CN102074689A - Method for preparing lithium iron phosphate composite material - Google Patents
Method for preparing lithium iron phosphate composite material Download PDFInfo
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- CN102074689A CN102074689A CN201010602891XA CN201010602891A CN102074689A CN 102074689 A CN102074689 A CN 102074689A CN 201010602891X A CN201010602891X A CN 201010602891XA CN 201010602891 A CN201010602891 A CN 201010602891A CN 102074689 A CN102074689 A CN 102074689A
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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
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- 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
Abstract
The invention discloses a method for preparing a lithium iron phosphate composite material. The method comprises the following steps of: 1) preparing a titanium-doped precursor, namely adding a lithium source, an iron source, a titanium source and a phosphorus source according to the molar ratio of (1-1.05):(0.97-0.995):(0.005-0.03):1 into a ball mill together with a carbon source, ball-milling for 6 to 12 hours, performing spray drying and sieving; 2) preparing titanium-doped lithium iron phosphate, namely calcining dried materials under the protection of inert gas at the temperature of between 350 and 500 DEG C for 3 to 5 hours, crushing, and calcining at the temperature of between 600 and 800 DEG C for 8 to 16 hours; and 3) coating titanium dioxide, namely mixing the titanium-doped lithium iron phosphate prepared in the step 2) and the titanium source, drying, and calcining in the inert gas at the temperature of between 400 and 800 DEG C for 4 to 8 hours. The lithium iron phosphate composite material prepared by the method has higher compactness, high electrochemical performance and high machining performance; and the method has a relatively stable process and is easy to industrialize.
Description
Technical field
The present invention relates to a kind of anode material for lithium-ion batteries, particularly relate to a kind of preparation method of composite ferric lithium phosphate material.
Background technology
LiFePO4 (LiFePO
4), environmental friendliness cheap because of its cost of material, specific capacity height, characteristics such as cycle performance and security performance excellence particularly, make it great market prospects be arranged, be considered to the anode material for lithium-ion batteries of new generation of tool development and application potentiality in the required large-sized power field of power supplies of various removable field of power supplies, particularly electric motor cars.But LiFePO
4Have the shortcoming of the low and ions diffusion rate variance of conductivity, cause high-rate charge-discharge capability difference and actual specific capacity low, this has greatly limited its extensive use in practical field.
People's research attentiveness mainly concentrates on this field of LiFePO4 conductivity that solves at present.Improve LiFePO
4The main method of conductivity is that carbon coats and metal ion mixing.And existing carbon method for coating can significantly reduce the tap density of material, causes its volume energy density lower, is difficult to practical application; Though existing metal ion mixing method has increased substantially the conductivity of material, also have certain gap apart from expectation target, remain further to be improved.
Summary of the invention
The purpose of this invention is to provide a kind of good conductivity, volume energy density height, chemical property and the processing characteristics preparation method of composite ferric lithium phosphate material preferably.
The objective of the invention is to be achieved through the following technical solutions:
A kind of preparation method of composite ferric lithium phosphate material is characterized in that may further comprise the steps:
1) the titanium precursor body is mixed in preparation: with lithium source, source of iron, titanium source and phosphorus source according to mol ratio 1～1.05: with carbon source join in ball mill at 0.97～0.995: 0.005～0.03: 1, the consumption of carbon source makes its mass percent in finished product less than 2%, add quantitative deionized water and zirconium ball and do abrasive media, ball milling 6～12 hours, after making the raw material porphyrize and mixing, carry out spray drying, sieve;
2) the titanium LiFePO4 is mixed in preparation: dried material under inert gas shielding, 350～500 ℃ of calcinings 3～5 hours, is pulverized the back 600 ℃～800 ℃ calcinings 8～16 hours;
3) cladding titanium dioxide: with step 2) preparation mix titanium LiFePO4 and titanium source behind combination drying, under inert gas, calcined 4～8 hours in 400 ℃～800 ℃.
