CN106159265A - The preparation method of the anode slurry of lithium iron phosphate battery of graphene-containing combined conductive agent - Google Patents
The preparation method of the anode slurry of lithium iron phosphate battery of graphene-containing combined conductive agent Download PDFInfo
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- CN106159265A CN106159265A CN201610822426.4A CN201610822426A CN106159265A CN 106159265 A CN106159265 A CN 106159265A CN 201610822426 A CN201610822426 A CN 201610822426A CN 106159265 A CN106159265 A CN 106159265A
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- graphene
- lifepo4
- conductive agent
- iron phosphate
- lithium iron
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- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01M—PROCESSES OR MEANS, e.g. BATTERIES, FOR THE DIRECT CONVERSION OF CHEMICAL ENERGY INTO ELECTRICAL ENERGY
- H01M4/00—Electrodes
- H01M4/02—Electrodes composed of, or comprising, active material
- H01M4/36—Selection of substances as active materials, active masses, active liquids
- H01M4/58—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
-
- 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
-
- 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
-
- 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
-
- 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
- H01M4/362—Composites
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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
-
- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01M—PROCESSES OR MEANS, e.g. BATTERIES, FOR THE DIRECT CONVERSION OF CHEMICAL ENERGY INTO ELECTRICAL ENERGY
- H01M4/00—Electrodes
- H01M4/02—Electrodes composed of, or comprising, active material
- H01M4/62—Selection of inactive substances as ingredients for active masses, e.g. binders, fillers
- H01M4/624—Electric conductive fillers
- H01M4/625—Carbon or graphite
-
- 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 provides the preparation method of the anode slurry of lithium iron phosphate battery of a kind of graphene-containing combined conductive agent, and the method includes: LiFePO4, SP and Graphene are dried process respectively；LiFePO4, SP, Graphene and bonding agent is taken according to corresponding mass score another name；The LiFePO4 weighed is mixed homogeneously with SP, Graphene；The bonding agent weighed is configured to binder solution with solvent NMP；By the LiFePO4 of gained, SP, the compounding substances average mark 2 of Graphene～4 batches, and it is dividedly in some parts in binder solution, is stirred, and adds appropriate solvent NMP, obtain the slurry that viscosity is 5000 10000cP.The present invention can improve the electric conductivity of material, strengthens cycle performance of battery.
Description
Technical field
The present invention relates to field of lithium, just especially relate to the ferric phosphate lithium cell of a kind of graphene-containing combined conductive agent
The preparation method of pole slurry.
Background technology
Ferric phosphate lithium cell, because of advantages such as high security, long-life, low price, environmental protection, is sent out at power and energy storage field
Wave important function.But the low conductivity (10 of LiFePO4-9S/cm) and low ion diffusion rates causes its low specific capacity, limit
Its use；In cell fabrication processes, add amount of conductive agent, the most effectively contact between conductive particle and fill full activity
The space of material, forms conductive network, to improve the electrical property of lithium ion battery in active material.
The most extremely ion and electron mixed conductor, electron conduction is relevant with positive conductive quality, and particle passes
The property led is relevant with the pore volume of positive pole, and many hollow structures can provide the storage place of electrolyte, provides buffering for electrode fast reaction
Ion source, conductive agent is in the electric conductivity of the effect mainly raising positive pole of positive pole.Conductive agent adds among positive electrode active materials,
Through dispersed, conductive agent is fully contacted with active substance, can reduce electrode polarization in cyclic process, is just improving
The specific capacity of pole material and cycle performance.
Lithium ion battery conductive agent mainly has granular conductive agent and threadiness conductive agent, wherein one-component conductive agent such as second
Acetylene black, white carbon black, Delanium and native graphite, metallic fiber, CNT etc..Granular conductive agent low price, user
Just, it is the most conventional conductive agent.Threadiness conductive agent has bigger draw ratio, advantageously forms conductive net, can effectively carry
Caking property between high positive electrode and between positive electrode and collector, improves the energy density of battery, easily forms conduction
Network is two factors that threadiness conductive agent is superior to granule conductive agent with serving as physical binder.It is disadvantageous in that fibre
Dimension shape conductive agent is owing to being long fiber, less with positive active material contact point, not as good as granular conductive agent, by itself and granule
Shape conductive agent is combined, and can bring out the best in each other.
Compared with one-component conductive agent, double-component conductive agent can utilize the most excellent of two kinds or two or more conductive agent
Gesture, forms cooperative effect.There are some researches show, in SP (conductive black) with KS6 combined conductive agent, the total consumption of conductive agent is 8%
(wt%) time, along with the increase of SP content, the energy density of combined conductive agent increases, and the sheet resistance of electrode reduces, although
The diffusion rate of particle reduces, but the rate charge-discharge performance of electrode is improved, and shows the shape paired electrode of conductive channel
Performance have a great impact, two kinds of conductive agent components, when a suitable ratio, have than one-component conductive agent and more preferably follow
Ring performance.Although conductive agent usage amount is few, be the important component part of lithium ion battery, its kind, shape, specific surface area,
Dispersive property affects the electrical property of battery, by different conductive agent compound uses, reaches the emphasis institute that synergy is research
?.
