CN107381529A - The preparation method of high performance lithium ion battery positive electrode material lithium iron phosphate - Google Patents
The preparation method of high performance lithium ion battery positive electrode material lithium iron phosphate Download PDFInfo
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- CN107381529A CN107381529A CN201710657592.8A CN201710657592A CN107381529A CN 107381529 A CN107381529 A CN 107381529A CN 201710657592 A CN201710657592 A CN 201710657592A CN 107381529 A CN107381529 A CN 107381529A
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- lithium
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- ion battery
- positive electrode
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Classifications
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- 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
- H01M10/00—Secondary cells; Manufacture thereof
- H01M10/05—Accumulators with non-aqueous electrolyte
- H01M10/052—Li-accumulators
- H01M10/0525—Rocking-chair batteries, i.e. batteries with lithium insertion or intercalation in both electrodes; Lithium-ion batteries
-
- 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
-
- 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 present invention relates to the preparation method of high performance lithium ion battery positive electrode material lithium iron phosphate, this method is used as source of iron and phosphorus source using the ferric phosphate for being doped with a small amount of ferrous phosphate, and add dispersant in reaction raw materials and reacted in autoclave, the material of preparation is successively spray-dried, sinter and tunnel drying handles to obtain lithium iron phosphate positive material.The high LiFePO4 product of even particle size distribution, compacted density has been prepared in the present invention.
Description
Technical field
The present invention relates to the preparation in battery material field, more particularly to high performance lithium ion battery positive electrode material lithium iron phosphate
Method.
Background technology
Lithium ion battery is the green high-capacity battery of a new generation, have voltage is high, energy density is big, good cycle, from
The many merits such as small, memory-less effect, the operating temperature range of discharging be wide, are widely used in mobile phone, notebook computer, number
Camera, video camera, electronic instrument etc., also have in fields such as UPS, electric tool, electric bicycle, electric automobile, energy-storage batteries
There is the application prospect of light.In recent years, the yield of lithium ion battery is skyrocketed through, and application field constantly expands, it has also become two
The eleventh century new high-tech product significant to national economy and people's lives.
At present, lithium ion battery has reached its maturity in the compact battery field of portable type electronic product, and application is just
Progressively to middle Large Copacity, in high-power power type and accumulation energy type field of batteries expand.Positive electrode is the weight of lithium ion battery
Part is wanted, its performance largely determines the combination property of battery.Therefore, the research to positive electrode and performance
Improvement is one of core of lithium ion battery development.
The content of the invention
The present invention is intended to provide the preparation method of high performance lithium ion battery positive electrode material lithium iron phosphate, uses source of iron, lithium
LiFePO4 is made in sintering after source, carbon source and dispersant react at high temperature, has obtained even particle size distribution and powder is compacted
The high product of density.
The preparation method of the lithium iron phosphate positive material of the present invention, comprises the following steps:
S1. source of iron and phosphorus source are added into reactor, distilled water is added and prepares mixed solution;The source of iron is with phosphorus source
It is doped with the ferric phosphate of a small amount of ferrous phosphate;
S2. the mass ratio of addition lithium source, carbon source and dispersant into mixed solution, the iron phosphorus source and dispersant is 100:
0.05-0.2, it is 5-60% to stir and adjust solid content, then heats to 120-180 DEG C, reaction time 1-3h;
S3. said mixture material is fed directly into spray dryer and is carried out continuously be spray-dried twice, EAT is
120-150 DEG C, 100-120 DEG C of outlet temperature;
S4. dried material is sintered under inert gas shielding;
S5. material after sintering is subjected to tunnel drying and produces lithium iron phosphate positive material, drying temperature is 100-150 DEG C.
Preferably, the ratio of ferrous phosphate is 0-10% in the source of iron and phosphorus source.
Preferably, the mol ratio of the iron phosphorus source and lithium source is 1:1-1.05.
Preferably, the mass ratio of the iron phosphorus source and carbon source is 1:0.02-0.1.
Preferably, the sintering temperature is 500-800 DEG C, sintering time 6-15h.
Preferably, the lithium source is the one or more in lithium hydroxide, lithium carbonate, lithium acetate, lithium oxalate.
Preferably, the carbon source be electrically conductive graphite, it is CNT, graphene, sucrose, glucose, fructose, citric acid, poly-
One or more in vinyl alcohol, polyethylene glycol, polyethers.
