CN107768655A - A kind of manufacture method based on closs packing ferric lithium phosphate precursor material - Google Patents
A kind of manufacture method based on closs packing ferric lithium phosphate precursor material Download PDFInfo
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- CN107768655A CN107768655A CN201711025498.7A CN201711025498A CN107768655A CN 107768655 A CN107768655 A CN 107768655A CN 201711025498 A CN201711025498 A CN 201711025498A CN 107768655 A CN107768655 A CN 107768655A
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- lithium
- phosphate
- ferric
- manufacture method
- closs packing
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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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- 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
- H01M4/583—Carbonaceous material, e.g. graphite-intercalation compounds or CFx
- H01M4/587—Carbonaceous material, e.g. graphite-intercalation compounds or CFx for inserting or intercalating light metals
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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 a kind of manufacture method based on closs packing ferric lithium phosphate precursor material.The invention belongs to technical field of lithium ion.A kind of manufacture method based on closs packing ferric lithium phosphate precursor material, including following technical process：Step 1：Prepare ball shape ferric phosphate：Anhydrous iron phosphate is subjected to dry ball milling, obtains the ball shape ferric phosphate of 0.3 3 μm of particle mean size；Step 2：Prepare spherical precursor：By using short carbon chain sugar alcohol as carbon source, after ball shape ferric phosphate is well mixed with lithium source and carbon source, pure water is added, is ground under water solution system, then the drying spherical precursor of 5 50 μ m diameters is made in spray drying process；Step 3：Prepare high-density lithium iron phosphate：By converter type high temperature sintering, in N2Under the protection of atmosphere, 580 780 DEG C of calcinings, insulation, high compacted density lithium iron phosphate material is obtained.The present invention is easy to get with raw material, and cheap, technique is simple, simple operation, the advantages that greatly improving the volume energy density of lithium ion battery.
Description
Technical field
The invention belongs to technical field of lithium ion, and closs packing ferric lithium phosphate precursor material is based on more particularly to one kind
The manufacture method of material.
Background technology
At present, preparing lithium ion battery using lithium iron phosphate positive material has security good, has extended cycle life and capacity
Conservation rate is high, and multiplying power discharging ability is strong.Therefore, lithium iron phosphate positive material is considered as the preferable positive pole of power lithium-ion battery
Material.
In order to solve the problems such as ferric phosphate lithium cell gravimetric specific energy is low, cost is high.Lithium-ion-power cell was making
Cheng Zhong, compacted density have large effect to battery performance.The real density of LiFePO4 is 3.6g/cm3, still, at present with one
As technique to prepare the compacted density of LiFePO4 be 2.1-2.4g/cm3(coming from lithium battery grade lithium iron phosphate preparation method).Typically
For, compacted density is bigger, and the capacity of same specification size battery is higher with regard to what can be done, so compacted density is also seen as material energy
One of reference index of metric density.
It is believed that under conditions of battery specifications model is fixed, process conditions are certain, compacted density is bigger, monomer electricity
The capacity in pond is higher, and the unit integrated cost of battery is also lower.Compacted density is too small, and the transmission of lithium ion is apart from limited, electrode
Thickness is just restricted, and positive pole just applies very thin, and being unfavorable for battery raising capacity, (Yang Hong etc., power technology, compacted density is to height
The influence .33 (2009/11) of magnification lithium ion battery performance：11).The compacted density of existing preparation method LiFePO4
Industrial demand can not be met.
The content of the invention
The present invention provides one kind for technical problem present in solution known technology and is based on closs packing LiFePO4 forerunner
The manufacture method of body material.
It is easy to get it is an object of the invention to provide one kind with raw material, cheap, technique is simple, and simple operation can be significantly
The manufacture method based on closs packing ferric lithium phosphate precursor material for the features such as improving the volume energy density of lithium ion battery.
Closs packing refers in materialogy, particle with a kind of closelypacked state of the shape of subglobular, now have compared with
Big bulk density.If the primary particle of LiFePO4 is distributed in a manner of closely packed, the compacted density of material should
It can increase substantially.
A kind of manufacture method based on closs packing ferric lithium phosphate precursor material proposed by the present invention, can greatly improve lithium
The volume energy density of ion battery.Using the carbon source of few carbon sugar, work mainly is carried out by converter type high temperature sintering by the present invention
Skill is improved, to realize the densification of LiFePO4.
A kind of manufacture method based on closs packing ferric lithium phosphate precursor material, its technique are：The first step mainly manufactures
Spherical ferric phosphate, using the improvement by using short carbon chain sugar alcohol as carbon source, to improve the compacted density of material.Second step is
Spherical secondary agglomeration body is manufactured by spray drying technology.3rd step is by converter type high temperature sintering, and it is close to obtain high-pressure solid
The LiFePO 4 material of degree.
