CN104752692A - Preparation method for LiFePO4/C composite anode material - Google Patents
Preparation method for LiFePO4/C composite anode material Download PDFInfo
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- CN104752692A CN104752692A CN201310743761.1A CN201310743761A CN104752692A CN 104752692 A CN104752692 A CN 104752692A CN 201310743761 A CN201310743761 A CN 201310743761A CN 104752692 A CN104752692 A CN 104752692A
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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
- H01M4/362—Composites
- H01M4/364—Composites as mixtures
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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
- 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
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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
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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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Abstract
The invention discloses a preparation method for an LiFePO4/C composite anode material. The method includes the steps of: (1) mixing: weighing the raw material iron phosphate or its hydrate and a lithium source compound according to an Li/Fe mole ratio of 1-1.06: 1, adding a carbon source and conducting mixing, then adding a ball milling medium to conduct ball milling for 1-10h so as to obtain a precursor slurry; (2) drying: conducting drying by a high speed air blowing electrostatic spray drying technology, separating an air channel from a slurry channel by internal and external casing pipes, erupting high speed air flow from the external casing pipe, and ejecting the slurry obtained in step (1) from the central internal pipe to form particles or fiber, thus obtaining a precursor; and (3) heat treatment: conducting high temperature heat treatment for 2-16h on the precursor under inert atmosphere protection, and then performing cooling to room temperature under inert atmosphere, thus obtaining the LiFePO4/C composite anode material. The method provided by the invention applies the high speed air blowing electrostatic spray drying technology, ca significantly lower the inlet temperature of dry gas, reduce energy consumption, improve drying efficiency and reduce production cost, and at the same time maintains the excellent electrical properties of the LiFePO4/C anode material.
Description
Technical field
The present invention relates to a kind of preparation method of ferrous phosphate lithium/carbon composite positive pole, belong to electrochemical energy field of material technology.
Background technology
Lithium ion battery is a kind of range of application high-efficiency energy-storage device very widely, and its development trend is the future development towards more high-energy-density, overlength cycle life and high security.LiFePO 4, as one of the positive electrode of lithium ion battery, is the positive electrode be widely used at present, particularly enjoys industrial circle to pay close attention to because of the cycle life of its overlength and outstanding fail safe and lower production cost.
The production technology of current LiFePO 4 is mainly high temperature solid-state method, hydro thermal method and sol-gel process etc., and this several method respectively has pluses and minuses, and hydro thermal method has the advantage of controlled prepared material grain diameter, but industrial installation is complicated, industrial production difficulty; Sol-gel method craft is complicated, and production cost is higher; Mainly grain diameter is comparatively large at present for solid phase method, and be difficult to control, in spray-drying process, energy consumption is comparatively large, is therefore necessary to develop new dry technology, reduces the production cost of LiFePO 4, be beneficial to applying of LiFePO 4.
High-voltage electrostatic spraying technology is novel dried technology extensively concerned in the last few years, its equipment mainly comprise charging pump, high-voltage DC power supply, nozzle and gatherer four part composition, in dry run, voltage is applied at nozzle place, its operation principle is that charged drop or jet are under electrostatic repulsion, electrostatic field force and surface tension acting in conjunction, extremely fast move from a pole to another, solvent/evaporate in motion process, can realize the quick continuous drying of suspension.
Summary of the invention
The object of the present invention is to provide a kind of preparation method possessing excellent electrical ferrous phosphate lithium/carbon composite positive pole.In solid-phase ball milling preparation process, adopt more efficient dry technology to carry out drying to slurry, greatly improve spray-drying efficiency, improve production capacity, reduce energy consumption, thus reduce material cost.