Preferably, the dispersant is trimethylolpropane, pentaerythrite, bipentaerythrite, lauryl sodium sulfate, ten
Dialkyl sulfonates, APES, dioctyl succinate disulfonate acid, Sucrose Fatty Acid Ester, fatty acid sorbitan, poly- sorb
One or more in ester, polyoxyethylene, methyl anyl alcohol, cellulose derivative, fatty acid polyethylene glycol ester.
Preferably, the inert gas refers to any one gas or gas not chemically reacted with reactant and product
Body mixture, such as the one or more in hydrogen, nitrogen, carbon monoxide, decomposed ammonia and periodic table of elements zero group gas.
Preferably, the reaction pressure is 0.5-10Mpa.
The beneficial effects of the invention are as follows:
1) present invention using ferrous phosphate doping phosphoric acid iron as raw material, can be by controlling the ratio of phosphorus, iron, lithium to control
LiFePO4 processed is in performances such as the electric capacity of different multiplying, cycle lives;
2) present invention adds a small amount of dispersant in reactant, can be well mixed material by stirring, eliminate
Ball milling process, shortens incorporation time, saves equipment investment and power consumption, reduces production cost;Improve production simultaneously
The electric capacity and cycle efficieny of product;
3) present invention mixes to material at high temperature using autoclave so that Granularity Distribution is uniform and powder
Compacted density is higher.
Embodiment
Embodiment 1
Present embodiment discloses the preparation method of high performance lithium ion battery positive electrode material lithium iron phosphate, including following step
Suddenly:
S1. 100g is put into reactor and is doped with the ferric phosphate of ferrous phosphate and accounted for as iron phosphorus source, wherein ferrous phosphate
1%, it is then injected into 200g distilled water and prepares mixed solution, pressure is 2MPa in reactor;
S2. lithium carbonate, glucose and trimethylolpropane are added into mixed solution, stirs and adjusts solid content and be
50%, 150 DEG C are then warming up in the case where being stirred continuously, reaction 1h makes it well mixed;Mole of the iron phosphorus source and lithium carbonate
Than for 1:1, the mass ratio of the iron phosphorus source and glucose is 1:0.05, the mass ratio of the iron phosphorus source and trimethylolpropane is
100:0.05;
S3. material after mixing is fed directly into spray dryer and is carried out continuously be spray-dried twice, EAT 150
DEG C, outlet temperature is 120 DEG C;
S4. material after drying is sintered under inert gas shielding, sintering temperature is 800 DEG C, sintering time 8h;
S5. material after sintering is subjected to tunnel drying at 100 DEG C and produces lithium iron phosphate positive material.
The compacted density of the LiFePO 4 material of the present embodiment is 1.88g/cm3.
Embodiment 2
Present embodiment discloses the preparation method of high performance lithium ion battery positive electrode material lithium iron phosphate, including following step
Suddenly:
S1. 100g is put into reactor and is doped with the ferric phosphate of ferrous phosphate and accounted for as iron phosphorus source, wherein ferrous phosphate
10%, it is then injected into 200g distilled water and prepares mixed solution, pressure is 5MPa in reactor;
S2. lithium acetate, sucrose and pentaerythrite are added into mixed solution, it is 60% to stir and adjust solid content, then
120 DEG C are warming up in the case where being stirred continuously, reaction 3h makes it well mixed;The iron phosphorus source and the mol ratio of lithium carbonate are 1:1, institute
The mass ratio for stating iron phosphorus source and sucrose is 1:0.1, the mass ratio of the iron phosphorus source and pentaerythrite is 100:0.1;
S3. material after mixing is fed directly into spray dryer and is carried out continuously be spray-dried twice, EAT 150
DEG C, outlet temperature is 120 DEG C;
S4. material after drying is sintered under inert gas shielding, sintering temperature is 600 DEG C, and sintering time is
15h;
S5. material after sintering is subjected to tunnel drying at 150 DEG C and produces lithium iron phosphate positive material.
The compacted density of the LiFePO 4 material of the present embodiment is 1.85g/cm3.