Described source of iron is ferrous oxalate, iron oxide or ferric phosphate;
Described lithium source is lithium carbonate, lithium hydroxide or lithium dihydrogen phosphate;
Described phosphorus source is ammonium dihydrogen phosphate, ferric phosphate or lithium dihydrogen phosphate;
Described carbon source is glucose sugar, sucrose, polyethylene glycol, citric acid or superconduction carbon black;
The described titanium of step 1) source is titanium dioxide, lithium titanate, titanium sulfate or butyl titanate;
The described titanium of step 3) source is titanium dioxide or butyl titanate;
It is 1: 1～2 (quality) that the quantitative deionized water of adding described in the step 1) satisfies solid-to-liquid ratio;
It is 2～4: 1 (quality) that the quantitative zirconium ball of adding described in the step 1) satisfies ratio of grinding media to material;
It is 1: 1～2 (quality) that the quantitative deionized water of adding described in the step 1) satisfies solid-to-liquid ratio;
It is 2～4: 1 (quality) that the quantitative zirconium ball of adding described in the step 1) satisfies ratio of grinding media to material;
Drying described in the step 1) is a spray drying;
The solid phase ball milling that is mixed into described in the step 3) mixes, and ratio of grinding media to material is 1～2: 1, and the ball milling time is 0.5～2 hour;
The described mixing of step 3) can also be that the wet method super-fine ball milling mixes, and solid content is 50%, and the ball milling time is 1～2 hour;
Its covering amount of the described cladding titanium dioxide of step 3) is 0.8%～2%.
The invention has the advantages that: in building-up process, except passing through Doped with Titanium ion (Ti
4+), replace a spot of iron position in the LiFePO4, outside the conductivity that improves LiFePO 4 material, also adopting outside carbon coated once more, cladding titanium dioxide improves LiFePO
4The conductivity of material further improves its high rate charge-discharge performance.Owing to reduced the consumption (below 2%) of carbon coated,, increased the volumetric specific energy of material so improved the tap density of material effectively.Doped with Titanium ion (the Ti that adopts preparation method of the present invention to produce
4+) LiFePO of cladding titanium dioxide simultaneously
4Composite material has higher tap density and good electrochemical and processing characteristics.In addition, the preparation method of the low-carbon (LC) composite ferric lithium phosphate material of titanium doped and cladding titanium dioxide of the present invention, process stabilizing, step are simple relatively, easily realize industrialization.
Description of drawings
Fig. 1 is a composite ferric lithium phosphate material preparation method's of the present invention flow chart;
Fig. 2 mixes the XRD figure of the low-carbon (LC) composite ferric lithium phosphate material of titanium and cladding titanium dioxide for prepared according to the methods of the invention;
Fig. 3 mixes the SEM figure of the low-carbon (LC) composite ferric lithium phosphate material of titanium and cladding titanium dioxide for prepared according to the methods of the invention.
Embodiment
Referring to Fig. 1, the preparation method of composite ferric lithium phosphate material of the present invention may further comprise the steps:
1) the titanium precursor body is mixed in preparation: with lithium source, source of iron, titanium source and phosphorus source according to mol ratio 1～1.05: with carbon source join in ball mill at 0.97～0.995: 0.005～0.03: 1, the consumption of carbon source makes its mass percent in finished product less than 2%, add quantitative deionized water and zirconium ball and do abrasive media, ball milling 6～12 hours, after making the raw material porphyrize and mixing, carry out spray drying, sieve;
2) the titanium LiFePO4 is mixed in preparation: dried material under inert gas shielding, 350～500 ℃ of calcinings 3～5 hours, is pulverized the back 600 ℃～800 ℃ calcinings 8～16 hours;
3) cladding titanium dioxide: with step 2) preparation mix titanium LiFePO4 and titanium source behind combination drying, under inert gas, calcined 4～8 hours in 400 ℃～800 ℃.
