CN106904588A - A kind of lithium ion battery with high energy density positive electrode and preparation method thereof - Google Patents
A kind of lithium ion battery with high energy density positive electrode and preparation method thereof Download PDFInfo
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- CN106904588A CN106904588A CN201710172806.2A CN201710172806A CN106904588A CN 106904588 A CN106904588 A CN 106904588A CN 201710172806 A CN201710172806 A CN 201710172806A CN 106904588 A CN106904588 A CN 106904588A
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- positive electrode
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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
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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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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2006/00—Physical properties of inorganic compounds
- C01P2006/40—Electric properties
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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
- H01M2004/026—Electrodes composed of, or comprising, active material characterised by the polarity
- H01M2004/028—Positive electrodes
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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 present invention relates to anode material for lithium-ion batteries, a kind of lithium ion battery with high energy density positive electrode and preparation method thereof is related in particular to, belong to power battery technology field.The present invention provides one kind by formula LiMn1‑xFexPO4The lithium ion battery with high energy density positive electrode of expression, in formula, 0.5≤X ＜ 1.The present invention also provides a kind of preparation method of above-mentioned positive electrode, and the positive electrode of preparation has the advantages that preferable electric conductivity, energy density is high, gram volume is big；And process is simple, low cost, efficiency high, safety and environmental protection, it is adapted to large-scale production.
Description
Technical field
The present invention relates to anode material for lithium-ion batteries, a kind of lithium ion battery with high energy density positive pole is related in particular to
Material and preparation method thereof, belongs to power battery technology field.
Background technology
With the quick consumption of the fossil fuels such as oil, coal and incident serious greenhouse effects and environment dirt
Dye, the demand of regenerative resource of the people for cleaning is also growing day by day.Lithium rechargeable battery belongs to clean energy resource field, tool
There is security good, good cycle has extended cycle life, the features such as nontoxic, be hopeful to be used as large-sized power power supply and big
Type accumulation power supply.
Lithium ion battery as a kind of environmental protection high-performance secondary cell, with energy density it is high, it is average output electricity
Pressure height, output power, self discharge is small, efficiency for charge-discharge is high, memory-less effect the advantages of, various portable type electronic products,
More and more applied in communication tool, electric automobile and hybrid vehicle.Lithium ion battery since the commercialization,
The research of positive electrode is the focus of the area research all the time.The positive electrode of lithium ion battery mainly have cobalt acid lithium, LiMn2O4,
Lithium nickelate, ternary material, LiFePO4 etc..Wherein LiFePO4 have it is nontoxic, pollution-free, have a safety feature, raw material sources
Extensively, it is cheap, the advantages of long lifespan, become the preferable positive electrode of lithium ion battery of new generation.Synthesizing iron lithium phosphate
Common method have high temperature solid-state method, sol-gel process and hydro-thermal method etc..Though this several method respectively has advantage, one is there is also
A little obvious defects.Such as, the particle diameter of high temperature solid-state method synthesizing iron lithium phosphate particle is larger, and charge-discharge performance is not ideal；Colloidal sol-
The technique of gel method is relative complex, and production cost is higher；Though hydro-thermal method can control particle diameter, industrial difficulty is larger.Separately
On the one hand, LiFePO4 poorly conductive in itself, lithium ion diffusion is slow when causing battery high power charging-discharging, and compacted density is small, energy
Metric density is low, and gram volume is small, and charge rate is slow, and the shortcomings of endurance is short, these shortcomings also counteracts that LiFePO 4 material
Using.
Therefore, it is quite necessary to develop new composite ferric lithium phosphate material and its technology of preparing to improve the comprehensive of LiFePO4
Performance is closed, promotes its heavy industrialization application.
The content of the invention
In view of the shortcomings of the prior art, present invention solves the technical problem that being to provide a kind of high energy density lithium ion electricity
Pond positive electrode and preparation method thereof, the preparation that the present invention is provided positive electrode cost is relatively low, the feature of environmental protection preferably, with preferable
Electric conductivity, the advantages of energy density is high, gram volume is big.
To realize the purpose of the present invention, the present invention is adopted the following technical scheme that：
A kind of lithium ion battery with high energy density positive electrode, uses formula LiMn1-xFexPO4Represent, wherein 0.5≤X ＜ 1.
Further, in above-mentioned cell positive material, the formula, 0.5≤X≤0.9.