Summary of the invention
It is an object of the invention to: the problem existed for prior art, it is provided that a kind of graphene-containing combined conductive agent
The preparation method of anode slurry of lithium iron phosphate battery, solves the not enough problem of conventional conductive agent electric conductivity.
The goal of the invention of the present invention is achieved through the following technical solutions:
The preparation method of the anode slurry of lithium iron phosphate battery of a kind of graphene-containing combined conductive agent, it is characterised in that should
Method includes:
LiFePO4, SP and Graphene are dried process respectively；
LiFePO4, SP, Graphene and bonding agent, wherein LiFePO4 mass ratio is taken according to corresponding mass score another name
92%～95%, SP mass ratio is 1%～3%, and Graphene mass ratio is 0.5%～1.5%, bonding agent mass ratio be 2%～
4%, it is 40%～45% to weigh solvent NMP (N-Methyl pyrrolidone) according to the mass fraction of solute；
The LiFePO4 weighed is mixed homogeneously with SP, Graphene；
The bonding agent weighed is configured to binder solution with solvent NMP；
By the LiFePO4 of gained, SP, the compounding substances average mark 2 of Graphene～4 batches, and it is molten to be dividedly in some parts binding agent
In liquid, it is stirred, and adds appropriate solvent NMP, obtain the slurry that viscosity is 5000-10000cP.
As further technical scheme, during dried, LiFePO4 powder is toasted under the conditions of 110 DEG C～140 DEG C 3
～5h.
As further technical scheme, during dried, SP and Graphene are toasted 6～10h at 100 DEG C～130 DEG C.
As further technical scheme, the LiFePO4 weighed is mixed homogeneously with SP, Graphene, during mixing, environment
Temperature controls at≤35 DEG C, and humid control is at≤25%RH.
As further technical scheme, during mixing, use LiFePO4 and SP, Graphene in double planetary mixer
Mix homogeneously 1～2h, controls blender revolution 10～20rpm, rotation 100～200rpm.
As further technical scheme, when the bonding agent weighed is configured to binder solution with solvent NMP, environment temperature
Degree controls at≤35 DEG C, and humid control is at≤25%RH.
As further technical scheme, during preparation adhesive solution, use and bonding agent is stirred at double-planet with solvent NMP
Mix mix homogeneously 3～5h in machine, control blender revolution 20～30rpm, rotation 1000～1500rpm.
As further technical scheme, LiFePO4, SP, the compounding substances of Graphene are joined in binder solution
When being stirred, ambient temperature controls at≤35 DEG C, and humid control is at≤25%RH.
As further technical scheme, LiFePO4, SP, the compounding substances of Graphene are joined in binder solution
When being stirred, use double planetary mixer, and control to revolve round the sun 25～40rpm, rotation 1000～2000rpm.
As further technical scheme, every batch of LiFePO4, SP, the compounding substances of Graphene join binder solution
In, all need to stir 20～30min, then after adding appropriate solvent NMP, be stirred for 2-3h.
Compared with prior art, the present invention, in lithium iron phosphate cathode slurry preparation process, uses Graphene and SP (conduction
White carbon black) combined conductive agent, Graphene is laminated structure, and each carbon atom has the electronics of a non-bonding, electronics in Graphene
Movement velocity reached the 1/300 of the light velocity, be the most superior conductive agent, the laminated structure of Graphene determine Graphene with
The contact point of active substance is inadequate, and by Graphene and granular conductive black compound use, conductive black is filled in active matter
In the middle of matter and flake graphite alkene, add the contact point of conductive agent and active substance, the electric conductivity of combination electrode can be improved, and then
Improve lithium ion battery electrical property.
Accompanying drawing explanation
Fig. 1 is the fabrication processing figure of the present invention.
Detailed description of the invention
The present invention is described in detail with specific embodiment below in conjunction with the accompanying drawings.
Embodiment
Graphene is the graphite material of a kind of single or multiple lift, and in the Graphene of monolayer, each carbon atom has one
The electronics of non-bonding, in Graphene, the movement velocity of electronics has reached the 1/300 of the light velocity, considerably beyond electronics at general conductor
In movement velocity, there is good electric conductivity.Graphene can improve the electric conductivity of both positive and negative polarity as lithium ion battery conductive agent
Can, significantly improve the charge-discharge performance of battery and the efficiency of battery and cycle life, be with a wide range of applications.
