CN108011104A - A kind of high compacted density lithium iron phosphate positive material and preparation method thereof - Google Patents
A kind of high compacted density lithium iron phosphate positive material and preparation method thereof Download PDFInfo
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- CN108011104A CN108011104A CN201711315675.5A CN201711315675A CN108011104A CN 108011104 A CN108011104 A CN 108011104A CN 201711315675 A CN201711315675 A CN 201711315675A CN 108011104 A CN108011104 A CN 108011104A
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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
- 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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- 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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Abstract
The invention discloses a kind of high compacted density lithium iron phosphate positive material and preparation method thereof, select size two kinds of particles slurry, in the grinding stage by the way that bulky grain slurry and little particle slurry are mixed according to a certain ratio, then high compacted density LiFePO4 is made through drying process and heat treatment respectively, the LiFePO4 density of preparation is big, preparation process flow is simple, cost is low, can be applied to industrialized production, realize automated control, finished product lithium iron phosphate performance is good, economize on resources, improve production efficiency.
Description
Technical field
The invention belongs to field of lithium ion battery, specifically, is related to a kind of high compacted density lithium iron phosphate positive material
And preparation method thereof.
Background technology
Compacted density has battery performance on large effect, compacted density and piece specific capacity, efficiency, internal resistance and battery
Cycle performance has close relationship.In general, compacted density is bigger, and the capacity of battery is higher with regard to what can be done, so compacting is close
Degree is also seen as one of reference index of material energy densities, and under conditions of process conditions are certain, compacted density is bigger, battery
Capacity is higher.The usable compacted density of LiFePO4 restricts battery largely in 2.1-2.3g/cm3 currently on the market
Energy density, existing production technology is more using repeatedly compacting and sintering, and manufacturing process is extremely complex, and production cost significantly carries
Height, product batches stability are poor.
In view of this it is special to propose the present invention.
The content of the invention
The technical problem to be solved in the present invention is to overcome the deficiencies of the prior art and provide a kind of high compacted density ferric phosphate
Lithium anode material and preparation method thereof, selects size two kinds of particles slurry, in the grinding stage by by bulky grain slurry and small
Grain slurry is mixed according to a certain ratio, and high compacted density LiFePO4 then is made through drying process and heat treatment respectively,
The LiFePO4 density of preparation is big, and preparation process flow is simple, cost is low, can be applied to industrialized production, realizes automation
Control, finished product lithium iron phosphate performance is good, economizes on resources, and improves production efficiency.
In order to solve the above technical problems, the present invention is using the basic conception of technical solution：
A kind of high compacted density lithium iron phosphate positive material preparation method, comprises the following steps：
Step S1, prepares bulky grain slurry, by pure water, ferric phosphate, lithium source, carbon source, additive in proportion mixed grinding into
Particle diameter is 0.6-1.5 μm of mixture, obtains bulky grain slurry；
Step S2, prepare little particle slurry, by pure water, ferric phosphate, lithium source, carbon source, additive in proportion mixed grinding into
Particle diameter is 0.05-0.6 μm of mixture, obtains little particle slurry；
Step S3, prepares ferric lithium phosphate precursor powder, and bulky grain slurry, little particle slurry are mixed according to a certain percentage
Close, it is spray-dried thereafter, obtain ferric lithium phosphate precursor powder；
Step S4, prepares LiFePO4 finished product, ferric lithium phosphate precursor powder is placed in atmosphere furnace after being heat-treated,
It is broken into promoting the circulation of qi again, obtain LiFePO4 finished product.
Further, the lithium source is lithium phosphate, lithium carbonate, lithium hydroxide, lithium acetate, one kind in lithium oxalate or any
Combination.
Further, the carbon source is one kind in glucose, sucrose, citric acid, phenolic resin, graphite, carbon nanotubes
Or any combination.
Further, the additive for magnesium acetate, aluminium oxide, titanium oxide, niobium pentaoxide, zirconium oxide one kind or appoint
Meaning combination.
Further, the pure water, ferric phosphate, lithium source, carbon source, the quality proportioning of additive are 200:
(90-110):(20-30):(8-13):(0.3-1.0)。
Further, the pure water, ferric phosphate, lithium source, carbon source, the quality proportioning of additive are 200:100：25:10:
0.5。
Further, the particle diameter of bulky grain slurry is 0.8-1.1 μm in the step S1, step S2 small particles slurries
Particle diameter is 0.2-0.4 μm.
Further, bulky grain slurry, the mass mixing ratio of little particle slurry are 1 in the step S3:9~9:1.It is excellent
Selection of land, quality are mixed than for 2:8-4:6.