Manufacture method of the invention based on closs packing ferric lithium phosphate precursor material is adopted the technical scheme that：
A kind of manufacture method based on closs packing ferric lithium phosphate precursor material, is characterized in：Based on closs packing ferric phosphate
The manufacture method of lithium persursor material includes following technical process：
Step 1：Prepare ball shape ferric phosphate
Anhydrous iron phosphate is subjected to dry ball milling, obtains the ball shape ferric phosphate of 0.3-3 μm of particle mean size；
Step 2：Prepare spherical precursor
By using short carbon chain sugar alcohol as carbon source, after ball shape ferric phosphate is well mixed with lithium source and carbon source, add pure
Water, ground under water solution system, then the drying spherical precursor of 5-50 μ m diameters is made in spray drying process；
Step 3：Prepare high-density lithium iron phosphate
By converter type high temperature sintering, in N2Under the protection of atmosphere, 580-780 DEG C of calcining, insulation, high compacted density is obtained
LiFePO 4 material.
Manufacture method of the invention based on closs packing ferric lithium phosphate precursor material can also adopt the following technical scheme that：
The described manufacture method based on closs packing ferric lithium phosphate precursor material, is characterized in：Prepare ball shape ferric phosphate
When, anhydrous iron phosphate dry ball milling device therefor is ball mill, from 0.8-2mm zirconia balls, the ball material weight of dry ball milling
Than for 1-10：1, ball milling 1-10h, obtains ball shape ferric phosphate under air, room temperature environment.
The described manufacture method based on closs packing ferric lithium phosphate precursor material, is characterized in：Prepare spherical precursor
When, the solid content weight ratio of control system is 30-70%, ratio of grinding media to material 1-10：1,1-10h is ground under air, room temperature environment, so
After be spray-dried.
The described manufacture method based on closs packing ferric lithium phosphate precursor material, is characterized in：Prepare spherical precursor
When, short carbon chain sugar alcohol is pentose xylitol, arabite, or tetrose antierythrite；Lithium source be lithium carbonate, lithium hydroxide or
One kind of lithium dihydrogen phosphate.
The described manufacture method based on closs packing ferric lithium phosphate precursor material, is characterized in：Grinding device therefor is
Ball mill, a diameter of 0.8-2mm zirconia balls, 300-350 DEG C of the EAT of spray drying device, leaving air temp 100-
120 DEG C, slurry flow setting 90-110ml/min.
The described manufacture method based on closs packing ferric lithium phosphate precursor material, is characterized in：Prepare high density phosphoric acid
During iron lithium, the programming rate of converter type high temperature sintering is 8-12 DEG C/min, soaking time 4h-10h.
The present invention has the advantages and positive effects of：
Manufacture method based on closs packing ferric lithium phosphate precursor material as a result of the brand-new technical scheme of the present invention,
Compared with prior art, the present invention is easy to get with raw material, and cheap, technique is simple, simple operation, can greatly improve lithium ion
The advantages that volume energy density of battery.
Brief description of the drawings
Fig. 1 is that the present invention is schemed based on closs packing ferric lithium phosphate precursor ball shape ferric phosphate lithium material SEM.
Embodiment
In order to further understand the content, features and effects of the present invention, hereby enumerating following examples, and coordinate accompanying drawing
Describe in detail as follows：
Refering to accompanying drawing 1.
Embodiment 1
A kind of manufacture method based on closs packing ferric lithium phosphate precursor material, including following technical process：
Step 1：Prepare ball shape ferric phosphate
10 kilograms of anhydrous iron phosphates are subjected to dry ball millings first, load 10 kilograms of 2mm diameter zirconium oxides ball, air,
30L ball mill ball milling 10h are used under room temperature environment, obtain the ball shape ferric phosphate of 3 μm of average diameter.
Step 2：Prepare spherical precursor
After the ferric phosphate is well mixed with 2.5 kilograms of lithium carbonates and 0.45 kilogram of xylitol, 10 kilograms of water are added, in water
Under solution system, 10 hours (loading 20 kilograms of 2mm diameter zirconium oxides ball) is ground with 20L ball mills, then passes through spraying
Seasoning, EAT set 325 DEG C, and leaving air temp sets 110 DEG C, flow set 100ml/min, and 50 μm of dryings of diameter are made
Spherical precursor.