The present invention uses to combine Graphene with conductive black and prepares lithium ion cell positive slurry as combined conductive agent
Material, with graphite as negative pole, makes lithium ion battery.Granular conductive black is filled mutually with flake graphite alkene, forms conduction
Networking, is favorably improved the cycle performance of battery.
As it is shown in figure 1, the present invention provides the slurry-stirring process of a kind of graphene composite conductive agent LiFePO4, including walking as follows
Rapid:
(1) each raw material (LiFePO4, SP, Graphene) is dried process.By LiFePO4 powder at 110 DEG C～140
3～5h are toasted under the conditions of DEG C；Conductive agent (SP and Graphene) toasts 6～10h at 100 DEG C～130 DEG C.
(2) LiFePO4, SP, Graphene, binding agent, solvent NMP, wherein LiFePO4 mass ratio are weighed according to mass ratio
92%～95%, SP mass ratio is 1%～3%, and bonding agent mass ratio is 2%～4%, Graphene mass ratio be 0.5%～
1.5%；It is 40%～45% to weigh solvent NMP with the mass fraction of solute.
(3) LiFePO4 in step (2) is mixed homogeneously in double planetary mixer with SP, Graphene 1-2h.Environment
Temperature controls at≤35 DEG C, and humid control is at≤25%RH；Revolution 10～20rpm, rotation 100～200rpm.
(4) by the raw material binding agent in step (2), solvent NMP, be configured to binder solution, ambient temperature control≤
35 DEG C, humid control is at≤25%RH；During preparation, in double planetary mixer mix, revolution 20～30rpm, rotation 1000～
1500rpm；Time 3～5h.
(5) by the LiFePO4 of gained, SP, the compounding substances average mark 2 of Graphene～4 batches of (the present embodiment in step (3)
It is divided into 3 batches), after first adds the binder solution in step (4), it is stirred 20～30min；Then add second batch,
And stir；Until adding last batch of, adding appropriate solvent the most again, stirring 2～3h, obtaining viscosity is 5000-10000cP's
Slurry.During omnidistance stirring, ambient temperature controls at≤35 DEG C, and humid control is at≤25%RH；Stirring uses double planetary mixer,
Control revolution 25～40rpm, rotation 1000～2000rpm.
The foregoing is only presently preferred embodiments of the present invention, not in order to limit the present invention, it is noted that all
Any amendment, equivalent and the improvement etc. made within the spirit and principles in the present invention, should be included in the guarantor of the present invention
Within the scope of protecting.
Claims (10)
1. the preparation method of the anode slurry of lithium iron phosphate battery of a graphene-containing combined conductive agent, it is characterised in that the party
Method includes:
LiFePO4, SP and Graphene are dried process respectively；
Take LiFePO4, SP, Graphene and bonding agent according to corresponding mass score another name, wherein LiFePO4 mass ratio 92%～
95%, SP mass ratio is 1%～3%, and Graphene mass ratio is 0.5%～1.5%, and bonding agent mass ratio is 2%～4%, presses
It is 40%～45% to weigh solvent NMP according to the mass fraction of solute；
The LiFePO4 weighed is mixed homogeneously with SP, Graphene；
The bonding agent weighed is configured to binder solution with solvent NMP；
By the LiFePO4 of gained, SP, the compounding substances average mark 2 of Graphene～4 batches, and it is dividedly in some parts binder solution
In, it is stirred, and adds appropriate solvent NMP, obtain the slurry that viscosity is 5000-10000cP.
The preparation side of the anode slurry of lithium iron phosphate battery of a kind of graphene-containing combined conductive agent the most according to claim 1
Method, it is characterised in that during dried, toasts 3～5h under the conditions of 110 DEG C～140 DEG C by LiFePO4 powder.
The preparation side of the anode slurry of lithium iron phosphate battery of a kind of graphene-containing combined conductive agent the most according to claim 1
Method, it is characterised in that during dried, toasts 6～10h by SP and Graphene at 100 DEG C～130 DEG C.
The preparation side of the anode slurry of lithium iron phosphate battery of a kind of graphene-containing combined conductive agent the most according to claim 1
Method, it is characterised in that mixed homogeneously with SP, Graphene by the LiFePO4 weighed, during mixing, ambient temperature controls≤35
DEG C, humid control is at≤25%RH.
The preparation side of the anode slurry of lithium iron phosphate battery of a kind of graphene-containing combined conductive agent the most according to claim 1
Method, it is characterised in that during mixing, uses and LiFePO4 mixs homogeneously with SP, Graphene in double planetary mixer 1～2h,
Control blender revolution 10～20rpm, rotation 100～200rpm.