Further, the condition of heat treatment is in atmosphere furnace in the step S4：500-850 DEG C of bar in atmosphere of inert gases
Isothermal reaction 6-15h under part.Preferably, isothermal reaction 8-12h under the conditions of 650-750 DEG C.
Further, the inert gas is nitrogen, argon gas, one kind or any combination in helium.
A kind of high compacted density lithium iron phosphate positive material, by above-mentioned high compacted density lithium iron phosphate positive material preparation side
Method is prepared.
After adopting the above technical scheme, the present invention has the advantages that compared with prior art.
The present invention first prepares size two kinds of particles slurry, in the grinding stage by the way that bulky grain slurry and little particle slurry are pressed
Mixed according to certain proportioning, high compacted density LiFePO4, the phosphorus of preparation then is made through drying process and heat treatment respectively
Sour iron lithium density is big, and preparation process flow is simple, cost is low, can be applied to industrialized production, realizes automated control, finished product
Property it is good, economize on resources, improve production efficiency.
The compacted density of the obtained LiFePO4 of the present invention is played in 2.4-2.6g/cm3, the gram volume of full battery 1C
More than 144mAh/g, when simplifying the technological process of production, can effectively improve the compacted density of LiFePO4, meet country and
Battery Plant meets enterprise to production cost control and automated production to lifting the demand of energy density, highly practical, beneficial to pushing away
Wide application.
The embodiment of the present invention is described in further detail below in conjunction with the accompanying drawings.
Brief description of the drawings
A part of the attached drawing as the application, for providing further understanding of the invention, of the invention is schematic
Embodiment and its explanation are used to explain the present invention, but do not form inappropriate limitation of the present invention.Obviously, drawings in the following description
Only some embodiments, to those skilled in the art, without creative efforts, can be with
Other accompanying drawings are obtained according to these attached drawings.In the accompanying drawings：
Fig. 1 is the method for the present invention flow diagram.
It should be noted that these attached drawings and word description are not intended as the design model limiting the invention in any way
Enclose, but idea of the invention is illustrated for those skilled in the art by reference to specific embodiment.
Embodiment
To make the purpose, technical scheme and advantage of the embodiment of the present invention clearer, below in conjunction with the embodiment of the present invention
In attached drawing 1, the technical solution in embodiment is clearly and completely described, following embodiments be used for illustrate the present invention, but
It is not limited to the scope of the present invention.
Embodiment 1：
(1) by by pure water, ferric phosphate, lithium source, carbon source and additive according to mass ratio be 200:90:20:8:0.3 matches somebody with somebody
Fang Jinhang dispensings, after grinding 1.5h, obtain the slurry A that particle diameter is 0.8 μm；
(2) by by pure water, ferric phosphate, lithium source, carbon source and additive according to mass ratio be 200:90:20:8:0.3 matches somebody with somebody
Fang Jinhang dispensings, after grinding 4.5h, obtain the slurry B that particle diameter is 0.2 μm；
(3) by slurry A and B according to mass ratio 3：7 are mixed to get mixed slurry C, are then spray-dried slurry C,
Obtain ferric lithium phosphate precursor powder D；
(4) ferric lithium phosphate precursor powder D is placed in nitrogen atmosphere stove and is heat-treated, temperature is 650 DEG C, during constant temperature
Between be 8h, then by the LiFePO4 semi-finished product powder being thermally treated resulting in into promoting the circulation of qi it is broken after obtain LiFePO4 finished product.
Embodiment 2：
(1) by by pure water, ferric phosphate, lithium source, carbon source and additive according to mass ratio be 200:100:25:10:0.5
Formula carries out dispensing, after grinding 1.5h, obtains the slurry A that particle diameter is 0.9 μm；
(2) by by pure water, ferric phosphate, lithium source, carbon source and additive according to mass ratio be 200:100:25:10:0.5
Formula carries out dispensing, after grinding 4.5h, obtains the slurry B that particle diameter is 0.3 μm；
(3) by slurry A and B according to mass ratio 3：7 are mixed to get mixed slurry C, are then spray-dried slurry C,
Obtain ferric lithium phosphate precursor powder D；
(4) ferric lithium phosphate precursor powder D is placed in nitrogen atmosphere stove and is heat-treated, temperature is 700 DEG C, during constant temperature
Between be 10h, then by the LiFePO4 semi-finished product powder being thermally treated resulting in into promoting the circulation of qi it is broken after obtain LiFePO4 finished product.