A kind of preparation method of lithium ion battery with high energy density positive electrode, specifically includes following steps：
(1) with LiMn1-xFexPO4Proportioning weigh water-soluble lithium source compound, water-soluble iron source compound, water-soluble manganese
Source compound, P source compound and carbon source material, wherein 0.5≤X≤0.9, adds deionized water mixing wiring solution-forming, spraying is dry
The dry solution obtains mixture；
(2) mixture that step (1) is obtained is sintered：220~260 DEG C pre-oxidize 2~3h in atmosphere, in N2Atmosphere
Under enclosing, with 2~10 DEG C of min-1Speed be warming up to 800~1000 DEG C and keep 5~8h, in N2Room is naturally cooled under atmosphere
Temperature, obtains lithium ion battery with high energy density positive electrode.
Further, above-mentioned Li source compound is lithium acetate, the one kind in lithium nitrate, lithium hydroxide, lithium carbonate.
Further, above-mentioned Fe source compound is the one kind in ferrous nitrate, ferrous acetate, ferrous sulfate.
Further, above-mentioned manganese source compound is the one kind in manganese acetate, manganese nitrate, manganese chloride, manganese sulfate.
Further, above-mentioned P source compound is the one kind in phosphoric acid, ammonium dihydrogen phosphate, diammonium hydrogen phosphate.
Further, above-mentioned carbon source material is in sucrose, glucose, citric acid, polyvinyl alcohol, polyvinylpyrrolidone
It is a kind of.
Further, above-mentioned water-soluble lithium source compound is 1 with the mol ratio of carbon source material: (1~1.5).
Further, in the lithium ion battery with high energy density positive electrode for being obtained after above-mentioned sintering phosphorus content be 2~
8%.
The device have the advantages that：
(1) a kind of lithium ion battery with high energy density positive electrode of the invention and preparation method thereof, by ferric phosphate
Adulterate appropriate manganese in lithium material lattice, by the energy density for improving the average voltage of material to lift material.
(2) a kind of lithium ion battery with high energy density positive electrode of the invention and preparation method thereof, in heat treatment process
In, precise control material particle size and phosphorus content, the further gram volume of lifting material.
(3) a kind of lithium ion battery with high energy density positive electrode of the invention and preparation method thereof, process is simple, cost
Low, efficiency high, safety and environmental protection is adapted to large-scale production.
Specific embodiment
Presently in connection with embodiment, the present invention is further detailed explanation.
Embodiment 1
A kind of lithium ion battery with high energy density positive electrode, its formula is LiMn0.5Fe0.5PO4Represent.
A kind of lithium ion battery with high energy density positive electrode LiMn0.5Fe0.5PO4Preparation method, specifically include as follows
Step：
(1) it is 1 by mol ratio with water-soluble lithium source compound as measurement unit:0.5:0.5:1:1 weigh lithium acetate,
Ferrous nitrate, manganese acetate, phosphoric acid and sucrose, add deionized water mixing wiring solution-forming, are spray-dried the solution and are mixed
Thing；
(2) mixture that step (1) is obtained is sintered：220 DEG C pre-oxidize 3h in atmosphere, in N2Under atmosphere, with 2
℃min-1Speed be warming up to 800 DEG C and keep 8h, in N2Room temperature is naturally cooled under atmosphere, the height that phosphorus content is 2% is obtained
Energy density anode material for lithium-ion batteries.
Embodiment 2
A kind of lithium ion battery with high energy density positive electrode, its formula is LiMn0.4Fe0.6PO4Represent.
A kind of lithium ion battery with high energy density positive electrode LiMn0.4Fe0.6PO4Preparation method, specifically include as follows
Step：
(1) it is 1 by mol ratio with water-soluble lithium source compound as measurement unit:0.4:0.6:1:1.1 weigh nitric acid
Lithium, ferrous acetate, manganese nitrate, ammonium dihydrogen phosphate and glucose, add deionized water mixing wiring solution-forming, are spray-dried described molten
Liquid obtains mixture；
(2) mixture that step (1) is obtained is sintered：240 DEG C pre-oxidize 2.5h in atmosphere, in N2Under atmosphere,
With 5 DEG C of min-1Speed be warming up to 850 DEG C and keep 7h, in N2Room temperature is naturally cooled under atmosphere, it is 3% to obtain phosphorus content
Lithium ion battery with high energy density positive electrode.
Embodiment 3
A kind of lithium ion battery with high energy density positive electrode, its formula is LiMn0.3Fe0.7PO4Represent.
A kind of lithium ion battery with high energy density positive electrode LiMn0.3Fe0.7PO4Preparation method, specifically include as follows
Step：
(1) it is 1 by mol ratio with water-soluble lithium source compound as measurement unit:0.3:07:1:1.2 weigh hydroxide
Lithium, ferrous sulfate, manganese chloride, diammonium hydrogen phosphate and citric acid, add deionized water mixing wiring solution-forming, are spray-dried described molten
Liquid obtains mixture；
(2) mixture that step (1) is obtained is sintered：250 DEG C pre-oxidize 2h in atmosphere, in N2Under atmosphere, with 8
℃min-1Speed be warming up to 900 DEG C and keep 6h, in N2Room temperature is naturally cooled under atmosphere, the height that phosphorus content is 5% is obtained
Energy density anode material for lithium-ion batteries.
