CN103779563A - Method for preparing copper/carbon-coated lithium iron phosphate - Google Patents
Method for preparing copper/carbon-coated lithium iron phosphate Download PDFInfo
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- CN103779563A CN103779563A CN201410024883.XA CN201410024883A CN103779563A CN 103779563 A CN103779563 A CN 103779563A CN 201410024883 A CN201410024883 A CN 201410024883A CN 103779563 A CN103779563 A CN 103779563A
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- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01M—PROCESSES OR MEANS, e.g. BATTERIES, FOR THE DIRECT CONVERSION OF CHEMICAL ENERGY INTO ELECTRICAL ENERGY
- H01M4/00—Electrodes
- H01M4/02—Electrodes composed of, or comprising, active material
- H01M4/36—Selection of substances as active materials, active masses, active liquids
- H01M4/58—Selection of substances as active materials, active masses, active liquids of inorganic compounds other than oxides or hydroxides, e.g. sulfides, selenides, tellurides, halogenides or LiCoFy; of polyanionic structures, e.g. phosphates, silicates or borates
- H01M4/5825—Oxygenated metallic salts or polyanionic structures, e.g. borates, phosphates, silicates, olivines
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01B—NON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
- C01B25/00—Phosphorus; Compounds thereof
- C01B25/16—Oxyacids of phosphorus; Salts thereof
- C01B25/26—Phosphates
- C01B25/45—Phosphates containing plural metal, or metal and ammonium
-
- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01M—PROCESSES OR MEANS, e.g. BATTERIES, FOR THE DIRECT CONVERSION OF CHEMICAL ENERGY INTO ELECTRICAL ENERGY
- H01M4/00—Electrodes
- H01M4/02—Electrodes composed of, or comprising, active material
- H01M4/62—Selection of inactive substances as ingredients for active masses, e.g. binders, fillers
- H01M4/624—Electric conductive fillers
- H01M4/625—Carbon or graphite
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- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01M—PROCESSES OR MEANS, e.g. BATTERIES, FOR THE DIRECT CONVERSION OF CHEMICAL ENERGY INTO ELECTRICAL ENERGY
- H01M4/00—Electrodes
- H01M4/02—Electrodes composed of, or comprising, active material
- H01M4/62—Selection of inactive substances as ingredients for active masses, e.g. binders, fillers
- H01M4/624—Electric conductive fillers
- H01M4/626—Metals
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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
Abstract
The invention discloses a method for preparing copper/carbon-coated lithium iron phosphate. The method comprises the following steps: (1) ball-milling and mixing a lithium source, an iron source, a phosphorus source, a carbon source and a copper source, and adding a ball-milling solvent for full ball-milling, wherein the lithium source is a mixture of lithium iron phosphate and water-soluble lithium salt or lithium hydroxide, and the phosphorus source is at least one of phosphoric acid, ammonium dihydrogen phosphate and diammonium hydrogen phosphate; (2) after the ball-milling, performing spray drying treatment to obtain a precursor, and ball-milling the prepared precursor for 2-8h; and (3) after the ball-milling, heating the precursor for 400-800 DEG C at the temperature rise speed of 1-30 DEG C/min under the protection of inert gas, keeping the temperature constant for 5-15h, cooling to room temperature, and performing crushing to obtain a product. The method is full and uniform in reaction. The lithium iron phosphate prepared through the method is good in conductive performance and good in electrochemical performance.
Description
Technical field
A kind of method of preparing copper carbon-coated LiFePO 4 for lithium ion batteries with complex lithium source of the present invention, belongs to anode material of lithium battery preparation method.
Background technology
Have after removal lithium embedded function from A.K.Padhi reported first LiFePO4 in 1997, this material is just considered to most potential anode material for lithium-ion batteries, and it both can be widely used in high power battery, also can be applicable to the energy-storage battery of regenerative resource.The anode material of lithium battery using is both at home and abroad mainly cobalt acid lithium (LiCoO
2), it is the principal element that determines lithium battery performance, account for 30% of lithium battery material cost, cobalt acid lithium has more outstanding chemical property, it has discharge capacity high (135-140mAh/g), discharge platform is high by (80%, the advantage such as 3.6V), but it has very large shortcoming simultaneously: 1, production cost is high, price is high, the main material of producing cobalt acid lithium is expensive cobalt resource, its price is generally floated between ten thousand yuan/ton of 25-40, in cobalt acid lithium, cobalt content accounts for 61%, has therefore determined that the price of cobalt acid lithium must be expensive.2, the high-temperature behavior of cobalt acid lithium is bad, can not heavy-current discharge, cannot use as electrokinetic cell.LiFePO
4with at present common positive electrode LiCoO
2, LiNiO
2, LiMn
2o
4compare with the oxide of vanadium etc., not only price is lower for the oxide of iron, reserves abundant, nontoxic, and environmental pollution is little, is therefore day by day subject to researcher's attention.Lithium cell anode material of lithium iron phosphate has become the study hotspot in this field.