For achieving the above object, the present invention is by the following technical solutions:
A preparation method for ferrous phosphate lithium/carbon composite positive pole, comprises the following steps:
(1) batch mixing: be take raw material ferric phosphate or its hydrate and Li source compound at 1 ~ 1.06: 1 by Li/Fe mol ratio, adds carbon source mixing, then adds ball-milling medium ball milling 1 ~ 10 hour, obtain precursor pulp;
(2) dry: application high-speed air-blowing electrostatic spray dry technology carries out drying, internal and external casing separates gas circuit and slurry passage, high velocity air sprays from outer tube, and the slurry that step (1) obtains therefrom intracardiac pipe inspection goes out, and forms droplet or stable high-speed jet; Drop or jet are from a pole in the process of another polar motion, and ball-milling medium volatilizees, and drop or jet solidification, form particle or fiber, obtain presoma;
(3) heat treatment: presoma step (2) obtained high-temperature heat treatment 2 ~ 16 hours under inert atmosphere protection, products therefrom is cooled to room temperature under an inert atmosphere, obtains ferrous phosphate lithium/carbon composite positive pole.
In the method, LiOH, Li can be selected as Li source compound
2cO
3or the mixture of the two.
In the method, the mixture of one or more in glucose, sucrose, fructose, cyclodextrin, polyethylene glycol (PEG), polyvinyl alcohol (PVA), PVP (PVP) and polyvinyl butyral resin (PVB) can be selected as carbon-source cpd.Preferred glucose, sucrose is considered from cost of material.According to the requirement to pattern, the mixture of appropriate polymer as the one or more than one in polyethylene glycol, polyvinyl alcohol, PVP (PVP), polyvinyl butyral resin (PVB) can be added, the total consumption of carbon source controls at 4% ~ 20% of all material qualities (comprising ferric phosphate, Li source compound and carbon source), is preferably 6% ~ 15%.
In the method, described ball-milling medium is one or both the mixture in deionized water and ethanol, and its addition is 2 ~ 5 times of solid gross mass.
In described step (2), what apply is high-speed air-blowing electrostatic spray dry technology, on the basis of high-voltage electrostatic spraying technology, adopt internal and external casing that gas circuit and slurry passage are separated, high velocity air sprays from outer tube, slurry under the acting in conjunction of mechanical thrust, high velocity air " siphon " and high voltage electric field actuating force therefrom intracardiac pipe inspection go out, form droplet or stable high-speed jet.The drop formed or stable high-speed jet are from a pole in the process of another polar motion, and solvent evaporates, drop or jet solidification, form particle or fiber.Electric field strength used in this technology is 30 ~ 100KV/m, and voltage is the direct voltage of 15 ~ 100KV; The flow velocity of gas is 50 ~ 400m/s, and the temperature of gas is 60 ~ 240 DEG C, is preferably 60 ~ 180 DEG C; The slurry consumption of the single shower nozzle of central inner pipe is 0.1 ~ 50mL/min.
When to form the ball-milling medium of slurry be water, adopt that high-speed air-blowing electrostatic spray dry technology dry gas temperature is minimum can be 80 DEG C, and adopt the spray-dired gas temperature of traditional two-fluid will more than 140 DEG C; When to form the ball-milling medium of slurry be ethanol, adopt that high-speed air-blowing electrostatic spray dry technology dry gas temperature is minimum can be down to 60 DEG C, and adopt the spray-dired gas temperature of traditional two-fluid will more than 80 DEG C.Therefore, high-speed air-blowing electrostatic spray dry technology is adopted greatly can to reduce energy consumption.
The invention has the advantages that:
The present invention applies the inlet temperature that high-speed air-blowing electrostatic spray dry technology significantly can reduce dry gas in solid-phase ball milling preparation technology, reduce energy consumption, improve drying efficiency, reduce production cost, keep ferrous phosphate lithium/carbon composite positive pole (LiFePO simultaneously
4/ C positive electrode material) excellent electrical property.
Present invention process process is simple, practical.
Accompanying drawing explanation
Fig. 1 is the LiFePO of embodiment 1 gained
4the XRD diffraction pattern of/C positive electrode material.
Fig. 2 is the LiFePO of embodiment 1 gained
4the charging and discharging curve of/C positive electrode material.
Fig. 3 is the LiFePO of embodiment 2 gained
4the transmission electron microscope photo of/C positive electrode material.
Embodiment
The invention will be further described by the following examples, but the present invention is not limited to following examples.
