: high temperature solid-state method, carbothermic method, microwave heating method, hydrothermal method, coprecipitation method, sol-gel method, microemulsion method, template etc., in above-mentioned some method to the requirement height of equipment, the operating process more complicated, process control is strict, preparation process can cause in various degree pollution to environment, and the cost height, efficient is low, is difficult to accomplish produce in enormous quantities.
Summary of the invention
The invention provides a kind of simple method for preparing nano-lithium iron phosphate of cathode material of lithium ion battery.Entire reaction course of the present invention is simple, no toxic substance or environmental pollution deposits yields, and environmental friendliness belongs to the preparation method of Green Chemistry, and present method can realize scale operation, and required chemical reagent cheapness is easily purchased.
Technical scheme of the present invention is achieved in that and may further comprise the steps:
(1) weighing mole proportioning is the Ferrox (FeC of 1:1:1:1
2O
42H
2O), primary ammonium phosphate (NH
4H
2PO
4), Lithium Acetate (CH
3COOLi2H
2O) and lauric acid (C
12H
24O
2), in high energy ball mill ball milling 4-8 hour, compressing tablet after the cryodrying;
(2) product behind the dry compressing tablet is placed porcelain boat, put into resistance wire horizontal pipe stove, under argon gas (or nitrogen) protective atmosphere, adopt following calcination process: with 3-5 ℃ of min
-1Temperature rise rate be heated to 500-700 ℃, be incubated 5-12 hour, cool to room temperature then with the furnace, can obtain nanometer ferrous phosphate lithium LiFePO
4
The present invention adopts solid sintering technology synthesis nano LiFePO
4With raw material FeC
2O
42H
2O, NH
4H
2PO
4, CH
3COOLi2H
2O and C
12H
24O
2Mix, increase the process of high-energy ball milling; Adopt solid sintering technology, control its temperature and constant temperature time, prepare the nano level LiFePO of good dispersity
4Material.This invention provides a kind of organic additive that can improve its surface conductivity and specific discharge capacity, and a kind of method for preparing solid phase that is used to prepare the anode material for lithium-ion batteries of nanometer ferrous phosphate lithium particularly is provided.
Embodiment
Embodiment one:
The weighing mol ratio is the FeC of 1:1:1:1
2O
42H
2O, NH
4H
2PO
4, CH
3COOLi2H
2O and C
12H
24O
2, ball milling is 4 hours in high energy ball mill, compressing tablet after the cryodrying; Product behind the dry compressing tablet is placed porcelain boat, put into resistance wire horizontal pipe stove, under argon gas (or nitrogen) protective atmosphere, adopt following calcination process: with 3 ℃ of min
-1Temperature rise rate be heated to 600 ℃, be incubated 12 hours, cool to room temperature then with the furnace, can obtain particle diameter mainly at the nano level LiFePO of 80nm-200nm
4Material.
Embodiment two:
The weighing mol ratio is the FeC of 1:1:1:1
2O
42H
2O, NH
4H
2PO
4, CH
3COOLi2H
2O and C
12H
24O
2, ball milling is 4 hours in high energy ball mill, compressing tablet after the cryodrying; Product behind the dry compressing tablet is placed porcelain boat, put into resistance wire horizontal pipe stove, under argon gas (or nitrogen) protective atmosphere, adopt following calcination process: with 3 ℃ of min
-1Temperature rise rate be heated to 550 ℃, be incubated 12 hours, cool to room temperature then with the furnace, can obtain particle diameter mainly at the nano level LiFePO of 100nm-400nm
4Material.
Embodiment three:
The weighing mol ratio is the FeC of 1:1:1:1
2O
42H
2O, NH
4H
2PO
4, CH
3COOLi2H
2O and C
12H
24O
2, ball milling is 4 hours in high energy ball mill, compressing tablet after the cryodrying; Product behind the dry compressing tablet is placed porcelain boat, put into resistance wire horizontal pipe stove, under argon gas (or nitrogen) protective atmosphere, adopt following calcination process: with 3 ℃ of min
-1Temperature rise rate be heated to 600 ℃, be incubated 5 hours, cool to room temperature then with the furnace, can obtain particle diameter mainly at the nano level LiFePO of 300nm-800nm
4Material.
Embodiment four:
The weighing mol ratio is the FeC of 1:1:1:1
2O
42H
2O, NH
4H
2PO
4, CH
3COOLi2H
2O and C
12H
24O
2, ball milling is 4 hours in high energy ball mill, compressing tablet after the cryodrying; Product behind the dry compressing tablet is placed porcelain boat, put into resistance wire horizontal pipe stove, under argon gas (or nitrogen) protective atmosphere, adopt following calcination process: with 3 ℃ of min
-1Temperature rise rate be heated to 700 ℃, be incubated 12 hours, cool to room temperature then with the furnace, can obtain particle diameter mainly at the nano level LiFePO of 100nm-200nm
4Material.