Embodiment 3：
(1) by by pure water, ferric phosphate, lithium source, carbon source and additive according to mass ratio be 200:110:30:13:1.0
Formula carries out dispensing, after grinding 1.5h, obtains the slurry A that particle diameter is 1.0 μm；
(2) by by pure water, ferric phosphate, lithium source, carbon source and additive according to mass ratio be 200:100:25:10:0.5
Formula carries out dispensing, after grinding 4.5h, obtains the slurry B that particle diameter is 0.4 μm；
(3) by slurry A and B according to mass ratio 3：7 are mixed to get mixed slurry C, are then spray-dried slurry C,
Obtain ferric lithium phosphate precursor powder D；
(4) ferric lithium phosphate precursor powder D is placed in nitrogen atmosphere stove and is heat-treated, temperature is 750 DEG C, during constant temperature
Between be 12h, then by the LiFePO4 semi-finished product powder being thermally treated resulting in into promoting the circulation of qi it is broken after obtain LiFePO4 finished product.
Comparative example 1：
(1) by by pure water, ferric phosphate, lithium source, carbon source and additive according to mass ratio be 200:100:25:10:0.5
Formula carries out dispensing, after grinding 3-6h, obtains the slurry A that particle diameter is 0.3-1.0 μm；
(2) ferric lithium phosphate precursor powder D is placed in nitrogen atmosphere stove and is heat-treated, temperature is 700 DEG C, during constant temperature
Between be 10h, then by the LiFePO4 semi-finished product powder being thermally treated resulting in into promoting the circulation of qi it is broken after obtain LiFePO4 finished product.
Embodiment is compared as follows table with comparative example experimental data：
According to experimental result, the LiFePO4 of method preparation using the present invention, density is obviously improved, full battery
The gram volume of 1C plays more than 144mAh/g, effectively improves LiFePO4 compacted density, improves performance.The obtained ferric phosphate of the present invention
The compacted density of lithium first prepares size two kinds of particles slurry in 2.4-2.6g/cm3, in the grinding stage by by bulky grain slurry
Mixed according to a certain ratio with little particle slurry, high compacted density phosphoric acid then is made through drying process and heat treatment respectively
Iron lithium, the LiFePO4 density of preparation is big, and preparation process flow is simple, cost is low, can be applied to industrialized production, realizes certainly
Dynamicization controls, good into moral character, economizes on resources, and improves production efficiency
The above is only presently preferred embodiments of the present invention, not makees limitation in any form to the present invention, though
So the present invention is disclosed above with preferred embodiment, but is not limited to the present invention, any technology people for being familiar with this patent
Member without departing from the scope of the present invention, when the technology contents using above-mentioned prompting make it is a little change or be modified to
The equivalent embodiment of equivalent variations, as long as being the content without departing from technical solution of the present invention, the technical spirit pair according to the present invention
Any simple modification, equivalent change and modification that above example is made, in the range of still falling within the present invention program.
Claims (10)
1. a kind of high compacted density lithium iron phosphate positive material preparation method, it is characterised in that comprise the following steps：
Step S1, prepares bulky grain slurry, by pure water, ferric phosphate, lithium source, carbon source, additive in proportion mixed grinding into particle diameter
For 0.6-1.5 μm of mixture, bulky grain slurry is obtained；
Step S2, prepares little particle slurry, by pure water, ferric phosphate, lithium source, carbon source, additive in proportion mixed grinding into particle diameter
For 0.05-0.6 μm of mixture, little particle slurry is obtained；
Step S3, prepares ferric lithium phosphate precursor powder, and bulky grain slurry, little particle slurry are mixed according to a certain percentage, you
By spray drying, ferric lithium phosphate precursor powder is obtained；
Step S4, prepares LiFePO4 finished product, ferric lithium phosphate precursor powder is placed in atmosphere furnace after being heat-treated, then into
Promoting the circulation of qi is broken, obtains LiFePO4 finished product.
A kind of 2. high compacted density lithium iron phosphate positive material preparation method according to claim 1, it is characterised in that institute
Lithium source is stated as lithium phosphate, lithium carbonate, lithium hydroxide, lithium acetate, one kind or any combination in lithium oxalate.
A kind of 3. high compacted density lithium iron phosphate positive material preparation method according to claim 1, it is characterised in that institute
Carbon source is stated as glucose, sucrose, citric acid, phenolic resin, graphite, one kind or any combination in carbon nanotubes.
A kind of 4. high compacted density lithium iron phosphate positive material preparation method according to claim 1, it is characterised in that institute
Additive is stated as magnesium acetate, aluminium oxide, titanium oxide, niobium pentaoxide, one kind or any combination of zirconium oxide.
A kind of 5. high compacted density lithium iron phosphate positive material preparation method according to claim 1, it is characterised in that institute
It is 200 to state pure water, ferric phosphate, lithium source, carbon source, the quality proportioning of additive:(90-110):(20-30):(8-13):(0.3-
1.0)。
A kind of 6. high compacted density lithium iron phosphate positive material preparation method according to claim 5, it is characterised in that institute
It is 200 to state pure water, ferric phosphate, lithium source, carbon source, the quality proportioning of additive:100：25:10:0.5.