Described source of iron is ferrous oxalate, iron oxide or ferric phosphate;
Described lithium source is lithium carbonate, lithium hydroxide or lithium dihydrogen phosphate;
Described phosphorus source is ammonium dihydrogen phosphate, ferric phosphate or lithium dihydrogen phosphate;
Described carbon source is glucose sugar, sucrose, polyethylene glycol, citric acid or superconduction carbon black;
The described titanium of step 1) source is titanium dioxide, lithium titanate, titanium sulfate or butyl titanate;
The described titanium of step 3) source is titanium dioxide or butyl titanate.
Below in conjunction with specific embodiment preparation method of the present invention is elaborated:
Embodiment 1
In ball mill, add 5kg zirconium ball and 2.5L deionized water, add 2.4875molFe while stirring
2O
3, 2.575mol Li
2CO
3, 5mol NH
4H
2PO
4, 0.025mol Ti (SO
4)
2(being dissolved in water) and 81g glucose, ball milling 6 hours after making the raw material porphyrize and mixing, carries out spray drying, crosses 100 mesh sieves; To mix the titanium precursor body under argon shield after the spray drying, in 350 ℃ of calcinings 5 hours, discharging was pulverized the back at 750 ℃ of calcining 16h; That gets generation mixes titanium LiFePO4 600g, adds titanium dioxide 12.25g, and 650g zirconium ball, solid phase ball milling be after 2 hours, and under inert gas 400 ℃, calcining 8h.The tap density of products obtained therefrom is 1.31g/ml, and phosphorus content is 1.27%; The battery of making, 1C discharge capacity are 125mAh/g.
In ball mill, add 5kg zirconium ball and 2.4L deionized water, add 4.925mol ferrous oxalate, 5mol LiH while stirring
2PO
4, 0.015mol Li
4Ti
5O
12, the 200g polyethylene glycol, ball milling 12 hours after making the raw material porphyrize and mixing, carries out spray drying, crosses 100 mesh sieves; To mix the titanium precursor body under argon shield after the spray drying, in 400 ℃ of calcinings 4 hours, discharging was pulverized the back at 600 ℃ of calcining 12h; That gets generation mixes titanium LiFePO4 600g, and adding 230mL concentration is the ethanolic solution of 0.5mol/L butyl titanate, adds 400g water again, ultra-fine ball milling 2h, spray drying then, under inert gas conditions 700 ℃ at last, calcining 6h.The tap density of products obtained therefrom is 1.18g/ml, and phosphorus content is 1.73%; The battery of making, 1C discharge capacity are 132mAh/g.
Embodiment 3
In ball mill, add 2kg zirconium ball and 1L deionized water, add 4.85mol ferric phosphate, 5.25mol LiOHH while stirring
2O, 0.15mol NH
4H
2PO
4, 300mL concentration is 0.5mol/L butyl titanate ethanolic solution and 27g superconduction carbon black, ball milling 8 hours after making the raw material porphyrize and mixing, carries out spray drying, crosses 100 mesh sieves; To mix the titanium precursor body under argon shield after the spray drying, in 500 ℃ of calcinings 3 hours, discharging was pulverized the back at 800 ℃ of calcining 8h; That gets preparation mixes titanium LiFePO4 600g, adds titanium dioxide 5g, and 1.2kg zirconium ball, solid phase ball milling be after 0.5 hour, and under inert gas 800 ℃, calcining 4h.The tap density of products obtained therefrom is 1.24g/ml, and phosphorus content is 1.46%; The battery of making, 1C discharge capacity are 129mAh/g.
A spot of as can be seen coated by titanium dioxide does not cause the marked change that material is formed from the XRD figure (Fig. 2) of synthetic sample, does not find dephasign, still is the LiFePO4 peak of pure phase.
The sample that synthesizes as can be seen from the SEM figure (Fig. 3) of synthetic sample is the aggregation of fine particle, the distribution homogeneous, and the raising high rate performance that so promptly helps material can improve drawing abillity again.