The preparation side of the anode slurry of lithium iron phosphate battery of a kind of graphene-containing combined conductive agent the most according to claim 1
Method, it is characterised in that when the bonding agent weighed is configured to binder solution with solvent NMP, ambient temperature controls at≤35 DEG C,
Humid control is at≤25%RH.
The preparation side of the anode slurry of lithium iron phosphate battery of a kind of graphene-containing combined conductive agent the most according to claim 1
Method, it is characterised in that during preparation adhesive solution, uses and bonding agent mixs homogeneously with solvent NMP in double planetary mixer 3
～5h, control blender revolution 20～30rpm, rotation 1000～1500rpm.
The preparation side of the anode slurry of lithium iron phosphate battery of a kind of graphene-containing combined conductive agent the most according to claim 1
Method, it is characterised in that LiFePO4, SP, the compounding substances of Graphene are joined when being stirred in binder solution, environment
Temperature controls at≤35 DEG C, and humid control is at≤25%RH.
The preparation side of the anode slurry of lithium iron phosphate battery of a kind of graphene-containing combined conductive agent the most according to claim 1
Method, it is characterised in that LiFePO4, SP, the compounding substances of Graphene are joined when being stirred in binder solution, uses
Double planetary mixer, and control to revolve round the sun 25～40rpm, rotation 1000～2000rpm.
The preparation of the anode slurry of lithium iron phosphate battery of a kind of graphene-containing combined conductive agent the most according to claim 1
Method, it is characterised in that every batch of LiFePO4, SP, the compounding substances of Graphene join in binder solution, all need to stir 20
～30min, then after adding appropriate solvent NMP, it is stirred for 2-3h.
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| CN201610822426.4A CN106159265B (en) | 2016-09-14 | 2016-09-14 | The preparation method of the anode slurry of lithium iron phosphate battery of containing graphene combined conductive agent |
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| CN201610822426.4A CN106159265B (en) | 2016-09-14 | 2016-09-14 | The preparation method of the anode slurry of lithium iron phosphate battery of containing graphene combined conductive agent |
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Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN106784679A (en) * | 2016-12-12 | 2017-05-31 | 江西安驰新能源科技有限公司 | A kind of lithium iron phosphate cathode slurry and preparation method thereof |
| CN107093724A (en) * | 2017-04-27 | 2017-08-25 | 柳州豪祥特科技有限公司 | The preparation method of anode material of lithium battery |
| CN108199042A (en) * | 2018-01-09 | 2018-06-22 | 河北工业大学 | A kind of preparation method of spherical LiFePO 4 mixed type pole piece |
| CN113036085A (en) * | 2021-03-26 | 2021-06-25 | 湖北亿纬动力有限公司 | Positive pole piece and preparation method and application thereof |
Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103682413A (en) * | 2013-12-27 | 2014-03-26 | 山东精工电子科技有限公司 | High-rate long-cycle-life lithium iron phosphate battery and preparation method thereof |
| CN103811764A (en) * | 2014-02-21 | 2014-05-21 | 合肥国轩高科动力能源股份公司 | Preparation method of graphene dry powder for LFP (lithium ferric phosphate) anode paste |
| CN105406070A (en) * | 2015-12-18 | 2016-03-16 | 山东精工电子科技有限公司 | Preparation method of lithium ion battery positive pole size |
-
2016
- 2016-09-14 CN CN201610822426.4A patent/CN106159265B/en not_active Expired - Fee Related
Patent Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103682413A (en) * | 2013-12-27 | 2014-03-26 | 山东精工电子科技有限公司 | High-rate long-cycle-life lithium iron phosphate battery and preparation method thereof |
| CN103811764A (en) * | 2014-02-21 | 2014-05-21 | 合肥国轩高科动力能源股份公司 | Preparation method of graphene dry powder for LFP (lithium ferric phosphate) anode paste |
| CN105406070A (en) * | 2015-12-18 | 2016-03-16 | 山东精工电子科技有限公司 | Preparation method of lithium ion battery positive pole size |
Cited By (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN106784679A (en) * | 2016-12-12 | 2017-05-31 | 江西安驰新能源科技有限公司 | A kind of lithium iron phosphate cathode slurry and preparation method thereof |
| CN106784679B (en) * | 2016-12-12 | 2019-11-19 | 江西安驰新能源科技有限公司 | A kind of lithium iron phosphate cathode slurry and preparation method thereof |
| CN107093724A (en) * | 2017-04-27 | 2017-08-25 | 柳州豪祥特科技有限公司 | The preparation method of anode material of lithium battery |
| CN108199042A (en) * | 2018-01-09 | 2018-06-22 | 河北工业大学 | A kind of preparation method of spherical LiFePO 4 mixed type pole piece |
| CN113036085A (en) * | 2021-03-26 | 2021-06-25 | 湖北亿纬动力有限公司 | Positive pole piece and preparation method and application thereof |
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