Embodiment 3
Present embodiment discloses the preparation method of high performance lithium ion battery positive electrode material lithium iron phosphate, including following step
Suddenly:
S1. 100g is put into reactor and is doped with the ferric phosphate of ferrous phosphate and accounted for as iron phosphorus source, wherein ferrous phosphate
5%, it is then injected into 200g distilled water and prepares mixed solution, pressure is 8MPa in reactor;
S2. lithium hydroxide, electrically conductive graphite and polyoxyethylene are added into mixed solution, stirs and adjusts solid content and be
10%, 180 DEG C are then warming up in the case where being stirred continuously, reaction 1.5h makes it well mixed;The iron phosphorus source and lithium carbonate rub
You are than being 1:1.05, the mass ratio of the iron phosphorus source and electrically conductive graphite is 1:0.05, the iron phosphorus source and polyoxyethylated quality
Than for 100:0.2;
S3. material after mixing is fed directly into spray dryer and is carried out continuously be spray-dried twice, EAT 120
DEG C, outlet temperature is 110 DEG C;
S4. material after drying is sintered under inert gas shielding, sintering temperature is 700 DEG C, and sintering time is
12h;
S5. material after sintering is subjected to tunnel drying at 130 DEG C and produces lithium iron phosphate positive material.
The compacted density of the LiFePO 4 material of the present embodiment is 1.80g/cm3.
LiFePO 4 material prepared by embodiment 1-3 is mixed with polyvinyl chloride, nmp solvent and conductive black,
Further stirring 3-5h fully mixes to obtain slurry after ultrasonic disperse, and slurry is applied on aluminium foil front, and drying obtains positive pole
Pole piece;Using lithium paper tinsel as button cell to electrode, is assembled into the glove box full of argon gas, constant current charge-discharge test is carried out,
Charging/discharging voltage is 2.5-4.2V, tests specific capacitance of the LiFePO4 under different multiplying at room temperature.
Test result such as following table:
Embodiment | 1 | 2 | 3 |
Specific capacitance (mAh/g) under 0.1C multiplying powers | 182 | 180 | 183 |
Specific capacitance (mAh/g) under 1C multiplying powers | 175 | 172 | 174 |
Specific capacitance (mAh/g) under 10C multiplying powers | 116 | 115 | 118 |
Cycle efficieny (1000 weeks) | 81% | 80% | 78% |
Powder compacted density (g/cm3) | 1.88 | 1.85 | 1.80 |
Comparative example 1
Present embodiment discloses the preparation method of high performance lithium ion battery positive electrode material lithium iron phosphate, including following step
Suddenly:
S1. 100g is put into reactor and is doped with the ferric phosphate of ferrous phosphate and accounted for as iron phosphorus source, wherein ferrous phosphate
5%, it is then injected into 200g distilled water and prepares mixed solution, pressure is 8MPa in reactor;
S2. lithium hydroxide, electrically conductive graphite are added into mixed solution, it is 10% to stir and adjust solid content, then not
180 DEG C are warming up under disconnected stirring, reaction 1.5h makes it well mixed;The iron phosphorus source and the mol ratio of lithium carbonate are 1:1.05
The mass ratio of the iron phosphorus source and electrically conductive graphite is 1:0.05;
S3. material after mixing is fed directly into spray dryer and is carried out continuously be spray-dried twice, EAT 120
DEG C, outlet temperature is 110 DEG C;
S4. material after drying is sintered under inert gas shielding, sintering temperature is 700 DEG C, and sintering time is
12h;
S5. material after sintering is subjected to tunnel drying at 130 DEG C and produces lithium iron phosphate positive material.
The compacted density of the LiFePO 4 material of the present embodiment is 1.45g/cm3.
Comparative example 2
Present embodiment discloses the preparation method of high performance lithium ion battery positive electrode material lithium iron phosphate, including following step
Suddenly:
S1. 100g is put into reactor and is doped with the ferric phosphate of ferrous phosphate and accounted for as iron phosphorus source, wherein ferrous phosphate
5%, it is then injected into 200g distilled water and prepares mixed solution, pressure is 8MPa in reactor;
S2. lithium hydroxide, electrically conductive graphite are added into mixed solution, it is 10% to stir and adjust solid content, then not
180 DEG C are warming up under disconnected stirring, reaction 6h makes it well mixed;The iron phosphorus source and the mol ratio of lithium carbonate are 1:1.05 institute
The mass ratio for stating iron phosphorus source and electrically conductive graphite is 1:0.05;
S3. material after mixing is fed directly into spray dryer and is carried out continuously be spray-dried twice, EAT 120
DEG C, outlet temperature is 110 DEG C;
S4. material after drying is sintered under inert gas shielding, sintering temperature is 700 DEG C, and sintering time is
12h;
S5. material after sintering is subjected to tunnel drying at 130 DEG C and produces lithium iron phosphate positive material.