Claims (7)
1. the preparation method of a composite ferric lithium phosphate material is characterized in that may further comprise the steps:
1) the titanium precursor body is mixed in preparation: with lithium source, source of iron, titanium source and phosphorus source according to mol ratio 1～1.05: with carbon source join in ball mill at 0.97～0.995: 0.005～0.03: 1, the consumption of carbon source makes the mass percent of carbon in the finished product less than 2%, add quantitative deionized water and zirconium ball and do abrasive media, ball milling 6～12 hours, after making the raw material porphyrize and mixing, carry out spray drying, sieve;
2) the titanium LiFePO4 is mixed in preparation: dried material under inert gas shielding, 350～500 ℃ of calcinings 3～5 hours, is pulverized the back 600 ℃～800 ℃ calcinings 8～16 hours;
3) cladding titanium dioxide: with step 2) preparation mix titanium LiFePO4 and titanium source after mixing drying, under inert gas, calcined 4～8 hours in 400 ℃～800 ℃.
2. preparation method according to claim 1 is characterized in that: the described titanium of step 1) source is titanium dioxide, lithium titanate, titanium sulfate or butyl titanate; The described titanium of step 3) source is titanium dioxide or butyl titanate;
3. preparation method according to claim 1 is characterized in that: it is 1: 1～2 (quality) that the quantitative deionized water of the adding described in the step 1) satisfies solid-to-liquid ratio;
4. preparation method according to claim 1 is characterized in that: it is 2～4: 1 (quality) that the quantitative zirconium ball of the adding described in the step 1) satisfies ratio of grinding media to material;
5. preparation method according to claim 1 is characterized in that: the solid phase ball milling that is mixed into described in the step 3) mixes, and ratio of grinding media to material is 1～2: 1, and the ball milling time is 0.5～2 hour;
6. preparation method according to claim 1 is characterized in that: the described wet method super-fine ball milling that is mixed into of step 3) mixes, and solid content is 50%, and the ball milling time is 1～2 hour;
7. preparation method according to claim 1 is characterized in that: the covering amount of titanium dioxide is 0.8%～2% (mass percent) in the step 3).
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Cited By (21)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102509801A (en) * | 2011-11-15 | 2012-06-20 | 河北师范大学 | Method for preparing metal-doped lithium iron phosphate as cathode material of lithium ion battery |
| CN102642820A (en) * | 2012-03-29 | 2012-08-22 | 天津巴莫科技股份有限公司 | Preparation method of high-density spherical lithium iron phosphate |
| CN102738454A (en) * | 2012-07-19 | 2012-10-17 | 北大先行科技产业有限公司 | Surface coating material for cathode material of lithium ion battery and preparation method |
| CN102751493A (en) * | 2012-06-27 | 2012-10-24 | 武陟县鑫凯科技材料有限公司 | Preparation method of lithium iron phosphate |
| CN103022462A (en) * | 2012-12-20 | 2013-04-03 | 中国东方电气集团有限公司 | Preparation method for high-conductivity lithium titanate cathode material of lithium battery |
| CN103840146A (en) * | 2012-11-27 | 2014-06-04 | 西安物华新能源科技有限公司 | Preparation method of high-tap-density lithium titanate material |
| CN104752694A (en) * | 2013-12-30 | 2015-07-01 | 北京有色金属研究总院 | Improvement method for low temperature electrochemical performance of LiFePO4 material |