Embodiment 1
Take LITHIUM BATTERY Li
2cO
3, ferric phosphate, mol ratio is 1: 1, add sucrose mixing, the addition of sucrose is 10% of mixture gross mass, take deionized water as abrasive media, its addition is 4 times of solid gross mass, grinds 1 hour, the slurry application high-speed air-blowing electrostatic spray seasoning of gained is dry, and voltage is 15KV; Electric field strength controls at 30KV/m, and spout gas flow rate is at 50m/s; The slurry consumption of single spraying head is at 0.1mL/min, and gas temperature, at 100 DEG C, obtains presoma, presoma is placed in the pit-type furnace roasting under argon gas atmosphere, and programming rate is 2 DEG C/min, and 650 DEG C of insulation 16h, obtain LiFePO
4/ C positive electrode material, as shown in Figure 1, XRD test is pure phase olivine-type LiFePO
4.Be to electrode with lithium metal, assembly simulation half-cell test electrical property, as shown in Figure 2, under 0.1C, its specific discharge capacity is 159mAh/g.
Embodiment 2
Take LITHIUM BATTERY LiOHH
2o, ferric phosphate, mol ratio is 1: 1.06, add glucose mixing, the addition of glucose is 20% of mixture gross mass, with deionized water and alcohol mixeding liquid (both mass ratioes are for 1: 1) for abrasive media, its addition is 5 times of solid gross mass, grinds 10 hours, the slurry application high-speed air-blowing electrostatic spray seasoning of gained is dry, and voltage is 100KV; Electric field strength controls at 100KV/m, and spout gas flow rate is at 400m/s; The slurry consumption of single spraying head is at 50mL/min, and gas temperature, at 180 DEG C, obtains presoma, presoma is placed in the pit-type furnace roasting under argon gas atmosphere, and programming rate is 10 DEG C/min, and 800 DEG C of insulation 2h, obtain LiFePO
4/ C positive electrode material, Fig. 3 transmission electron microscope photo display carbon is coated comparatively even, and under 0.1C, its specific discharge capacity is 157mAh/g.
Embodiment 3
Take LITHIUM BATTERY Li
2cO
3, ferric phosphate, mol ratio is 1: 1.06, add PVP (PVP) mixing, the addition of PVP is 4% of mixture gross mass, take absolute ethyl alcohol as abrasive media, its addition is 4 times of solid gross mass, grinds 4 hours, the slurry application high-speed air-blowing electrostatic spray seasoning of gained is dry, and voltage is 50KV; Electric field strength controls at 50KV/m, and spout gas flow rate is at 300m/s; The slurry consumption of single spraying head is at 10mL/min, and gas temperature, at 60 DEG C, obtains presoma, presoma is placed in the pit-type furnace roasting under argon gas atmosphere, and programming rate is 5 DEG C/min, and 700 DEG C of insulation 5h, obtain LiFePO
4/ C positive electrode material, under 0.1C, its specific discharge capacity is 161mAh/g.
Embodiment 4
Take LITHIUM BATTERY LiOHH
2o, ferric phosphate, mol ratio is 1: 1.04, add PVP and sucrose (the two mass ratio is 1: 1) mixing, add that total amount is mixture gross mass 10% of PVP and sucrose, take deionized water as abrasive media, its addition is 5 times of solid gross mass, grinds 5 hours, the slurry application high-speed air-blowing electrostatic spray seasoning of gained is dry, and voltage is 50KV; Electric field strength controls at 50KV/m, and spout gas flow rate is at 200m/s; The slurry consumption of single spraying head is at 10mL/min, and gas temperature, at 160 DEG C, obtains presoma, presoma is placed in the pit-type furnace roasting under argon gas atmosphere, and programming rate is 5 DEG C/min, and 650 DEG C of insulation 5h, obtain LiFePO
4/ C positive electrode material, under 0.1C, its specific discharge capacity is that under 162mAh/g, 5C, specific discharge capacity is 130mAh/g.
