CN105576200A - Method for coating after molding of lithium iron phosphate - Google Patents
Method for coating after molding of lithium iron phosphate Download PDFInfo
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- CN105576200A CN105576200A CN201510941351.7A CN201510941351A CN105576200A CN 105576200 A CN105576200 A CN 105576200A CN 201510941351 A CN201510941351 A CN 201510941351A CN 105576200 A CN105576200 A CN 105576200A
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- lifepo4
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- lithium
- iron phosphate
- lithium iron
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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
- H01M4/366—Composites as layered products
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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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- 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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- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
- Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
- Y02E—REDUCTION OF GREENHOUSE GAS [GHG] EMISSIONS, RELATED TO ENERGY GENERATION, TRANSMISSION OR DISTRIBUTION
- Y02E60/00—Enabling technologies; Technologies with a potential or indirect contribution to GHG emissions mitigation
- Y02E60/10—Energy storage using batteries
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- Crystallography & Structural Chemistry (AREA)
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- Battery Electrode And Active Subsutance (AREA)
Abstract
The invention belongs to the technical field of new energy source powder and particularly relates to a method for coating after molding of lithium iron phosphate. The method comprises the following steps: mixing a lithium source, an iron source, ammonium metavanadate, a phosphorus source, sucrose and pure water to form paste; putting the paste into a stirring mill to be ground and mixed; then adding the pure water and grinding; drying and sintering; adding a carbon source and alcohol for ball milling to obtain mixed paste; and drying the mixed paste and sintering under the protection of inert gas to obtain the coated lithium iron phosphate. According to the method for coating after the molding of the lithium iron phosphate, provided by the invention, the coating effect of the lithium iron phosphate can guarantee sizes of grain diameters of the lithium iron phosphate, and a carbon coating layer is uniform. With the adoption of the method for coating after the molding of the lithium iron phosphate, when a prepared lithium iron phosphate positive electrode active material is used as a positive electrode material of a lithium battery, good machining properties are kept and electrochemical properties are good.
Description
Technical field
The invention belongs to new forms of energy powder technology field, particularly a kind of shaping rear coated method of LiFePO4.
Background technology
LiFePO4 (the LiFePO of olivine-type
4) because raw material is extensive, low price, environmental friendliness, as having the outstanding properties such as Heat stability is good, specific energy height during positive electrode, LiFePO 4 material is thought in the industry the positive electrode of lithium-ion-power cell best at present with its excellent specific property, is the developing direction of Vehicular battery.
There are high temperature solid-state method, hydro thermal method, coprecipitation and microwave heating method etc. in traditional LiFePO4 preparation side.But adopt high temperature solid-state method in the method for actual production LiFePO4 more.
The carbon source that the method for coating of the LiFePO4 of current main flow adopts is coating.The LiFePO4 excellent electrical property that carbon is coated, but common process causes carbon coating layer uneven.
For the weakness of prior art, the invention provides a kind of shaping rear coated method of LiFePO4, by first preparing LiFePO4, carrying out the LiFePO4 after shaping coatedly can ensureing the coated and excellent properties of uniform carbon.
Summary of the invention
Object of the present invention, is the shortcoming and defect overcoming said method, a kind of covered effect optimizing LiFePO4 provided by the invention, has the shaping rear coated method of LiFePO4 of uniform carbon coating layer while can ensureing LiFePO4 particle size.
Object of the present invention can be achieved through the following technical solutions:
The shaping rear coated method of LiFePO4, comprises the steps:
(1) by the lithium source in raw material, source of iron, ammonium metavanadate and phosphorus source, mol ratio by Li: Fe: V: P is (1-1.03): (0.9-1): (0.01-0.15): 1 mixes, and adding sucrose, described sucrose amount weighs by the phosphorus content 3-5wt% of raw material total amount.Add ammonium metavanadate, be conducive to the chemical property improving LiFePO4;
(2) by the raw material in step (1) and pure water in mass ratio 1:2-5 make mixed slurry, enter ground and mixed 1-3 hour in agitator mill; Preferably, raw material and pure water 1:3 in mass ratio, ground and mixed 2 hours, is conducive to raw material and fully disperses to improve grinding effect in slip;
(3) mixed slurry in step (2) is entered ultra-fine grinding mill and add pure water grinding 1-2 hour in the ratio of water material mass ratio 1:1-2 again;
(4) by the mixed slurry in step (3) at 200-400 DEG C of spraying dry, obtain ferric lithium phosphate precursor; At 200-400 DEG C of spraying dry, be conducive to slurry solution and be fully dried to presoma powder and can not Yin Wendu is too high makes sucrose excessive decomposition in presoma;
(5) ferric lithium phosphate precursor in step (4) is sintered under inert gas shielding, be warming up to 600 DEG C-800 DEG C, insulation 4-15 hour;
(6), after the sintering feed in step (5) being added the phosphorus content 3wt%-7wt% carbon source of raw material total amount, add alcohol in alcohol with the ratio of material mass ratio 1:1 and enter planetary ball mill, obtain mixed slurry; Due to carbon containing in alcohol, be therefore conducive to better carrying out the coated of LiFePO4; It is coated that the carbon added specifically is that secondary adds carbon, be conducive to supplementary once sintered time loss carbon provide carbon source for follow-up secondary carbon is coated simultaneously.
