CN107742709A - A kind of lithium iron phosphate battery anode active material and its preparation and application - Google Patents
A kind of lithium iron phosphate battery anode active material and its preparation and application Download PDFInfo
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- CN107742709A CN107742709A CN201710963169.0A CN201710963169A CN107742709A CN 107742709 A CN107742709 A CN 107742709A CN 201710963169 A CN201710963169 A CN 201710963169A CN 107742709 A CN107742709 A CN 107742709A
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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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- 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
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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
- C01B25/37—Phosphates of heavy metals
- C01B25/375—Phosphates of heavy metals of iron
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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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- 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 present invention relates to technical field of lithium ion, and in particular to one kind reduces ferric phosphate lithium cell polarity effect and improves sour lithium iron battery electrochemistry (high rate performance) lithium iron phosphate battery anode active material and its preparation and application.Active material is two layers, first layer active material, and the second layer active material coated on first layer surface of active material;The first layer active material is counted in parts by weight, by 80~95 parts of lithium iron phosphate positive material, 3~12 parts of conductive agent, 3~10 parts of first kind binding agent composition;The second layer active material is counted in parts by weight, by 85~98 parts of lithium iron phosphate positive material, 1~8 part of conductive agent, 5~8 parts of the second class binding agent composition.The double-deck lithium iron phosphate positive material pole piece prepared using method of modifying of the present invention, compared to the common LiFePO4 pole piece containing identical conduction agent, its battery polarization is greatly lowered, so that the high rate performance tool of LiFePO4 is significantly improved.The cycle performance of the product is excellent simultaneously.
Description
Technical field
The present invention relates to technical field of lithium ion, and in particular to one kind reduces ferric phosphate lithium cell polarity effect and improved
Sour lithium iron battery electrochemistry (high rate performance) lithium iron phosphate battery anode active material and its preparation and application.
Background technology
As secondary cell of new generation, lithium ion battery is considered as most promising secondary cell.With traditional lead
The secondary cells such as sour battery, Ni-MH battery, NI-G are compared, and lithium ion battery has that operating voltage is high, have extended cycle life, energy is close
Spend many advantages such as big, memoryless function.Since the nineties in last century, lithium ion battery occurred, with lithium ion battery material
And the continuous development and progress of key technology, it has been widely used in the fields such as electronic product, new-energy automobile, Aero-Space.
Wherein positive electrode is the critical material of lithium ion battery, its property and price directly determine the performance of lithium ion battery with into
This.At present, domestic anode material for lithium-ion batteries be concentrated mainly on LiMn2O4, ternary lithium (including nickel cobalt manganese and nickel cobalt aluminium) and
LiFePO4, wherein, due to LiFePO4 (LiFePO4) there is good cycling stability, safe, raw material sources to enrich, no
Containing advantages such as toxic metals, it is considered to be one of most promising material in existing positive electrode.But due to phosphoric acid
Iron lithium has special olivine crystalline structure, and electronics and lithium ion are relatively low in material internal transmission rate, so as to cause phosphoric acid
Iron lithium internal polarization in charge and discharge process is larger, high rate charge-discharge poor performance, seriously hinders its answering in electrokinetic cell
With.Therefore improving LiFePO4 high rate performance has larger scientific meaning.
The pertinent literature and patent of modified phosphate iron lithium high rate performance mainly have:Carbon coating, the nanosizing of material, aluminum foil coating
Cover carbon coating and the conductive agent from excellent electric conductivity.Such as:Patent CN105633403A, it is related to a kind of positive electrode and presents
Core shell structure, kernel are cellular nano LiFePO4, and shell is lithium metaaluminate compound coating layer, ferric phosphate prepared by this method
Lithium high rate performance is excellent;But this method is because the LiFePO4 used is nanoscale cellular material, and outer layer contains clad,
So that the material tap density is relatively low, cause its volume energy density not high.