A kind of 7. high compacted density lithium iron phosphate positive material preparation method according to claim 1, it is characterised in that institute
The particle diameter for stating bulky grain slurry in step S1 is 0.8-1.1 μm, and the particle diameter of step S2 small particles slurries is 0.2-0.4 μm.
A kind of 8. high compacted density lithium iron phosphate positive material preparation method according to claim 1, it is characterised in that institute
State bulky grain slurry in step S3, the mass mixing ratio of little particle slurry is 1:9~9:1.
A kind of 9. high compacted density lithium iron phosphate positive material preparation method according to claim 1, it is characterised in that institute
Stating the condition being heat-treated in step S4 in atmosphere furnace is：Isothermal reaction 6-15h under the conditions of 500-850 DEG C in atmosphere of inert gases.
10. a kind of high compacted density lithium iron phosphate positive material, it is characterised in that by any high-pressure solids of claim 1-9
Density lithium iron phosphate positive material preparation method is prepared.
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| CN109192953A (en) * | 2018-09-07 | 2019-01-11 | 桑顿新能源科技有限公司 | A kind of high magnification spherical LiFePO 4 carbon composite anode material and preparation method thereof |
| CN109301179A (en) * | 2018-08-22 | 2019-02-01 | 江苏元景锂粉工业有限公司 | A kind of lithium battery lithium iron phosphate positive material and preparation method thereof |
| CN109336077A (en) * | 2018-08-29 | 2019-02-15 | 深圳市德方纳米科技股份有限公司 | A kind of lithium iron phosphate positive material and preparation method thereof |
| CN109336079A (en) * | 2018-11-20 | 2019-02-15 | 浙江瑞邦科技有限公司 | A kind of preparation method of high-pressure solid LiFePO 4 material |
| CN109795998A (en) * | 2018-12-29 | 2019-05-24 | 合肥融捷能源材料有限公司 | A kind of preparation method and lithium iron phosphate positive material promoting lithium iron phosphate positive material compacted density |
| CN110436431A (en) * | 2019-06-29 | 2019-11-12 | 佛山市德方纳米科技有限公司 | A kind of preparation method and lithium ion battery of lithium iron phosphate positive material |
| CN112310374A (en) * | 2020-10-30 | 2021-02-02 | 合肥融捷能源材料有限公司 | Method for preparing high-compaction low-specific-surface-area lithium iron phosphate by sectional grinding-spray drying |
| CN113086959A (en) * | 2021-02-26 | 2021-07-09 | 雅安锂盛新能企业管理中心(有限合伙) | High-compaction low-temperature lithium iron phosphate material, lithium battery positive plate and preparation method thereof |
| WO2021190490A1 (en) * | 2020-03-25 | 2021-09-30 | 比亚迪股份有限公司 | Lithium iron phosphate positive electrode sheet, preparation method therefor, and lithium iron phosphate lithium-ion battery |
| CN114068919A (en) * | 2020-08-06 | 2022-02-18 | 比亚迪股份有限公司 | Lithium iron phosphate positive electrode active material, preparation method thereof, positive plate and battery |
| CN114068920A (en) * | 2020-08-06 | 2022-02-18 | 比亚迪股份有限公司 | Lithium iron phosphate positive electrode active material, preparation method thereof, positive plate and battery |
| CN114314548A (en) * | 2021-12-29 | 2022-04-12 | 湖北万润新能源科技股份有限公司 | Titanium and zirconium co-doped carbon-coated lithium iron phosphate material and preparation method and application thereof |
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| CN109336077A (en) * | 2018-08-29 | 2019-02-15 | 深圳市德方纳米科技股份有限公司 | A kind of lithium iron phosphate positive material and preparation method thereof |
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| CN109336079A (en) * | 2018-11-20 | 2019-02-15 | 浙江瑞邦科技有限公司 | A kind of preparation method of high-pressure solid LiFePO 4 material |
| CN109795998A (en) * | 2018-12-29 | 2019-05-24 | 合肥融捷能源材料有限公司 | A kind of preparation method and lithium iron phosphate positive material promoting lithium iron phosphate positive material compacted density |
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| CN115367725B (en) * | 2022-08-29 | 2024-05-10 | 广东邦普循环科技有限公司 | Doped lithium iron phosphate and preparation method and application thereof |
| CN115818609A (en) * | 2022-11-24 | 2023-03-21 | 天津市捷威动力工业有限公司 | Lithium iron manganese phosphate material, preparation method thereof and battery |
| CN115650200A (en) * | 2022-12-06 | 2023-01-31 | 广州天赐高新材料股份有限公司 | Preparation method of high-energy-density lithium iron phosphate material |
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