The compacted density of the LiFePO 4 material of the present embodiment is 1.60g/cm3。
Comparative example 3
Present embodiment discloses the preparation method of high performance lithium ion battery positive electrode material lithium iron phosphate, including following step
Suddenly:
S1. 100g is put into reactor and is doped with the ferric phosphate of ferrous phosphate and accounted for as iron phosphorus source, wherein ferrous phosphate
5%, it is then injected into 200g distilled water and prepares mixed solution, pressure is 8MPa in reactor;
S2. lithium hydroxide, electrically conductive graphite and dodecyl sodium sulfate are added into mixed solution, stirs and adjusts solid content
For 10%, 80 DEG C are then warming up in the case where being stirred continuously, reaction 1.5h makes it well mixed;The iron phosphorus source and lithium carbonate rub
You are than being 1:1.05, the mass ratio of the iron phosphorus source and electrically conductive graphite is 1:0.05, the iron phosphorus source and dodecyl sodium sulfate
Mass ratio be 100:0.2;
S3. material after mixing is fed directly into spray dryer and is carried out continuously be spray-dried twice, EAT 120
DEG C, outlet temperature is 110 DEG C;
S4. material after drying is sintered under inert gas shielding, sintering temperature is 700 DEG C, and sintering time is
12h;
S5. material after sintering is subjected to tunnel drying at 130 DEG C and produces lithium iron phosphate positive material.
The compacted density of the LiFePO 4 material of the present embodiment is 1.70g/cm3。
LiFePO 4 material prepared by comparative example 1-3 and polyvinyl chloride, nmp solvent and conductive black are mixed
Close, further stirring 3-5h fully mixes to obtain slurry after ultrasonic disperse, and slurry is applied on aluminium foil front, and drying obtains just
Pole pole piece;Using lithium paper tinsel as to electrode, button cell is assembled into the glove box full of argon gas, carries out constant current charge-discharge survey
Examination, charging/discharging voltage 2.5-4.2V, specific capacitance of the LiFePO4 under different multiplying is tested at room temperature.
Test result such as following table:
Comparative example | 1 | 2 | 3 |
Specific capacitance (mAh/g) under 0.1C multiplying powers | 150 | 162 | 175 |
Specific capacitance (mAh/g) under 1C multiplying powers | 135 | 141 | 168 |
Specific capacitance (mAh/g) under 10C multiplying powers | 88 | 92 | 118 |
Cycle efficieny (1000 weeks) | 35% | 41% | 75% |
Powder compacted density (g/cm3) | 1.45 | 1.60 | 1.70 |
It can be seen that by embodiment 1-3 and comparative example 1-3 and add dispersant the electric capacity of product, circulation are imitated
Rate and the compacted density of powder have larger lifting.
The beneficial effects of the invention are as follows:
1) present invention using ferrous phosphate doping phosphoric acid iron as raw material, can be by controlling the ratio of phosphorus, iron, lithium to control
LiFePO4 processed is in performances such as the electric capacity of different multiplying, cycle lives;
2) present invention adds a small amount of dispersant in reactant, can be well mixed material by stirring, eliminate
Ball milling process, shortens incorporation time, saves equipment investment and power consumption, reduces production cost;Improve production simultaneously
The electric capacity and cycle efficieny of product;
3) present invention mixes to material at high temperature using autoclave so that Granularity Distribution is uniform and powder
Compacted density is higher.
Described above is the preferred embodiment of the present invention, it is noted that for those skilled in the art
For, under the premise without departing from the principles of the invention, some improvements and modifications can also be made, these improvements and modifications are also considered as
Protection scope of the present invention.
Claims (8)
1. the preparation method of high performance lithium ion battery positive electrode material lithium iron phosphate, it is characterised in that comprise the following steps:
S1. source of iron and phosphorus source are added into reactor, distilled water is added and prepares mixed solution;The source of iron is doping with phosphorus source
The ferric phosphate of a small amount of ferrous phosphate;
S2. the mass ratio of addition lithium source, carbon source and dispersant into mixed solution, the iron phosphorus source and dispersant is 100:
0.05-0.2, it is 5-60% to stir and adjust solid content, then heats to 120-180 DEG C, reaction time 1-3h;
S3. said mixture material is fed directly into spray dryer and is carried out continuously be spray-dried twice, EAT 120-
150℃;
S4. dried material is sintered under inert gas shielding;
S5. material after sintering is subjected to tunnel drying and produces lithium iron phosphate positive material, drying temperature is 100-150 DEG C.