Step 3：Prepare high-density lithium iron phosphate
Material is sintered in rotatable sintering furnace, in N2Under the protection of atmosphere, sintering temperature is 780 DEG C, programming rate 12
DEG C/min, it is incubated 4h.By the material manufacture iron phosphate lithium positive pole pole piece, compacted density can reach 2.65g/cm3。
Embodiment 2
A kind of manufacture method based on closs packing ferric lithium phosphate precursor material, including following technical process：
Step 1：Prepare ball shape ferric phosphate
10 kilograms of anhydrous iron phosphates are subjected to dry ball milling first, load 0.8mm diameter zirconium oxide ball double centners, in sky
100L ball mill ball milling 1h are used under gas, room temperature environment, obtain 0.3 μm of ball shape ferric phosphate.
Step 2：Prepare spherical precursor
After the ferric phosphate is well mixed with 2.5 kilograms of lithium carbonates and 0.5 kilogram of antierythrite, 10 kilograms of water are added,
Under aqueous phase system, 1h (loading 200 kilograms of 0.8mm diameter zirconium oxides ball) is ground with 200L ball mills, then passes through spraying
Seasoning, EAT set 325 DEG C, and leaving air temp sets 110 DEG C, flow set 100ml/min, and the dry of 5 μ m diameters is made
Dry spherical precursor.
Step 3：Prepare high-density lithium iron phosphate
Material is sintered in rotatable sintering furnace, in N2Under the protection of atmosphere, sintering temperature is 580 DEG C, programming rate 8
DEG C/min, it is incubated 10h.By the material manufacture iron phosphate lithium positive pole pole piece, compacted density can reach 2.6g/cm3。
Embodiment 3
A kind of manufacture method based on closs packing ferric lithium phosphate precursor material, including following technical process：
Step 1：Prepare ball shape ferric phosphate
Double centner anhydrous iron phosphate is subjected to dry ball milling first, loads 500 kilograms of 1mm diameter zirconium oxides ball, in sky
500L ball mill ball milling 5h are used under gas, room temperature environment, obtain 1 μm of ball shape ferric phosphate.
Step 2：Prepare spherical precursor
After the ferric phosphate is well mixed with 25 kilograms of lithium carbonates and 7 kilograms of xylitols, double centner water is added, in aqueous phase
Under system, 5h (load 1mm diameter zirconium oxides ball 500 kilograms) is ground with 500L ball mills, then by spray drying process,
EAT sets 325 DEG C, and leaving air temp sets 110 DEG C, flow set 100ml/min, and the ball of the drying of 20 μ m diameters is made
Shape presoma.
Step 3：Prepare high-density lithium iron phosphate
Material is sintered in rotatable sintering furnace, in N2Under the protection of atmosphere, sintering temperature is 700 DEG C, programming rate 10
DEG C/min, it is incubated 6h.By the material manufacture iron phosphate lithium positive pole pole piece, compacted density can reach 2.75g/cm3。
Embodiment 4
A kind of manufacture method based on closs packing ferric lithium phosphate precursor material, including following technical process：
Step 1：Prepare ball shape ferric phosphate
Double centner anhydrous iron phosphate is subjected to dry ball milling first, loads 800 kilograms of 1mm diameter zirconium oxides ball, in sky
800L ball mill ball milling 2.5h are used under gas, room temperature environment, obtain 2 μm of ball shape ferric phosphate.
Step 2：Prepare spherical precursor
After the ferric phosphate is well mixed with 25 kilograms of lithium carbonates and 7.5 kilograms of erythroses, double centner water is added, in water
Under phase system, 2.5h (loading 800 kilograms of 1mm diameter zirconium oxides ball) is ground with 800L ball mills, it is then dry by spraying
Dry method, EAT set 325 DEG C, and leaving air temp sets 110 DEG C, flow set 100ml/min, the drying of 10 μ m diameters is made
Spherical precursor.
Step 3：Prepare high-density lithium iron phosphate
Material is sintered in rotatable sintering furnace, in N2Under the protection of atmosphere, sintering temperature is 650 DEG C, programming rate 9
DEG C/min, it is incubated 8h.By the material manufacture iron phosphate lithium positive pole pole piece, compacted density can reach 2.7g/cm3。
There is the present embodiment described raw material to be easy to get, cheap, and technique is simple, simple operation, can greatly improve lithium from
The good effects such as the volume energy density of sub- battery.