The direction of electrokinetic cell is lithium-ion-power cell, and ferric phosphate lithium cell is the highest battery of current fail safe.Security performance is as most important performance of electrokinetic cell, in the time that lithium battery is short-circuited, can not produce because of short circuit blast.Its oxidizing temperature, higher than 400 degree, can be placed in fire and burn.So positive electrode is that the battery of cobalt acid lithium and LiMn2O4 has to take various means for improving safety, and LiFePO 4 of anode material is innately to have fail safe.So LiFePO4 also just becomes the preferred material of power battery anode material naturally, along with lithium battery is progressively expanded to the field such as electric bicycle, electric automobile, the demand of lithium cell anode material of lithium iron phosphate will significantly increase.
At present, the patent of preparation method's application of LiFePO4 is a lot, as Chinese patent application 201310414217.2 and CN103178266A etc., but these preparation methods exist presoma reaction inhomogeneous, react the defect such as insufficient, there is the problems such as electric conductivity is poor in the LiFePO4 preparing.
Summary of the invention
Technical problem to be solved by this invention is to provide a kind of reaction to prepare more fully, uniformly the method for the coated phosphoric acid abrasive grit of copper carbon, and LiFePO4 prepared by the method conducts electricity very well, chemical property is good.
Technical scheme of the present invention is as follows: a kind of method of preparing copper carbon-coated LiFePO 4 for lithium ion batteries, is characterized in that: complete in accordance with the following steps:
(1), lithium source, source of iron, phosphorus source, carbon source and Tong Yuan are carried out to ball milling mixing, and add the abundant ball milling of ball milling solvent, described lithium source is the mixing of lithium carbonate and water-soluble lithium salts or lithium hydroxide, and described phosphorus source is at least one in phosphoric acid, ammonium dihydrogen phosphate, diammonium hydrogen phosphate;
(2), ball milling carries out spray drying treatment after complete, obtains presoma, then by the presoma ball milling 2-8h making;
(3), ball milling complete after, presoma, under inert gas shielding, is heated to 400 ℃～800 ℃ with the programming rate of 1-30 ℃/min, and constant temperature 5～15 hours, then is cooled to room temperature, after fragmentation, obtain product.
Adopt technique scheme, in the time that liquid phase is mixed, the lithium salts of solubility and lithium hydroxide can mix more even with the powder such as source of iron.Especially in the time selecting lithium hydroxide, lithium hydroxide reacts with phosphoric acid, ammonium dihydrogen phosphate, diammonium hydrogen phosphate and belongs to acid-base neutralization reaction and can emit a large amount of heat, promotes the further generation of reaction.Add lithium carbonate as lithium source, lithium carbonate can produce a large amount of gas while reaction with phosphoric acid, ammonium dihydrogen phosphate, diammonium hydrogen phosphate, and in reactor liquid phase, inside can form moment explosion (bubble bursts) can to promote that product mixes with the source of iron in raw material more even.In the alkaline reaction environment mixing with lithium carbonate by solubility lithium salts or lithium hydroxide, add carbon source to react with copper ion and form copper carbon composite lithium iron phosphate presoma, then through the carbonization of reducing atmosphere sintering, copper ion is reduced to copper film and is jointly coated on LiFePO4 surface raising material conductivity.React prepared homogeneous presoma early stage by this compound promotion, the final synthetic LiFePO 4 material of sintering has excellent chemical property, particularly high rate capability.
As preferably: described in step (1), water-soluble lithium salts is lithium acetate.
In technique scheme: the mol ratio in described lithium source, source of iron, phosphorus source, copper source is 1:1:1:0.005-0.015, the quality of described carbon source is the 2-10% of all lithiums source, source of iron, phosphorus source gross mass.
As preferably: in step (1), described ball milling solvent is water, and the time of ball milling is 5-10 hour.
In technique scheme: described source of iron is at least one in di-iron trioxide, iron hydroxide, ferrous oxalate, iron oxide, described carbon source is at least one in sucrose, glucose, lactose, citric acid, starch, and described copper source is at least one in Schweinfurt green, copper nitrate, Kocide SD, copper carbonate, copper powder.