(7) mixed slurry in step (6) is carried out drying, obtain the coated presoma of LiFePO4;
(8) the coated presoma of LiFePO4 in step (7) is sintered under inert gas shielding, is warming up to 700 DEG C-900 DEG C, insulation 2-10 hour, obtain coated after LiFePO4.Current sintering is second time sintering, and being conducive to sucrose decomposition, to become carbon to carry out secondary coated.
In described step (1), source of iron is di-iron trioxide; Phosphorus source, lithium source are lithium dihydrogen phosphate and lithium carbonate.
The control of the particle diameter D50 in described step (2) after ground and mixed is at≤1.5 μm, and D90 controls at≤3 μm.
Intensification in described step (5), its programming rate is 2-10 DEG C/min.Be conducive to ensureing that material fully reacts in temperature-rise period.
Inert gas in described step (5) and step (8) is nitrogen.
In described step (5), the rear material carbon content control of sintering is at 0.5wt%-2wt%.
Carbon source in described step (6) is sucrose.
Intensification in described step (8), its programming rate is 2-10 DEG C/min.Be conducive to ensureing that material fully reacts in temperature-rise period.
The carbon content control of the LiFePO4 after coated in described step (8) is at 1.5wt% ~ 4wt%.
The covered effect of LiFePO4 provided by the invention, has the shaping rear coated method of LiFePO4 of uniform carbon coating layer while can ensureing LiFePO4 particle size.The shaping rear coated method of this LiFePO4, maintains processing characteristics good, the feature of excellent electrochemical performance when the lithium iron phosphate anode active material of preparation is used as anode material of lithium battery.
Accompanying drawing explanation
Fig. 1 is the flow chart for the shaping rear coated method of LiFePO4 of the present invention.
Embodiment
Below in conjunction with embodiment, the invention will be further described:
Embodiment 1
(1) weigh: by end product iron lithium phosphate material Li: Fe: V: P mol ratio be 1.02: 0.97: 0.03: 1 di-iron trioxide, lithium dihydrogen phosphate, lithium carbonate, ammonium metavanadate are carried out proportioning weighing, sucrose then weighs by phosphorus content 4wt%.
(2) prepare the coated presoma of LiFePO4: by load weighted raw material and pure water in mass ratio 1:3 make mixed slurry, to enter in agitator mill ground and mixed 2 hours; Mixed slurry is entered ultra-fine grinding mill to add pure water in the ratio of water material mass ratio 1:1 again and grind 1 hour; Then spraying dry, air-out 220 DEG C, air intake 330 DEG C, obtains ferric lithium phosphate precursor; Sinter under nitrogen protection, through with 3 DEG C/min, be warming up to 700 DEG C, be incubated 10 hours; After adding the phosphorus content 3wt% sucrose of raw material total amount, add alcohol in alcohol with the ratio of material mass ratio 1:1 and enter planetary ball mill, obtain mixed slurry; After oven for drying drying, obtain the coated presoma of LiFePO4.
(3) prepare coated LiFePO 4 for lithium ion batteries: sinter under nitrogen protection, be warming up to 700 DEG C with 3 DEG C/min, be incubated 6 hours, after sintering, carbon content is 1.94wt%.
Above-mentioned obtained LiFePO 4 material is tested, obtains following performance:
Button cell 0.1C first discharge specific capacity is 151.5mAh/g; 1C first discharge specific capacity is 133.3mAh/g;
LiFePO 4 material D50 particle diameter is 2.493 μm, D90 particle diameter is 4.939 μm.