2. the preparation method of high performance lithium ion battery positive electrode material lithium iron phosphate according to claim 1, its feature exists
In the ratio of ferrous phosphate is 0-10% in the source of iron and phosphorus source.
3. the preparation method of high performance lithium ion battery positive electrode material lithium iron phosphate according to claim 1 or 2, its feature
It is, the mol ratio of the iron phosphorus source and lithium source is 1:1-1.05.
4. the preparation method of high performance lithium ion battery positive electrode material lithium iron phosphate according to claim 3, its feature exists
In the mass ratio of the iron phosphorus source and carbon source is 1:0.02-0.1.
5. the preparation method of high performance lithium ion battery positive electrode material lithium iron phosphate according to claim 4, its feature exists
In the sintering temperature is 500-800 DEG C, sintering time 6-15h.
6. the preparation method of high performance lithium ion battery positive electrode material lithium iron phosphate according to claim 5, its feature exists
In the lithium source is the one or more in lithium hydroxide, lithium carbonate, lithium acetate, lithium oxalate.
7. the preparation method of the high performance lithium ion battery positive electrode material lithium iron phosphate according to claim 1 or 6, its feature
It is, the carbon source is electrically conductive graphite, CNT, graphene, sucrose, glucose, fructose, citric acid, polyvinyl alcohol, poly- second
One or more in glycol, polyethers.
8. the preparation method of high performance lithium ion battery positive electrode material lithium iron phosphate according to claim 7, its feature exists
In the dispersant is trimethylolpropane, pentaerythrite, bipentaerythrite, lauryl sodium sulfate, dodecyl sodium sulfonate
Sodium, APES, dioctyl succinate disulfonate acid, Sucrose Fatty Acid Ester, fatty acid sorbitan, polysorbate, polyoxyethylene,
One or more in methyl anyl alcohol, cellulose derivative, fatty acid polyethylene glycol ester.
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Cited By (3)
Publication number | Priority date | Publication date | Assignee | Title |
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CN108408710A (en) * | 2018-04-25 | 2018-08-17 | 深圳市寒暑科技新能源有限公司 | A kind of energy conservation and environmental protection prepares the device and preparation method of LiFePO4 |
CN111430685A (en) * | 2020-01-19 | 2020-07-17 | 蜂巢能源科技有限公司 | Modified lithium iron phosphate material and preparation method and application thereof |
EP3754766A4 (en) * | 2018-02-14 | 2021-09-29 | Fujitsu Limited | Positive electrode material and manufacturing method therefor, battery using positive electrode material and manufacturing method therefor, and electronic equipment using battery |
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CN106698383A (en) * | 2017-01-20 | 2017-05-24 | 中天储能科技有限公司 | Method of preparing lithium iron phosphate material by using coconut fibers |
CN106784702A (en) * | 2016-12-27 | 2017-05-31 | 德清崎辉机械科技有限公司 | A kind of preparation method of high active material |
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CN102856545A (en) * | 2012-09-11 | 2013-01-02 | 清华大学 | Preparation method of micro-nano-grade metal-ion-doped lithium iron phosphate anode material |
CN104300119A (en) * | 2013-07-17 | 2015-01-21 | 东莞市长安东阳光铝业研发有限公司 | Preparation method for lithium iron phosphate cathode material |
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Cited By (4)
Publication number | Priority date | Publication date | Assignee | Title |
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EP3754766A4 (en) * | 2018-02-14 | 2021-09-29 | Fujitsu Limited | Positive electrode material and manufacturing method therefor, battery using positive electrode material and manufacturing method therefor, and electronic equipment using battery |
CN108408710A (en) * | 2018-04-25 | 2018-08-17 | 深圳市寒暑科技新能源有限公司 | A kind of energy conservation and environmental protection prepares the device and preparation method of LiFePO4 |
CN111430685A (en) * | 2020-01-19 | 2020-07-17 | 蜂巢能源科技有限公司 | Modified lithium iron phosphate material and preparation method and application thereof |
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