Beneficial effect: the method that the present invention prepares LiFePO4 has following outstanding feature: when mix in liquid phase (1), the lithium hydroxide of solubility can mix more even with powders such as sources of iron.Especially in the time selecting lithium hydroxide, lithium hydroxide reacts with phosphoric acid, ammonium dihydrogen phosphate, diammonium hydrogen phosphate and belongs to acid-base neutralization reaction and can emit a large amount of heat, promotes the further generation of reaction.(2) add lithium carbonate as lithium source, lithium carbonate can produce a large amount of gas while reaction with phosphoric acid, ammonium dihydrogen phosphate, diammonium hydrogen phosphate, and in reactor liquid phase, inside can form moment explosion (bubble bursts) can to promote that product mixes with the source of iron in raw material more even.(3) in the alkaline reaction environment mixing with lithium carbonate by lithium hydroxide, add carbon source to react with copper ion and form copper carbon composite lithium iron phosphate presoma, then through the carbonization of reducing atmosphere sintering, copper ion is reduced to copper film and is jointly coated on LiFePO4 surface raising material conductivity.(4) react prepared homogeneous presoma early stage by this compound promotion, the final synthetic LiFePO 4 material of sintering has excellent chemical property, particularly high rate capability.
Accompanying drawing explanation
Fig. 1 is the lithium battery made with material prepared by the embodiments of the invention 1-5 discharge curve typical figure under 1C multiplying power;
Fig. 2 is the lithium ion battery made with material prepared by the embodiment of the present invention 1-5 cyclic curve typical figure under 1C multiplying power.
Fig. 3 is SEM figure before example 2 synthesized material fragmentations.
Fig. 4 is SEM figure after example 2 synthesized material fragmentations.
Embodiment
Below in conjunction with drawings and Examples, the invention will be further described:
Embodiment 1:
Get 0.2mol lithium hydroxide LiOHH
2o, 0.4mol lithium carbonate Li
2cO
3, 0.5mol di-iron trioxide Fe
2o
3, 1mol ammonium dihydrogen phosphate NH
4h
2pO
4with 4.75g glucose and 0.01mol Schweinfurt green.It is that ball milling solvent is at ball mill ball milling 8h that ball milling adds water after mixing; the quality of water is 2 times of all raw material quality; by dry the precursor powder of spraying; again by presoma ball milling 2h; precursor powder, putting into tube furnace take nitrogen as protection, is raised to 700 ℃ with 15 ℃/min, and constant temperature is after 8 hours; naturally cool to again room temperature and take out, obtain copper carbon-coated LiFePO 4 for lithium ion batteries finished material.
Positive electrode copper carbon-coated LiFePO 4 for lithium ion batteries that the present embodiment is made, acetylene black, PVDF in mass ratio 91:5:4 mix, then be coated on the aluminium foil of 0.02mm, after fully dry, obtain anode pole piece, then fill to obtain experimental cell at the glove box that is full of argon gas; Finally on LAND cell tester, carry out charge-discharge performance test: carry out charge-discharge test with 1C multiplying power, charging/discharging voltage is 3.65～2V, it is 128mAh/g that room temperature records reversible specific capacity first.
Embodiment 2:
Get 0.4mol lithium hydroxide LiOHH
2o, 0.3mol lithium carbonate Li
2cO
3, 0.5mol di-iron trioxide Fe
2o
3, 1mol diammonium hydrogen phosphate (NH
4)
2hPO
4with 18g glucose and 7.94g citric acid and 0.01mol copper carbonate.It is ball-milling medium ball mill ball milling 5h that ball milling adds water after mixing; the quality of water is 2 times of all raw material quality; by dry the precursor powder of spraying; again by presoma ball milling 8h; precursor powder, putting into tube furnace take nitrogen as protection, is raised to 650 ℃ with 15 ℃/min, and constant temperature is after 15 hours; naturally cool to again room temperature and take out, obtain copper carbon-coated LiFePO 4 for lithium ion batteries finished material.
Copper carbon-coated LiFePO 4 for lithium ion batteries that the present embodiment is made, acetylene black, PVDF in mass ratio 91:5:4 mix, and are then coated on the aluminium foil of 0.02mm, obtain anode pole piece, then fill to obtain experimental cell at the glove box that is full of argon gas after fully dry; Finally on LAND cell tester, carry out charge-discharge performance test: carry out charge-discharge test with 0.1C multiplying power, charging/discharging voltage is 3.65～2V, it is 138mAh/g that room temperature records reversible specific capacity first.