For another example patent CN103531797A, it is related to a kind of lithium battery conductive modified lithium iron phosphate positive material and its preparation
Method, it is conductive additive that this method, which mainly adds modified silver powder, improves material conductivity, and effectively suppresses the length of crystal
Greatly, dispersed LiFePO 4 material is obtained.LiFePO4 prepared by this method has that preparation technology is simple, discharge capacity
Greatly, the advantages that battery consistency is high.But silver powder is easy to produce potential safety hazard as conductive additive, and silver powder does conductive agent and made
Positive electrode adds material cost.
Therefore it is badly in need of the improved method that a kind of energy density is high, safe.
The content of the invention
The problem of existing for above-mentioned technology, the purpose of the present invention are on the basis of material cost is constant, there is provided a kind of
Reduce ferric phosphate lithium cell polarity effect and improve sour lithium iron battery electrochemistry (high rate performance) lithium iron phosphate battery anode activity material
Material and its preparation and application.
To achieve the above object, the present invention uses following technical scheme:
A kind of lithium iron phosphate battery anode active material, two layers of active material, first layer active material, and be coated on
The second layer active material of first layer surface of active material;
The first layer active material is counted in parts by weight, by 80~95 parts of lithium iron phosphate positive material, 3~12 parts
Conductive agent, 3~10 parts of first kind binding agent composition;
The second layer active material is counted in parts by weight, by 85~98 parts of lithium iron phosphate positive material, 1~8 part
Conductive agent, 5~8 parts of the second class binding agent composition.
In two layers of active material, LiFePO4 using particle diameter between 500~2000nm, tap density be 1.35~
1.65g/cm3Between nanoscale or submicron order LiFePO4 microballoon, its gram volume is 145~175mAh/g, first charge-discharge
Efficiency is 98.0~99.9%.
What the conductive agent in the first layer, second layer active material may be the same or different be selected from graphene, SP conductive agents,
It is one or more compound in acetylene black, CNT.
Conductive agent is 1.1 in mass ratio in conductive agent and second layer active material in the first layer active material:1~
5:1, conductive agent content is more than the conductive agent content in second layer active material wherein in first layer active material.
First binding agent is the copolymer of Kynoar or Kynoar-hexafluoropropene, and its molecular weight exists
Between 5000~20000;
Second binding agent is selected from polyvinyl chloride (PVC) or Kynoar (PVDF).
The first coating thickness is 3 with second coating thickness ratio:1~1:5.
A kind of preparation method of lithium iron phosphate battery anode active material:
(1) the first binding agent is dissolved in nmp solution, it is according still further to aforementioned proportion that LiFePO4 and conductive agent is fully mixed
Close, mixed liquor is added in the nmp solution of the first binding agent of dissolving several times after mixing, first 5~8h of ultrasonic disperse, then be put in
36~48h is sufficiently stirred in agitator, that is, obtains slurry 1, that is, obtains first layer active material;
(2) the second binding agent is dissolved in nmp solution, it is according still further to aforementioned proportion that LiFePO4 and conductive agent is fully mixed
Close, be added to mixed liquor in the nmp solution of the second binding agent of dissolving several times after mixing, first 5~8h of ultrasonic disperse, then be put in
24~36h is sufficiently stirred in agitator, that is, obtains slurry 2, the slurry 2 prepared is coated on first layer active material table
Face.
4~8 additions of the LiFePO4 and conductive agent mixed solution point, every time addition are separated by 2~3h.
In the first layer active material solution, adjustment nmp solution is 2 with solids content mass ratio:1-6:1 so that slurry
Material viscosity is 5000~15000Pa.S;
In the second layer active material solution, adjustment nmp solution is 3 with solids content mass ratio:1-7:1 so that slurry
Material viscosity is 1000~10000Pa.S.
A kind of application of lithium iron phosphate battery anode active material, the lithium iron phosphate battery anode active material are used to make
Standby lithium iron phosphate positive material pole piece is applied in lithium ion battery.The collector is aluminium foil.