Embodiment 5
Take LITHIUM BATTERY LiOHH
2o, ferric phosphate, mol ratio is 1: 1.04, add polyethylene glycol and sucrose (the two mass ratio is 1: 1) mixing, add that total amount is mixture gross mass 18% of polyethylene glycol and sucrose, take deionized water as abrasive media, its addition is 5 times of solid gross mass, grinds 5 hours, the slurry application high-speed air-blowing electrostatic spray seasoning of gained is dry, and voltage is 50KV; Electric field strength controls at 50KV/m, and spout gas flow rate is at 200m/s; The slurry consumption of single spraying head is at 10mL/min, and gas temperature, at 100 DEG C, obtains presoma, presoma is placed in the pit-type furnace roasting under nitrogen atmosphere, and programming rate is 5 DEG C/min, and 650 DEG C of insulation 5h, obtain LiFePO
4/ C positive electrode material, under 0.1C, its specific discharge capacity is that under 160mAh/g, 5C, specific discharge capacity is 128mAh/g.
Embodiment 6
Take LITHIUM BATTERY LiOHH
2o, ferric phosphate, mol ratio is 1: 1.03, add PVP and polyethylene glycol (the two mass ratio is 1: 1) mixing, add that total amount is mixture gross mass 12% of PVP and polyethylene glycol, take deionized water as abrasive media, its addition is 5 times of solid gross mass, grinds 5 hours, the slurry application high-speed air-blowing electrostatic spray seasoning of gained is dry, and voltage is 50KV; Electric field strength controls at 50KV/m, and spout gas flow rate is at 200m/s; The slurry consumption of single spraying head is at 10mL/min, and gas temperature, at 160 DEG C, obtains presoma, and presoma is placed in the pit-type furnace roasting under argon gas and nitrogen (volume ratio 1: 1) atmosphere, programming rate is 5 DEG C/min, and 650 DEG C of insulation 5h, obtain LiFePO
4/ C positive electrode material, under 0.1C, its specific discharge capacity is that under 163mAh/g, 5C, specific discharge capacity is 132mAh/g.
Embodiment 7
Take LITHIUM BATTERY Li
2cO
3, ferric phosphate, mol ratio is 1: 1, add sucrose mixing, the addition of sucrose is 4% of mixture gross mass, take deionized water as abrasive media, and its addition is 3 times of solid gross mass, grind 10 hours, the slurry application high-speed air-blowing electrostatic spray seasoning of gained is dry, voltage 15KV; Electric field strength controls at 30KV/m, and spout gas flow rate is at 50m/s; The slurry consumption of single spraying head is at 4mL/min, and gas temperature, at 100 DEG C, obtains presoma, presoma is placed in the pit-type furnace roasting under argon gas atmosphere, and programming rate is 2 DEG C/min, and 650 DEG C of insulation 16h, obtain LiFePO
4/ C positive electrode material, under 0.1C, its specific discharge capacity is that under 160.5mAh/g, 5C, specific discharge capacity is 131mAh/g.
Claims (9)
1. a preparation method for ferrous phosphate lithium/carbon composite positive pole, is characterized in that, comprises the following steps:
(1) batch mixing: be take raw material ferric phosphate or its hydrate and Li source compound at 1 ~ 1.06: 1 by Li/Fe mol ratio, adds carbon source mixing, then adds ball-milling medium ball milling and obtain precursor pulp in 1 ~ 10 hour;
(2) dry: application high-speed air-blowing electrostatic spray dry technology carries out drying, internal and external casing separates gas circuit and slurry passage, high velocity air sprays from outer tube, and the slurry that step (1) obtains therefrom intracardiac pipe inspection goes out, and forms droplet or stable high-speed jet; Drop or jet are from a pole in the process of another polar motion, and ball-milling medium volatilizees, and drop or jet solidification, form particle or fiber, obtain presoma;
(3) heat treatment: presoma step (2) obtained high-temperature heat treatment 2 ~ 16 hours under inert atmosphere protection, products therefrom is cooled to room temperature under an inert atmosphere, obtains ferrous phosphate lithium/carbon composite positive pole.
2. the preparation method of ferrous phosphate lithium/carbon composite positive pole according to claim 1, is characterized in that, described Li source compound is LiOH, Li
2cO
3in one or both.
3. the preparation method of ferrous phosphate lithium/carbon composite positive pole according to claim 1, is characterized in that, the addition of described carbon source is 4 ~ 20% of ferric phosphate, Li source compound and carbon source gross mass.