Embodiment 2
(1) weigh: by end product iron lithium phosphate material Li: Fe: V: P mol ratio be 1.02: 0.97: 0.03: 1 di-iron trioxide, lithium dihydrogen phosphate, lithium carbonate, ammonium metavanadate are carried out proportioning weighing, sucrose then weighs by phosphorus content 4wt%.
(2) the coated presoma of LiFePO4 is prepared: preparation method is with embodiment 1, and only adding carbon source ratio difference, is 7wt%.
(3) coated LiFePO 4 for lithium ion batteries is prepared: preparation method is with embodiment 1, and only after sintering, carbon content ratio is different, is 3.92wt%.
Above-mentioned obtained LiFePO 4 material is tested, obtains following performance:
Button cell 0.1C first discharge specific capacity is 130.1mAh/g; 1C first discharge specific capacity is 126.8mAh/g;
LiFePO 4 material D50 particle diameter is 3.102 μm, D90 particle diameter is 14.894 μm.
Embodiment 3
(1) weigh: by end product iron lithium phosphate material Li: Fe: V: P mol ratio be 1.02: 0.97: 0.03: 1 di-iron trioxide, lithium dihydrogen phosphate, lithium carbonate, ammonium metavanadate are carried out proportioning weighing, sucrose then weighs by phosphorus content 4wt%.
(2) the coated presoma of LiFePO4 is prepared: preparation method, with embodiment 1, only adds carbon source ratio and to rise to temperature different, and carbon source ratio is 7wt% and is warming up to 800 DEG C.
(3) coated LiFePO 4 for lithium ion batteries is prepared: preparation method is with embodiment 1, and only rise to temperature different with carbon content ratio after sintering, rise to temperature to 800 DEG C, carbon content is 2.48wt%.
Above-mentioned obtained LiFePO 4 material is tested, obtains following performance:
Button cell 0.1C first discharge specific capacity is 148.1mAh/g; 1C first discharge specific capacity is 124.7mAh/g;
LiFePO 4 material D50 particle diameter is 2.846 μm, D90 particle diameter is 8.331 μm.
The above is preferred embodiment of the present invention, but the present invention should not be confined to the content disclosed in this embodiment.The equivalence completed under not departing from spirit disclosed in this invention so every or amendment, all fall into the scope of protection of the invention.
Claims (9)
1. the shaping rear coated method of LiFePO4, comprises the steps:
(1) by the lithium source in raw material, source of iron, ammonium metavanadate, phosphorus source, mol ratio by Li: Fe: V: P is to mix at 1-1.03: 0.9-1: 0.01-0.15: 1, and adding sucrose, described sucrose amount weighs by the phosphorus content 3-5wt% of raw material total amount;
(2) by the raw material in step (1) and pure water in mass ratio 1:2-5 make mixed slurry, enter ground and mixed 1-3 hour in agitator mill;
(3) mixed slurry in step (2) is entered ultra-fine grinding mill and add pure water grinding 1-2 hour in the ratio of water material mass ratio 1:1-2 again;
(4) by the mixed slurry in step (3) at 200-400 DEG C of spraying dry, obtain ferric lithium phosphate precursor;
(5) ferric lithium phosphate precursor in step (4) is sintered under inert gas shielding, be warming up to 600 DEG C-800 DEG C, insulation 4-15 hour;
(6), after the sintering feed in step (5) being added the phosphorus content 3wt%-7wt% carbon source of raw material total amount, add alcohol in alcohol with the ratio of material mass ratio 1:1-2 and enter planetary ball mill, obtain mixed slurry;
(7) mixed slurry in step (6) is carried out drying, obtain the coated presoma of LiFePO4;
(8) the coated presoma of LiFePO4 in step (7) is sintered under inert gas shielding, is warming up to 700 DEG C-900 DEG C, insulation 2-10 hour, obtain coated after LiFePO4.
2. the shaping rear coated method of LiFePO4 as claimed in claim 1, is characterized in that: in described step (1), source of iron is di-iron trioxide; Phosphorus source, lithium source are lithium dihydrogen phosphate and lithium carbonate.
3. the shaping rear coated method of LiFePO4 as claimed in claim 1, is characterized in that: the control of the particle diameter D50 in described step (2) after ground and mixed is at≤1.5 μm, and D90 controls at≤3 μm.
4. the shaping rear coated method of LiFePO4 as claimed in claim 1, it is characterized in that: the intensification in described step (5), its programming rate is 2-10 DEG C/min.
5. the shaping rear coated method of LiFePO4 as claimed in claim 1, is characterized in that: the inert gas in described step (5) and step (8) is nitrogen.