Advantage for present invention:
Active material of the present invention fully dispersed active material and conductive agent, prevents active matter by adding a large amount of conductive agents
The local reunion of matter and conductive agent, on the basis of reducing volume capacity, the problem of improving LiFePO4 high rate performance.It is logical first
Cross and coat one layer containing the higher composite coating of conductive dosage in collection liquid surface, due to containing more conductive agent in the coating,
So as to significantly improve the contact impedance between positive electrode and collector, while this layer of conductive agent is to absorb the shape of micro-current
Formula, faster by the electric transmission that upper layer transport comes to collector, this layer of conductive agent can be good at BES in addition
Absorption, avoid upper layer of material electrolyte excessive, subsurface material electrolyte lack the problem of, so as to balance well electronics biography
The problem of defeated and lithium ion transport.
Secondly, on the premise of the conductive agents of special ratios of the present invention is sufficiently mixed with LiFePO4 so that active material it
Between form conductive network structure, the foundation of network structure is issued to corresponding effect in specific conductive agent content, works as conductive agent
During more than the content, the influence of the change of conductive agent content to the high rate performance of LiFePO4 mainly by reduce active material with
Contact impedance between collector realizes, so the present invention is mainly by the basis of conductive agent total content is constant,
Conductive network structure between equilibrium contact impedance and active material, the conductive agent proportioning being optimal, so as to reduce positive pole material
The internal resistance of material so that LiFePO4 high rate performance improves.So as to solve conventional method by excessive addition conductive electrode to improve
The problem of LiFePO4 high rate performance.
The double-deck iron phosphate lithium positive pole piece prepared using the inventive method, compared to traditional battery for being uniformly distributed conductive agent
High rate performance, which has, to be obviously improved, it is achieved thereby that on the premise of conductive agent total content is not changed, reduces battery polarization effect
Should, LiFePO4 high rate performance is improved, while the cycle performance of the product is also more excellent.
Brief description of the drawings
Fig. 1 is the performance comparison figure after bilayer provided in an embodiment of the present invention coats lithium iron phosphate positive material before modified.
Embodiment
Below will by embodiment, the present invention is further described, following experiments are intended merely to more succinct explanation sheet
Invention, is not limited the content.
Embodiment is the description detailed to each sport technique segment of the present invention, therefore the condition on being limited in right is being implemented
All should there are restriction or even further restriction in detail, such as detailed restriction to LiFePO4 in example.
Embodiment 1:
The anode pole piece includes:Collector, first layer active material coating on a current collector is coated, and coated on
The second layer active material coating of one layer of surface of active material.
The collector is that general commercial aluminium foil its average thickness is 19 μm;
The first layer active material coating is counted in parts by weight, by 7.5 parts of SP, 82.5 parts of LiFePO4s, 10 parts of PVDF
It is prepared;
Wherein, SP is the conductive agent that D50 is 50nm, and capacity is up to 155mAh under LiFePO4 average grain diameter 500nm, 0.1C
g-1, PVDF chemical compositions are polyvinyl chloride, as first kind binding agent.
The second layer active material coating is counted in parts by weight, by 2.5 parts of SP, 87.5 parts of LiFePO4s, 10 parts of PVDF
It is prepared.
Wherein, SP, LiFePO4 and PVDF are consistent with the composition in first coating.
Preparation method is as follows:
(1) first, according to the ratio of above-mentioned parts by weight, in the nmp solution that PVDF is dissolved in, NMP and total solids are made
Amount is than being 3:1 prepares the slurry that viscosity is 12000Pa.S, is stirred, it is substantially soluble in nmp solution, by SP and phosphorus
Sour iron lithium uses dry-mixed mixer, is sufficiently mixed 16 hours, and mixed material is divided 4 times, is added within 2 hours per minor tick above-mentioned
In nmp solution, after the addition of all active materials enters NMP, solution is thoroughly mixed 24 hours.Mixed slurry is applied
Spread on aluminium foil, coating thickness is 15 μm, moves into oven for drying.
(2) above-mentioned same method prepares coating slurry is used so that NMP is 4 with solids content ratio:1 viscosity is
8000Pa.S coating paste, when first coating is dried to and can not voluntarily flowed containing a small amount of NMP and slurry, by second layer slurry
Coated on first layer pulp surface, coating thickness is 15 μm, and roll-in is carried out after drying.Obtain double coating iron phosphate lithium positive pole poles
Piece.