| CN105489824A (en) * | 2015-11-28 | 2016-04-13 | 芜湖迈特电子科技有限公司 | Quick-charging portable power source using lithium titanate battery |
| CN105870436A (en) * | 2016-04-25 | 2016-08-17 | 何凤英 | Preparation method of lithium titanate negative electrode material for lithium ion battery |
| CN109599547A (en) * | 2018-12-07 | 2019-04-09 | 贝特瑞（天津）纳米材料制造有限公司 | NaTi2(PO4)3-TiO2Preparation method and application of/C composite electrode material |
| CN109659509A (en) * | 2018-11-07 | 2019-04-19 | 贵州唯特高新能源科技有限公司 | A kind of titanium dioxide uniformly coats the preparation method of battery-grade iron phosphate |
| CN109713299A (en) * | 2018-11-07 | 2019-05-03 | 贵州唯特高新能源科技有限公司 | A kind of preparation method of metal oxide Uniform Doped battery-grade iron phosphate |
| CN110550615A (en) * | 2019-10-14 | 2019-12-10 | 王敏 | Preparation method of high-energy-density lithium iron phosphate |
| CN111170294A (en) * | 2020-01-19 | 2020-05-19 | 江苏乐能电池股份有限公司 | Preparation method of low-cost lithium iron phosphate composite material |
| CN111403732A (en) * | 2020-03-30 | 2020-07-10 | 江西安驰新能源科技有限公司 | High-energy-density lithium iron phosphate battery |
| CN111740101A (en) * | 2020-06-17 | 2020-10-02 | 东莞东阳光科研发有限公司 | Lithium iron phosphate material and preparation method thereof |
| CN112713272A (en) * | 2020-12-18 | 2021-04-27 | 浙江金鹰瓦力新能源科技有限公司 | Preparation method of modified lithium battery positive electrode material |
| CN115259128A (en) * | 2022-08-05 | 2022-11-01 | 湖北融通高科先进材料有限公司 | Preparation method of high-compaction high-capacity low-cost lithium iron phosphate |
| CN115477296A (en) * | 2022-09-30 | 2022-12-16 | 欧赛新能源科技股份有限公司 | Method for preparing high-rate titanium-doped lithium iron phosphate by one-step process |
| CN116387496A (en) * | 2023-06-02 | 2023-07-04 | 瑞浦兰钧能源股份有限公司 | Secondary battery positive electrode material, secondary battery positive electrode plate and secondary battery |
| WO2023207121A1 (en) * | 2022-04-25 | 2023-11-02 | 湖北万润新能源科技股份有限公司 | High-compaction lithium iron phosphate positive electrode material and preparation method therefor, and positive electrode and battery thereof |
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| CN101580238A (en) * | 2009-06-21 | 2009-11-18 | 海特电子集团有限公司 | Method for manufacturing composite lithium iron phosphate material and composite lithium iron phosphate material manufactured thereof |
| CN101635350A (en) * | 2009-08-31 | 2010-01-27 | 北京理工大学 | Preparation method of LiFePO4 of positive material of lithium ion battery |
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| CN101635350A (en) * | 2009-08-31 | 2010-01-27 | 北京理工大学 | Preparation method of LiFePO4 of positive material of lithium ion battery |
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|---|---|---|---|---|
| CN102509801A (en) * | 2011-11-15 | 2012-06-20 | 河北师范大学 | Method for preparing metal-doped lithium iron phosphate as cathode material of lithium ion battery |
| CN102642820A (en) * | 2012-03-29 | 2012-08-22 | 天津巴莫科技股份有限公司 | Preparation method of high-density spherical lithium iron phosphate |
| CN102751493A (en) * | 2012-06-27 | 2012-10-24 | 武陟县鑫凯科技材料有限公司 | Preparation method of lithium iron phosphate |
| CN102738454A (en) * | 2012-07-19 | 2012-10-17 | 北大先行科技产业有限公司 | Surface coating material for cathode material of lithium ion battery and preparation method |
| CN102738454B (en) * | 2012-07-19 | 2015-04-29 | 北大先行科技产业有限公司 | Surface coating material for cathode material of lithium ion battery and preparation method |