Embodiment 3:
Get 0.5mol lithium hydroxide LiOHH
2o, 0.25mol lithium carbonate Li
2cO
3, 1mol iron hydroxide Fe (OH)
3, 1mol ammonium dihydrogen phosphate NH
4h
2pO
4, and 13.6g glucose and 0.005mol copper powder.It is ball-milling medium ball mill ball milling 10h that ball milling adds water after mixing; the quality of water is 3 times of all raw material quality; by dry the precursor powder of spraying; again by presoma ball milling 4h; precursor powder, putting into tube furnace take nitrogen as protection, is raised to 800 ℃ with 30 ℃/min, and constant temperature is after 5 hours; naturally cool to again room temperature and take out, obtain copper carbon-coated LiFePO 4 for lithium ion batteries finished material.
The coated LiFePO4 of copper carbon that the present embodiment is made, acetylene black, PVDF in mass ratio 91:5:4 mix, then be coated on the aluminium foil of 0.02mm, after fully dry, obtain anode pole piece, then fill to obtain experimental cell at the glove box that is full of argon gas; Finally on LAND cell tester, carry out charge-discharge performance test: carry out charge-discharge test with 0.1C multiplying power, charging/discharging voltage is 3.65～2V, it is 120mAh/g that room temperature records reversible specific capacity first.
Embodiment 4:
Get 0.8mol lithium hydroxide LiOHH
2o, 0.1mol lithium carbonate Li
2cO
3, 1mol ferrous oxalate FeC
2o
42H
2o, 1mol phosphoric acid H
3pO
4with 22.5g glucose and 0.015mol Kocide SD.It is ball-milling medium ball mill ball milling 8h that ball milling adds water after mixing; the quality of water is 2 times of all raw material quality; by dry the precursor powder of spraying; again by presoma ball milling 5h; precursor powder, putting into tube furnace take nitrogen as protection, is raised to 400 ℃ with 1 ℃/min, and constant temperature is after 15 hours; naturally cool to again room temperature and take out, obtain copper carbon-coated LiFePO 4 for lithium ion batteries finished material.
By positive electrode LiFePO
4/ C powder, acetylene black, PVDF in mass ratio 91:5:4 mix, and are then coated on the aluminium foil of 0.02mm, obtain anode pole piece, then fill to obtain experimental cell at the glove box that is full of argon gas after fully dry; Finally on LAND cell tester, carry out charge-discharge performance test: carry out charge-discharge test with 0.1C multiplying power, charging/discharging voltage is 3.65～2V, it is 132mAh/g that room temperature records reversible specific capacity first.
Embodiment 5:
Get 0.6mol lithium acetate, 0.2mol lithium carbonate Li
2cO
3, 1mol ferrous oxalate FeC
2o
42H
2o, 1mol diammonium hydrogen phosphate (NH
4)
2hPO
4with 0.1mol glucose and 14g citric acid 0.01mol copper nitrate.It is ball-milling medium ball mill ball milling 8h that ball milling adds water after mixing; the quality of water is 1.5 times of all raw material quality; by dry the precursor powder of spraying; again by presoma ball milling 2h; precursor powder, putting into tube furnace take nitrogen as protection, is raised to 700 ℃ with 15 ℃/min, and constant temperature is after 6 hours; naturally cool to again room temperature and take out, obtain copper carbon-coated LiFePO 4 for lithium ion batteries finished material.。
The coated LiFePO4 of copper carbon prepared by the present embodiment, acetylene black, PVDF in mass ratio 91:5:4 mix, then be coated on the aluminium foil of 0.02mm, after fully dry, obtain anode pole piece, then fill to obtain experimental cell at the glove box that is full of argon gas; Finally on LAND cell tester, carry out charge-discharge performance test: carry out charge-discharge test with 0.1C multiplying power, charging/discharging voltage is 3.65～2V, it is 118mAh/g that room temperature records reversible specific capacity first.
The present invention is not limited to specific embodiment, a kind of or mixing in all right sucrose of described carbon source, glucose, lactose, citric acid, starch.A kind of or the mixing such as all right Schweinfurt green in described copper source, copper nitrate, Kocide SD, copper carbonate, copper powder.Described source of iron can also be selected a kind of or mixing in di-iron trioxide, ferrous oxalate, iron hydroxide, iron oxide.Aim all falls within the scope of protection of the present invention as long as any distortion being equal on basis of the present invention.