There is no to embody the composition that limits in claim in above-described embodiment, and in preparation process several protrusions details
Conductive agent percentage composition is more than the conductive agent hundred in second layer active material in feature, such as viscosity, and first layer active material
Divide content.Simultaneously following condition limitations please be replenished described in the selection of above-described embodiment in two layers of active material, phosphoric acid
For iron lithium using particle diameter between 500~2000nm, tap density is 1.35~1.65g/cm3Between nanoscale or submicron order phosphorus
Sour iron lithium microballoon, its gram volume are 145~175mAh/g, and first charge-discharge efficiency is 98.0~99.9%.
Comparative example 1:
It is using with pulping process and coating process same as Example 1, difference:Coating is expected by 5 parts of SP, 85
Part LiFePO4,10 parts of PVDF are prepared, and one layer of active material is only coated in comparative example, and coating thickness is 30 μm.
Performance test:
Respectively using the positive plate prepared by embodiment 1 and comparative example 1 as positive pole, lithium piece is prepared into 2032 types for negative pole and buckled
Electricity, two battery multiplying powers and cycle performance are tested using blue electric system, test result is as shown in Figure 1.
By in Fig. 1 it is observed that with comparative example 1 commonsense method prepare iron phosphate lithium positive pole piece compared with, the present invention
Iron phosphate lithium positive pole piece prepared by the double-deck coating of preparation, has in high rate charge-discharge performance and is significantly improved.
Embodiment 2:
Difference from Example 1 is
First layer active material coating is counted in parts by weight, by 5 parts of SP and 2.5 part of CNTs, 82.5 parts of LiFePO4s,
10 parts of PVDF are prepared;
The CNT is that length is 10-20 microns, the Ω .cm of powder conductance≤70.
Second layer active material coating is counted in parts by weight, by 2 parts of SP and 1.5 part of CNTs, 86.5 parts of LiFePO4s,
10 parts of PVDF are prepared.
Embodiment 3:
Difference from Example 1 is
First layer active material coating is counted in parts by weight, by 7 parts of SP and 1 part of graphenes, 83 parts of LiFePO4s, and 10 parts
PVDF is prepared;
The graphene is that particle diameter distribution is 3-5 μm, and powder conductance is≤10 Ω .cm.
Second layer active material coating is counted in parts by weight, by 3 parts of SP and 1 part of graphenes, 86 parts of LiFePO4s, and 10 parts
PVDF is prepared.
Comparative example 2:
Each composition is counted in parts by weight in positive electrode coating, content:85 parts of LiFePO4,1 part of graphene, 4 parts
SP and 10 part of PVDF;Positive pole piece of lithium iron phosphate battery is prepared with embodiment 1 in preparation method.
Comparative example 3:
Raw materials by weight portion meter in positive electrode material layer, forms and is:85 parts of LiFePO4,1 part of CNT, 4
SP and 10 part of the PVDF of part;Positive pole piece of lithium iron phosphate battery is prepared with embodiment 1 in preparation method.
Application examples
The anode pole piece prepared by above-described embodiment 1 and comparative example 2,3, button electricity is prepared into, lithium piece is negative pole, and barrier film makes
With polyethylene, bath composition is 1.0M LiPF6inEC:DMC:EMC=1:1:1Vol%, and in 2.7V-4.2V voltage model
In enclosing, test respectively under 0.1C, 0.2C, 0.5C, 1.0C, 2.0C multiplying power and carry out charge-discharge test.Test structure such as table 1 below institute
Show.
Table 1:
There is above-mentioned table 1 to understand:Under 0.1C, 0.2C, 0.5C multiplying power, three kinds of pole piece discharge capacities are more or less the same, and work as multiplying power
When being increased to 1.0C, 2.0C, the capacity of embodiment 1 is substantially better than comparative example 2 and the pole piece of comparative example 3, illustrates the method system of embodiment 1
Standby LiFePO4 high rate performance is more excellent.