Claims (6)
1. a kind of manufacture method based on closs packing ferric lithium phosphate precursor material, it is characterized in that：Based on closs packing LiFePO4
The manufacture method of persursor material includes following technical process：
Step 1：Prepare ball shape ferric phosphate
Anhydrous iron phosphate is subjected to dry ball milling, obtains the ball shape ferric phosphate of 0.3-3 μm of particle mean size；
Step 2：Prepare spherical precursor
By using short carbon chain sugar alcohol as carbon source, after ball shape ferric phosphate is well mixed with lithium source and carbon source, pure water is added,
Ground under water solution system, then the drying spherical precursor of 5-50 μ m diameters is made in spray drying process；
Step 3：Prepare high-density lithium iron phosphate
By converter type high temperature sintering, in N2Under the protection of atmosphere, 580-780 DEG C of calcining, insulation, high compacted density phosphoric acid is obtained
Iron lithium material.
2. the manufacture method according to claim 1 based on closs packing ferric lithium phosphate precursor material, it is characterized in that：Prepare
During ball shape ferric phosphate, anhydrous iron phosphate dry ball milling device therefor is ball mill, from 0.8-2mm zirconia balls, dry ball milling
Ball material weight ratio be 1-10：1, ball milling 1-10h, obtains ball shape ferric phosphate under air, room temperature environment.
3. the manufacture method according to claim 1 based on closs packing ferric lithium phosphate precursor material, it is characterized in that：Prepare
During spherical precursor, the solid content weight ratio of control system is 30-70%, ratio of grinding media to material 1-10：1, grind under air, room temperature environment
1-10h is ground, is then spray-dried.
4. the manufacture method based on closs packing ferric lithium phosphate precursor material according to claim 1 or 3, it is characterized in that：
When preparing spherical precursor, short carbon chain sugar alcohol is pentose xylitol, arabite, or tetrose antierythrite；Lithium source is carbon
One kind of sour lithium, lithium hydroxide or lithium dihydrogen phosphate.
5. the manufacture method based on closs packing ferric lithium phosphate precursor material according to claim 1 or 3, it is characterized in that：
Grinding device therefor is ball mill, a diameter of 0.8-2mm zirconia balls, 300-350 DEG C of the EAT of spray drying device,
100-120 DEG C of leaving air temp, slurry flow setting 90-110ml/min.
6. the manufacture method according to claim 1 based on closs packing ferric lithium phosphate precursor material, it is characterized in that：Prepare
During high-density lithium iron phosphate, the programming rate of converter type high temperature sintering is 8-12 DEG C/min, soaking time 4h-10h.
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN109650366A (en) * | 2018-11-22 | 2019-04-19 | 湖北融通高科先进材料有限公司 | A kind of LiFePO4 and preparation method thereof |
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| US20030190528A1 (en) * | 2002-04-03 | 2003-10-09 | Saidi Mohammed Y. | Alkali-iron-cobalt phosphates and related electrode active materials |
| CN1675785A (en) * | 2002-07-22 | 2005-09-28 | 威伦斯技术公司 | Method of synthesizing electrochemically active materials from a slurry of precursors |
| CN102569795A (en) * | 2012-01-02 | 2012-07-11 | 株洲泰和高科技有限公司 | Comprehensive modification method for synthesis of lithium iron phosphate |
| CN103996846A (en) * | 2014-04-14 | 2014-08-20 | 江苏中欧材料研究院有限公司 | Preparation method for lithium iron phosphate positive electrode material with controllable particle size |
| CN106602061A (en) * | 2016-12-28 | 2017-04-26 | 天津先众新能源科技股份有限公司 | Preparation method of high-density lithium iron phosphate material |
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2017
- 2017-10-27 CN CN201711025498.7A patent/CN107768655A/en active Pending
Patent Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US20030190528A1 (en) * | 2002-04-03 | 2003-10-09 | Saidi Mohammed Y. | Alkali-iron-cobalt phosphates and related electrode active materials |
| CN1675785A (en) * | 2002-07-22 | 2005-09-28 | 威伦斯技术公司 | Method of synthesizing electrochemically active materials from a slurry of precursors |
| CN102569795A (en) * | 2012-01-02 | 2012-07-11 | 株洲泰和高科技有限公司 | Comprehensive modification method for synthesis of lithium iron phosphate |
| CN103996846A (en) * | 2014-04-14 | 2014-08-20 | 江苏中欧材料研究院有限公司 | Preparation method for lithium iron phosphate positive electrode material with controllable particle size |
| CN106602061A (en) * | 2016-12-28 | 2017-04-26 | 天津先众新能源科技股份有限公司 | Preparation method of high-density lithium iron phosphate material |
Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN109650366A (en) * | 2018-11-22 | 2019-04-19 | 湖北融通高科先进材料有限公司 | A kind of LiFePO4 and preparation method thereof |
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Application publication date: 20180306 |