Embodiment 4
A kind of lithium ion battery with high energy density positive electrode, its formula is LiMn0.2Fe0.8PO4Represent.
A kind of lithium ion battery with high energy density positive electrode LiMn0.2Fe0.8PO4Preparation method, specifically include as follows
Step：
(1) it is 1 by mol ratio with water-soluble lithium source compound as measurement unit:0.2:08:1:1.35 weigh carbonic acid
Lithium, ferrous acetate, manganese sulfate, diammonium hydrogen phosphate and polyvinyl alcohol, add deionized water mixing wiring solution-forming, and spray drying is described
Solution obtains mixture；
(2) mixture that step (1) is obtained is sintered：260 DEG C pre-oxidize 2h in atmosphere, in N2Under atmosphere, with
10℃min-1Speed be warming up to 1000 DEG C and keep 5h, in N2Room temperature is naturally cooled under atmosphere, it is 6.5% to obtain phosphorus content
Lithium ion battery with high energy density positive electrode.
Embodiment 5
A kind of lithium ion battery with high energy density positive electrode, its formula is LiMn0.1Fe0.9PO4Represent.
A kind of lithium ion battery with high energy density positive electrode LiMn0.1Fe0.9PO4Preparation method, specifically include as follows
Step：
(1) it is 1 by mol ratio with water-soluble lithium source compound as measurement unit:0.1:0.9:1:1.5 weigh acetic acid
Lithium, ferrous sulfate, manganese chloride, diammonium hydrogen phosphate and polyvinylpyrrolidone, add deionized water mixing wiring solution-forming, and spraying is dry
The dry solution obtains mixture；
(2) mixture that step (1) is obtained is sintered：260 DEG C pre-oxidize 3h in atmosphere, in N2Under atmosphere, with
10℃min-1Speed be warming up to 1000 DEG C and keep 5h, in N2Room temperature is naturally cooled under atmosphere, it is 8% to obtain phosphorus content
Lithium ion battery with high energy density positive electrode.
Comparative example 1 is compared with embodiment 5, and difference is：
Comparative example 1
A kind of lithium ion battery with high energy density positive electrode, its formula is LiMn0.1Fe0.9PO4Represent.
A kind of lithium ion battery with high energy density positive electrode LiMn0.1Fe0.9PO4Preparation method, specifically include as follows
Step：
(1) it is 1 by mol ratio with water-soluble lithium source compound as measurement unit:0.1:0.9:1 weighs lithium acetate, sulphur
Sour ferrous iron, manganese chloride, diammonium hydrogen phosphate, add deionized water mixing wiring solution-forming, are spray-dried the solution and obtain mixture；
(2) mixture that step (1) is obtained is sintered：260 DEG C pre-oxidize 3h in atmosphere, in N2Under atmosphere, with
10℃min-1Speed be warming up to 1000 DEG C and keep 5h, in N2Room temperature is naturally cooled under atmosphere, it is 8% to obtain phosphorus content
Lithium ion battery with high energy density positive electrode.
Comparative example 2 is also compared with embodiment 5, and difference is：
Comparative example 2
A kind of lithium ion battery with high energy density positive electrode, its formula is LiMn0Fe0.9PO4Represent.
A kind of lithium ion battery with high energy density positive electrode LiMn0Fe0.9PO4Preparation method, specifically include following step
Suddenly：
(1) it is 1 by mol ratio with water-soluble lithium source compound as measurement unit:0.9:1:1.5 weigh lithium acetate, sulphur
Sour ferrous, diammonium hydrogen phosphate and polyvinylpyrrolidone, add deionized water mixing wiring solution-forming, are spray-dried the solution and obtain
To mixture；
(2) mixture that step (1) is obtained is sintered：260 DEG C pre-oxidize 3h in atmosphere, in N2Under atmosphere, with
10℃min-1Speed be warming up to 1000 DEG C and keep 5h, in N2Room temperature is naturally cooled under atmosphere, it is 8% to obtain phosphorus content
Lithium ion battery with high energy density positive electrode.
Positive electrode prepared by above-described embodiment 1-5 and comparative example 1-2 is prepared into li-ion electrode, performance survey is carried out
Examination, test result is as shown in table 1：
Table 1
With above-mentioned according to desirable embodiment of the invention as enlightenment, by above-mentioned description, relevant staff is complete
Various changes and amendments can be carried out without departing from the scope of the technological thought of the present invention' entirely.The technology of this invention
Property scope is not limited to the content on specification, it is necessary to its technical scope is determined according to right.