It can be seen that the double-deck lithium iron phosphate positive material pole piece prepared using method of modifying of the present invention, compared to containing identical conduction
The common LiFePO4 pole piece of agent, its battery polarization are greatly lowered so that the high rate performance of LiFePO4 have it is bright
Aobvious raising.The cycle performance of the product is excellent simultaneously.
Claims (10)
- A kind of 1. lithium iron phosphate battery anode active material, it is characterised in that two layers of active material, first layer active material, And the second layer active material coated on first layer surface of active material;The first layer active material is counted in parts by weight, by 80~95 parts of lithium iron phosphate positive material, 3~12 parts of conduction Agent, 3~10 parts of first kind binding agent composition;The second layer active material is counted in parts by weight, by 85~98 parts of lithium iron phosphate positive material, 1~8 part of conduction Agent, 5~8 parts of the second class binding agent composition.
- 2. lithium iron phosphate battery anode active material as claimed in claim 1, it is characterised in that:Two layers of active material In, for LiFePO4 using particle diameter between 500~2000nm, tap density is 1.35~1.65g/cm3Between nanoscale or Asia Micron order LiFePO4 microballoon, its gram volume are 145~175mAh/g, and first charge-discharge efficiency is 98.0~99.9%.
- 3. lithium iron phosphate battery anode active material as claimed in claim 1, it is characterised in that:First layer, second layer activity What the conductive agent in material may be the same or different be selected from graphene, the one or more in SP conductive agents, acetylene black, CNT It is compound.
- 4. lithium iron phosphate battery anode active material as claimed in claim 1, it is characterised in that:The first layer active material In conductive agent and second layer active material in conductive agent be 1.1 in mass ratio:1~5:1, wherein led in first layer active material Electric agent content is more than the conductive agent content in second layer active material.
- 5. lithium iron phosphate battery anode active material as claimed in claim 1, it is characterised in that:First binding agent is poly- The copolymer of vinylidene or Kynoar-hexafluoropropene, its molecular weight is between 5000~20000;Second binding agent is selected from polyvinyl chloride (PVC) or Kynoar (PVDF).
- 6. lithium iron phosphate battery anode active material as claimed in claim 1, it is characterised in that:The first coating thickness with Second coating thickness ratio is 3:1~1:5.
- A kind of 7. preparation method of the described lithium iron phosphate battery anode active material described in claim 1, it is characterised in that:(1) the first binding agent is dissolved in nmp solution, be sufficiently mixed LiFePO4 and conductive agent according still further to aforementioned proportion, mixed Mixed liquor is added in the nmp solution of the first binding agent of dissolving several times after conjunction, first 5~8h of ultrasonic disperse, then is put in stirring 36~48h is sufficiently stirred in device, that is, obtains slurry 1, that is, obtains first layer active material;(2) the second binding agent is dissolved in nmp solution, be sufficiently mixed LiFePO4 and conductive agent according still further to aforementioned proportion, mixed Mixed liquor is added in the nmp solution of the second binding agent of dissolving several times after conjunction, first 5~8h of ultrasonic disperse, then is put in stirring 24~36h is sufficiently stirred in device, that is, obtains slurry 2, the slurry 2 prepared is coated on first layer surface of active material.
- 8. the preparation method of the described lithium iron phosphate battery anode active material as described in claim 7, it is characterised in that:Institute 4~8 additions of LiFePO4 and conductive agent mixed solution point are stated, addition every time is separated by 2~3h.
- 9. the preparation method of the described lithium iron phosphate battery anode active material as described in claim 7, it is characterised in that:Slurry viscosity is 5000~15000Pa.S in the first layer active material solution;Slurry viscosity is 1000~10000Pa.S in the second layer active material solution.
- A kind of 10. application of the described lithium iron phosphate battery anode active material described in claim 1, it is characterised in that:Institute State lithium iron phosphate battery anode active material and be used to prepare lithium iron phosphate positive material pole piece applied in lithium ion battery.
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