4. the preparation method of ferrous phosphate lithium/carbon composite positive pole according to claim 1, it is characterized in that, described carbon-source cpd is one or more in glucose, sucrose, fructose, cyclodextrin, polyethylene glycol, polyvinyl alcohol, PVP and polyvinyl butyral resin.
5. the preparation method of ferrous phosphate lithium/carbon composite positive pole according to claim 1, is characterized in that, described ball-milling medium is one or both the mixture in deionized water and ethanol, and its addition is 2 ~ 5 times of solid gross mass.
6. the preparation method of ferrous phosphate lithium/carbon composite positive pole according to claim 1, is characterized in that, electric field strength used in described step (2) is 30 ~ 100KV/m, and voltage is the direct voltage of 15 ~ 100KV.
7. the preparation method of ferrous phosphate lithium/carbon composite positive pole according to claim 1, is characterized in that, flow velocity gases used in described step (2) is 50 ~ 400m/s.
8. the preparation method of the ferrous phosphate lithium/carbon composite positive pole according to claim 1 or 7, is characterized in that, temperature gases used in described step (2) is 60 ~ 240 DEG C.
9. the preparation method of ferrous phosphate lithium/carbon composite positive pole according to claim 1, is characterized in that, in described step (2), the slurry consumption of the single shower nozzle of central inner pipe used is 0.1 ~ 50mL/min.
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Cited By (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN108899513A (en) * | 2018-07-03 | 2018-11-27 | 江苏乐能电池股份有限公司 | A kind of preparation method of the trielement composite material containing organic salt |
| WO2019043401A1 (en) * | 2017-09-04 | 2019-03-07 | Johnson Matthey Public Limited Company | Process for producing particulate carbon-coated lithium iron phosphate, carbon coated lithium iron phosphate and its uses |
| WO2019043403A1 (en) * | 2017-09-04 | 2019-03-07 | Johnson Matthey Public Limited Company | Process for producing particulate carbon-coated lithium iron phosphate, carbon coated lithium iron phosphate and its uses |
| WO2019043402A1 (en) * | 2017-09-04 | 2019-03-07 | Johnson Matthey Public Limited Company | Process for producing particulate carbon-coated lithium iron phosphate, carbon coated lithium iron phosphate and its uses |
| CN111682202A (en) * | 2019-09-02 | 2020-09-18 | 重庆特瑞电池材料股份有限公司 | Method for synthesizing rodlike lithium iron phosphate by PVA (polyvinyl alcohol) -assisted two-fluid spraying solid phase |
| CN112978790A (en) * | 2021-02-26 | 2021-06-18 | 海南大学 | Preparation method of lithium titanate with electrochemical oscillation effect |
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Cited By (8)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| WO2019043401A1 (en) * | 2017-09-04 | 2019-03-07 | Johnson Matthey Public Limited Company | Process for producing particulate carbon-coated lithium iron phosphate, carbon coated lithium iron phosphate and its uses |
| WO2019043403A1 (en) * | 2017-09-04 | 2019-03-07 | Johnson Matthey Public Limited Company | Process for producing particulate carbon-coated lithium iron phosphate, carbon coated lithium iron phosphate and its uses |
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| CN111682202A (en) * | 2019-09-02 | 2020-09-18 | 重庆特瑞电池材料股份有限公司 | Method for synthesizing rodlike lithium iron phosphate by PVA (polyvinyl alcohol) -assisted two-fluid spraying solid phase |
| CN111682202B (en) * | 2019-09-02 | 2022-12-27 | 重庆特瑞电池材料股份有限公司 | Method for synthesizing rodlike lithium iron phosphate by PVA (polyvinyl alcohol) -assisted two-fluid spraying solid phase |
| CN112978790A (en) * | 2021-02-26 | 2021-06-18 | 海南大学 | Preparation method of lithium titanate with electrochemical oscillation effect |
| CN112978790B (en) * | 2021-02-26 | 2022-05-17 | 海南大学 | Preparation method of lithium titanate with electrochemical oscillation effect |
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