6. the shaping rear coated method of LiFePO4 as claimed in claim 1, is characterized in that: in described step (5), the rear material carbon content control of sintering is at 0.5wt%-2wt%.
7. the shaping rear coated method of LiFePO4 as claimed in claim 1, is characterized in that: the carbon source in described step (6) is sucrose.
8. the shaping rear coated method of LiFePO4 as claimed in claim 1, it is characterized in that: the intensification in described step (8), its programming rate is 2-10 DEG C/min.
9. the shaping rear coated method of LiFePO4 as claimed in claim 1, is characterized in that: the carbon content control of the LiFePO4 after coated in described step (8) is at 1.5wt% ~ 4wt%.
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Cited By (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN106920946A (en) * | 2017-04-15 | 2017-07-04 | 三峡大学 | A kind of preparation method of aluminum oxide and carbon compound coating fluorophosphoric acid vanadium sodium positive electrode |
| CN107634205A (en) * | 2017-09-12 | 2018-01-26 | 合肥国轩高科动力能源有限公司 | A kind of preparation method of lithium iron phosphate positive material |
| CN109888260A (en) * | 2019-04-09 | 2019-06-14 | 上海卡耐新能源有限公司 | A kind of modification method for preparing and modified material of lithium iron phosphate positive material |
| CN110957491A (en) * | 2019-12-24 | 2020-04-03 | 广东石油化工学院 | Preparation method of fluoride ion-doped lithium iron phosphate material |
| CN114050259A (en) * | 2021-12-08 | 2022-02-15 | 程冲 | Preparation of single crystal high compaction lithium iron phosphate by primary reduction shaping secondary liquid phase coating method |
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| CN101844756A (en) * | 2009-03-25 | 2010-09-29 | 宝山钢铁股份有限公司 | Method for preparing lithium iron phosphate by using steel slag |
| CN103427072A (en) * | 2012-05-16 | 2013-12-04 | 上海宝钢磁业有限公司 | In-situ carbon coating method for lithium iron phosphate |
| CN104269553A (en) * | 2014-09-23 | 2015-01-07 | 上海宝钢磁业有限公司 | Method for preparing lithium iron phosphate material by adopting cold-rolled byproduct iron oxide |
| CN104409732A (en) * | 2014-12-11 | 2015-03-11 | 上海宝钢磁业有限公司 | Preparation method for lithium iron phosphate material by adopting mixed iron source |
-
2015
- 2015-12-15 CN CN201510941351.7A patent/CN105576200A/en active Pending
Patent Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN101844756A (en) * | 2009-03-25 | 2010-09-29 | 宝山钢铁股份有限公司 | Method for preparing lithium iron phosphate by using steel slag |
| CN103427072A (en) * | 2012-05-16 | 2013-12-04 | 上海宝钢磁业有限公司 | In-situ carbon coating method for lithium iron phosphate |
| CN104269553A (en) * | 2014-09-23 | 2015-01-07 | 上海宝钢磁业有限公司 | Method for preparing lithium iron phosphate material by adopting cold-rolled byproduct iron oxide |
| CN104409732A (en) * | 2014-12-11 | 2015-03-11 | 上海宝钢磁业有限公司 | Preparation method for lithium iron phosphate material by adopting mixed iron source |
Cited By (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN106920946A (en) * | 2017-04-15 | 2017-07-04 | 三峡大学 | A kind of preparation method of aluminum oxide and carbon compound coating fluorophosphoric acid vanadium sodium positive electrode |
| CN106920946B (en) * | 2017-04-15 | 2020-11-06 | 三峡大学 | Preparation method of aluminum oxide and carbon composite coated sodium vanadium fluorophosphate cathode material |
| CN107634205A (en) * | 2017-09-12 | 2018-01-26 | 合肥国轩高科动力能源有限公司 | A kind of preparation method of lithium iron phosphate positive material |
| CN109888260A (en) * | 2019-04-09 | 2019-06-14 | 上海卡耐新能源有限公司 | A kind of modification method for preparing and modified material of lithium iron phosphate positive material |
| CN110957491A (en) * | 2019-12-24 | 2020-04-03 | 广东石油化工学院 | Preparation method of fluoride ion-doped lithium iron phosphate material |
| CN114050259A (en) * | 2021-12-08 | 2022-02-15 | 程冲 | Preparation of single crystal high compaction lithium iron phosphate by primary reduction shaping secondary liquid phase coating method |
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Application publication date: 20160511 |