| CN103840146A (en) * | 2012-11-27 | 2014-06-04 | 西安物华新能源科技有限公司 | Preparation method of high-tap-density lithium titanate material |
| CN103022462A (en) * | 2012-12-20 | 2013-04-03 | 中国东方电气集团有限公司 | Preparation method for high-conductivity lithium titanate cathode material of lithium battery |
| CN103022462B (en) * | 2012-12-20 | 2015-07-08 | 中国东方电气集团有限公司 | Preparation method for high-conductivity lithium titanate cathode material of lithium battery |
| CN104752694A (en) * | 2013-12-30 | 2015-07-01 | 北京有色金属研究总院 | Improvement method for low temperature electrochemical performance of LiFePO4 material |
| CN105489824A (en) * | 2015-11-28 | 2016-04-13 | 芜湖迈特电子科技有限公司 | Quick-charging portable power source using lithium titanate battery |
| CN105870436A (en) * | 2016-04-25 | 2016-08-17 | 何凤英 | Preparation method of lithium titanate negative electrode material for lithium ion battery |
| CN109659509A (en) * | 2018-11-07 | 2019-04-19 | 贵州唯特高新能源科技有限公司 | A kind of titanium dioxide uniformly coats the preparation method of battery-grade iron phosphate |
| CN109713299A (en) * | 2018-11-07 | 2019-05-03 | 贵州唯特高新能源科技有限公司 | A kind of preparation method of metal oxide Uniform Doped battery-grade iron phosphate |
| CN109599547A (en) * | 2018-12-07 | 2019-04-09 | 贝特瑞（天津）纳米材料制造有限公司 | NaTi2(PO4)3-TiO2Preparation method and application of/C composite electrode material |
| CN109599547B (en) * | 2018-12-07 | 2022-05-13 | 天津市贝特瑞新能源科技有限公司 | NaTi2(PO4)3-TiO2Preparation method and application of/C composite electrode material |
| CN110550615A (en) * | 2019-10-14 | 2019-12-10 | 王敏 | Preparation method of high-energy-density lithium iron phosphate |
| CN111170294A (en) * | 2020-01-19 | 2020-05-19 | 江苏乐能电池股份有限公司 | Preparation method of low-cost lithium iron phosphate composite material |
| CN111403732A (en) * | 2020-03-30 | 2020-07-10 | 江西安驰新能源科技有限公司 | High-energy-density lithium iron phosphate battery |
| CN111740101B (en) * | 2020-06-17 | 2022-07-08 | 东莞东阳光科研发有限公司 | Lithium iron phosphate material and preparation method thereof |
| CN111740101A (en) * | 2020-06-17 | 2020-10-02 | 东莞东阳光科研发有限公司 | Lithium iron phosphate material and preparation method thereof |
| CN112713272A (en) * | 2020-12-18 | 2021-04-27 | 浙江金鹰瓦力新能源科技有限公司 | Preparation method of modified lithium battery positive electrode material |
| WO2023207121A1 (en) * | 2022-04-25 | 2023-11-02 | 湖北万润新能源科技股份有限公司 | High-compaction lithium iron phosphate positive electrode material and preparation method therefor, and positive electrode and battery thereof |
| CN115259128A (en) * | 2022-08-05 | 2022-11-01 | 湖北融通高科先进材料有限公司 | Preparation method of high-compaction high-capacity low-cost lithium iron phosphate |
| CN115259128B (en) * | 2022-08-05 | 2023-10-13 | 湖北融通高科先进材料集团股份有限公司 | Preparation method of high-compaction high-capacity low-cost lithium iron phosphate |
| CN115477296A (en) * | 2022-09-30 | 2022-12-16 | 欧赛新能源科技股份有限公司 | Method for preparing high-rate titanium-doped lithium iron phosphate by one-step process |
| CN116387496A (en) * | 2023-06-02 | 2023-07-04 | 瑞浦兰钧能源股份有限公司 | Secondary battery positive electrode material, secondary battery positive electrode plate and secondary battery |
| CN116387496B (en) * | 2023-06-02 | 2023-10-31 | 瑞浦兰钧能源股份有限公司 | Secondary battery positive electrode material, secondary battery positive electrode plate and secondary battery |
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|---|---|
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