Claims (3)
1. a method for preparing nano-lithium iron phosphate of cathode material of lithium ion battery is characterized in that, may further comprise the steps:
(1) weighing mole proportioning is the Ferrox (FeC of 1:1:1:1
2O
42H
2O), primary ammonium phosphate (NH
4H
2PO
4), Lithium Acetate (CH
3COOLi2H
2O) and the organic carbon additive, mixed 4-8 hour dry back compressing tablet;
(2) product behind the dry compressing tablet is placed porcelain boat, put into resistance wire horizontal pipe stove, under argon gas or nitrogen protection atmosphere, with 3-5 ℃ of min
-1Temperature rise rate be heated to 500-700 ℃, be incubated 5-12 hour, cool to room temperature then with the furnace, can obtain nanometer ferrous phosphate lithium LiFePO
4
2. the method for preparing nano-lithium iron phosphate of cathode material of lithium ion battery according to claim 1 is characterized in that, the organic carbon additive is lauric acid (C
12H
24O
2).
3. the method for preparing nano-lithium iron phosphate of cathode material of lithium ion battery according to claim 1 and 2 is characterized in that, described hybrid mode needs ball milling in high energy ball mill.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201010179297A CN101850957A (en) | 2010-05-21 | 2010-05-21 | Method for preparing nano-lithium iron phosphate of cathode material of lithium ion battery |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201010179297A CN101850957A (en) | 2010-05-21 | 2010-05-21 | Method for preparing nano-lithium iron phosphate of cathode material of lithium ion battery |
Publications (1)
| Publication Number | Publication Date |
|---|---|
| CN101850957A true CN101850957A (en) | 2010-10-06 |
Family
ID=42802674
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|---|---|---|---|
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Cited By (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102097617A (en) * | 2011-01-12 | 2011-06-15 | 福建师范大学 | Method for depositing silicon thin film on surface of lithium iron phosphate anode in lithium ion battery |
| CN102185126A (en) * | 2011-03-23 | 2011-09-14 | 中信国安盟固利动力科技有限公司 | Method for dispersing micro-scale and nano-scale electrode materials |
| CN102664257A (en) * | 2012-04-05 | 2012-09-12 | 扬州奇峰纳米材料有限公司 | Low-temperature solid-phase synthesis method of nanoscale LiFePO4 |
| CN102826533A (en) * | 2011-06-17 | 2012-12-19 | 周丽新 | Ferrous phosphate predecessor of lithium ion battery, lithium iron phosphate powder prepared from predecessor, and preparation methods of predecessor and powder |
| CN102992294A (en) * | 2011-09-09 | 2013-03-27 | 江西省金锂科技有限公司 | Method for preparing high-activity lithium iron phosphate cathode material with FeOOH |
| CN114188508A (en) * | 2021-10-28 | 2022-03-15 | 厦门理工学院 | Lithium iron phosphate cathode material, preparation method and application |
Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1812166A (en) * | 2005-01-28 | 2006-08-02 | 比亚迪股份有限公司 | Preperative method for ferrous phosphate radical lithium salt of lithium ion secondary cell active material |
| CN101533912A (en) * | 2008-03-11 | 2009-09-16 | 比亚迪股份有限公司 | Method for preparing lithium iron phosphate used as positive active material of lithium ion secondary battery |
-
2010
- 2010-05-21 CN CN201010179297A patent/CN101850957A/en active Pending
Patent Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1812166A (en) * | 2005-01-28 | 2006-08-02 | 比亚迪股份有限公司 | Preperative method for ferrous phosphate radical lithium salt of lithium ion secondary cell active material |
| CN101533912A (en) * | 2008-03-11 | 2009-09-16 | 比亚迪股份有限公司 | Method for preparing lithium iron phosphate used as positive active material of lithium ion secondary battery |
Non-Patent Citations (2)
| Title |
|---|
| 《Journal of Power Sources》 20061117 Daiwon Choi et al. Surfactant based sol-gel approach to nanostructured LiFePO4 for high rate Li-ion batteries 1064-1069 第163卷, 2 * |
| 《材料导报：研究篇》 20090731 梁风等 表面活性剂对溶胶-凝胶法合成L iFePO4 电化学性能的影响 96-98 第23卷, 第7期 2 * |
Cited By (8)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102097617A (en) * | 2011-01-12 | 2011-06-15 | 福建师范大学 | Method for depositing silicon thin film on surface of lithium iron phosphate anode in lithium ion battery |
| CN102185126A (en) * | 2011-03-23 | 2011-09-14 | 中信国安盟固利动力科技有限公司 | Method for dispersing micro-scale and nano-scale electrode materials |
| CN102826533A (en) * | 2011-06-17 | 2012-12-19 | 周丽新 | Ferrous phosphate predecessor of lithium ion battery, lithium iron phosphate powder prepared from predecessor, and preparation methods of predecessor and powder |
| CN102826533B (en) * | 2011-06-17 | 2014-09-10 | 周丽新 | Ferrous phosphate predecessor of lithium ion battery, lithium iron phosphate powder prepared from predecessor, and preparation methods of predecessor and powder |
| CN102992294A (en) * | 2011-09-09 | 2013-03-27 | 江西省金锂科技有限公司 | Method for preparing high-activity lithium iron phosphate cathode material with FeOOH |
| CN102664257A (en) * | 2012-04-05 | 2012-09-12 | 扬州奇峰纳米材料有限公司 | Low-temperature solid-phase synthesis method of nanoscale LiFePO4 |
| CN114188508A (en) * | 2021-10-28 | 2022-03-15 | 厦门理工学院 | Lithium iron phosphate cathode material, preparation method and application |
| CN114188508B (en) * | 2021-10-28 | 2023-02-14 | 厦门理工学院 | Lithium iron phosphate cathode material, preparation method and application |
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Application publication date: 20101006 |