Claims (10)
1. a kind of lithium ion battery with high energy density positive electrode, it is characterised in that：Use formula LiMn1-xFexPO4Represent, wherein
0.5≤X ＜ 1.
2. a kind of lithium ion battery with high energy density positive electrode as claimed in claim 1, it is characterised in that the formula
In, 0.5≤X≤0.9.
3. a kind of preparation method of lithium ion battery with high energy density positive electrode as claimed in claim 1, it is characterised in that
Comprise the following steps：
(1) with LiMn1-xFexPO4Proportioning weigh water-soluble lithium source compound, water-soluble iron source compound, water-soluble manganese source
Compound, P source compound and carbon source material, wherein 0.5≤X≤0.9, adds deionized water mixing wiring solution-forming, are spray-dried institute
State solution and obtain mixture；
(2) mixture that step (1) is obtained is sintered：220~260 DEG C pre-oxidize 2~3h in atmosphere, in N2Under atmosphere,
With 2~10 DEG C of min-1Speed be warming up to 800~1000 DEG C and keep 5~8h, in N2Room temperature is naturally cooled under atmosphere, is obtained
Lithium ion battery with high energy density positive electrode.
4. the preparation method of lithium ion battery with high energy density positive electrode as claimed in claim 2, it is characterised in that described
Li source compound be lithium acetate, the one kind in lithium nitrate, lithium hydroxide, lithium carbonate.
5. the preparation method of lithium ion battery with high energy density positive electrode as claimed in claim 2, it is characterised in that described
Fe source compound be the one kind in ferrous nitrate, ferrous acetate, ferrous sulfate.
6. the preparation method of lithium ion battery with high energy density positive electrode as claimed in claim 2, it is characterised in that described
Manganese source compound be the one kind in manganese acetate, manganese nitrate, manganese chloride, manganese sulfate.
7. the preparation method of lithium ion battery with high energy density positive electrode as claimed in claim 2, it is characterised in that described
P source compound be the one kind in phosphoric acid, ammonium dihydrogen phosphate, diammonium hydrogen phosphate.
8. the preparation method of lithium ion battery with high energy density positive electrode as claimed in claim 2, it is characterised in that described
Carbon source material be the one kind in sucrose, glucose, citric acid, polyvinyl alcohol, polyvinylpyrrolidone.
9. the preparation method of lithium ion battery with high energy density positive electrode as claimed in claim 2, it is characterised in that described
The mol ratio of water-soluble lithium source compound and carbon source material be 1: (1~1.5).
10. the preparation method of lithium ion battery with high energy density positive electrode as claimed in claim 2, it is characterised in that institute
Phosphorus content is 2~8% in the lithium ion battery with high energy density positive electrode obtained after the sintering stated.
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Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102394296A (en) * | 2011-11-28 | 2012-03-28 | 苏州大学 | Anode material for lithium battery and preparation method thereof, and lithium battery anode and lithium battery |
| CN102874789A (en) * | 2012-10-22 | 2013-01-16 | 苏州大学 | Lithium ion battery anode material lithium iron manganese phosphate and preparation method thereof |
| CN104347875A (en) * | 2014-09-28 | 2015-02-11 | 山东精工电子科技有限公司 | Positive electrode material lithium iron manganese phosphate of lithium-ion battery and a preparing method of positive electrode material |
| CN105329867A (en) * | 2015-11-11 | 2016-02-17 | 浙江兴海能源科技有限公司 | High-compaction preparation method of lithium ferric manganese phosphate |
| CN105514430A (en) * | 2015-12-30 | 2016-04-20 | 山东精工电子科技有限公司 | Spherical LiFexMnyPO4 anode material and preparation method thereof |
-
2017
- 2017-03-22 CN CN201710172806.2A patent/CN106904588B/en active Active
Patent Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102394296A (en) * | 2011-11-28 | 2012-03-28 | 苏州大学 | Anode material for lithium battery and preparation method thereof, and lithium battery anode and lithium battery |
| CN102874789A (en) * | 2012-10-22 | 2013-01-16 | 苏州大学 | Lithium ion battery anode material lithium iron manganese phosphate and preparation method thereof |
| CN104347875A (en) * | 2014-09-28 | 2015-02-11 | 山东精工电子科技有限公司 | Positive electrode material lithium iron manganese phosphate of lithium-ion battery and a preparing method of positive electrode material |
| CN105329867A (en) * | 2015-11-11 | 2016-02-17 | 浙江兴海能源科技有限公司 | High-compaction preparation method of lithium ferric manganese phosphate |
| CN105514430A (en) * | 2015-12-30 | 2016-04-20 | 山东精工电子科技有限公司 | Spherical LiFexMnyPO4 anode material and preparation method thereof |
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