Claims (5)
1. a method of preparing copper carbon-coated LiFePO 4 for lithium ion batteries, is characterized in that: complete in accordance with the following steps:
(1), lithium source, source of iron, phosphorus source, carbon source and Tong Yuan are carried out to ball milling mixing, and add the abundant ball milling of ball milling solvent, described lithium source is the mixing of lithium carbonate and water-soluble lithium salts or lithium hydroxide, and described phosphorus source is at least one in phosphoric acid, ammonium dihydrogen phosphate, diammonium hydrogen phosphate;
(2), ball milling carries out spray drying treatment after complete, obtains presoma, then by the presoma ball milling 2-8h making;
(3), ball milling complete after, presoma, under inert gas shielding, is heated to 400 ℃～800 ℃ with the programming rate of 1-30 ℃/min, and constant temperature 5～15 hours, then is cooled to room temperature, after fragmentation, obtain product.
2. the method for preparing according to claim 1 copper carbon-coated LiFePO 4 for lithium ion batteries, is characterized in that: described in step (1), water-soluble lithium salts is lithium acetate.
3. prepare according to claim 1 the method for copper carbon-coated LiFePO 4 for lithium ion batteries, it is characterized in that: the mol ratio in described lithium source, source of iron, phosphorus source, copper source is 1:1:1:0.005-0.015, the quality of described carbon source is the 2-10% of all lithiums source, source of iron, phosphorus source gross mass.
4. according to the method for preparing copper carbon-coated LiFePO 4 for lithium ion batteries described in claim 1-3 any one, it is characterized in that: in step (1), described ball milling solvent is water, and the time of ball milling is 5-10 hour.
5. according to the method for preparing copper carbon-coated LiFePO 4 for lithium ion batteries described in claim 1-3 any one, it is characterized in that: described source of iron is at least one in di-iron trioxide, iron hydroxide, ferrous oxalate, iron oxide, described carbon source is at least one in sucrose, glucose, lactose, citric acid, starch, and described copper source is at least one in Schweinfurt green, copper nitrate, Kocide SD, copper carbonate, copper powder.
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Cited By (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN106450177A (en) * | 2016-08-31 | 2017-02-22 | 珠海光宇电池有限公司 | Composite negative electrode material, preparation method and lithium battery |
| CN106920925A (en) * | 2015-12-27 | 2017-07-04 | 深圳市沃特玛电池有限公司 | A kind of lithium iron phosphate positive material preparation method |
| CN107814564A (en) * | 2016-09-13 | 2018-03-20 | 上海硅酸盐研究所中试基地 | Method prepared by a kind of phosphoric acid titanium compound batch of inexpensive carbon coating |
| CN109795998A (en) * | 2018-12-29 | 2019-05-24 | 合肥融捷能源材料有限公司 | A kind of preparation method and lithium iron phosphate positive material promoting lithium iron phosphate positive material compacted density |
| CN114551823A (en) * | 2021-12-28 | 2022-05-27 | 江苏容汇通用锂业股份有限公司 | Preparation method and application of metal-doped carbon in-situ coated lithium iron phosphate electrode material |
| CN116730313A (en) * | 2023-06-25 | 2023-09-12 | 江西智锂科技股份有限公司 | Preparation method of ultralow-temperature lithium iron phosphate positive electrode material |
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Cited By (7)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN106920925A (en) * | 2015-12-27 | 2017-07-04 | 深圳市沃特玛电池有限公司 | A kind of lithium iron phosphate positive material preparation method |
| CN106450177A (en) * | 2016-08-31 | 2017-02-22 | 珠海光宇电池有限公司 | Composite negative electrode material, preparation method and lithium battery |
| CN107814564A (en) * | 2016-09-13 | 2018-03-20 | 上海硅酸盐研究所中试基地 | Method prepared by a kind of phosphoric acid titanium compound batch of inexpensive carbon coating |
| CN107814564B (en) * | 2016-09-13 | 2019-12-17 | 上海硅酸盐研究所中试基地 | Low-cost carbon-coated titanium phosphate compound batch preparation method |
| CN109795998A (en) * | 2018-12-29 | 2019-05-24 | 合肥融捷能源材料有限公司 | A kind of preparation method and lithium iron phosphate positive material promoting lithium iron phosphate positive material compacted density |
| CN114551823A (en) * | 2021-12-28 | 2022-05-27 | 江苏容汇通用锂业股份有限公司 | Preparation method and application of metal-doped carbon in-situ coated lithium iron phosphate electrode material |
| CN116730313A (en) * | 2023-06-25 | 2023-09-12 | 江西智锂科技股份有限公司 | Preparation method of ultralow-temperature lithium iron phosphate positive electrode material |
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