CN108281640A - Proportioning process, based lithium-ion battery positive plate and the lithium ion battery of lithium ion battery anode glue size - Google Patents
Proportioning process, based lithium-ion battery positive plate and the lithium ion battery of lithium ion battery anode glue size Download PDFInfo
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- 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
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- 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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- H01M4/00—Electrodes
- H01M4/02—Electrodes composed of, or comprising, active material
- H01M4/13—Electrodes for accumulators with non-aqueous electrolyte, e.g. for lithium-accumulators; Processes of manufacture thereof
- H01M4/136—Electrodes based on inorganic compounds other than oxides or hydroxides, e.g. sulfides, selenides, tellurides, halogenides or LiCoFy
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- 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
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Abstract
The invention belongs to technical field of lithium ion, it is related to a kind of proportioning process of lithium ion battery anode glue size, based lithium-ion battery positive plate and lithium ion battery.The proportioning process of the lithium ion battery anode glue size of the present invention, includes the following steps:(a) progress of positive active material, conductive auxiliary agent, dispersant and thickener is dry-mixed, obtain mixed powder;(b) solvent is added, mixing obtains the primary slurry that solid content is 82wt%~85wt%;(c) solvent is added, mixing obtains the secondary slurries that solid content is 66wt%~68wt%;(d) solvent is added, mixing obtains the three-level slurry that solid content is 56wt%~59wt%, to which lithium ion battery anode glue size be made.Present invention process is simple, easy to operate, can significantly shorten the dispensing time, improves utilization rate of equipment and installations, while batch mixing is uniform, improves the dispersibility, consistency and fineness of slurry.
Description
Technical field
The invention belongs to technical field of lithium ion, in particular to a kind of matching for lithium ion battery anode glue size
Material technique, based lithium-ion battery positive plate and lithium ion battery.
Background technology
In existing secondary cell system, no matter from development space, or from the service life, than energy, operating voltage and from
From the point of view of the technical indicators such as discharge rate, lithium ion battery is all current most competitive secondary cell.Lithium ion battery has work
Make that voltage is high, energy density is big, has extended cycle life, the advantages that self-discharge rate is small, environmentally protective, becomes becoming for secondary cell development
Gesture;Be widely used to the power supply of the portable electricity consuming products such as wireless telecommunications, digital camera, laptop, and as aerospace,
There is wide answer in terms of the special application fields such as defence and military, electric vehicle, battery-operated motor cycle, field work, submarine power supply
Use foreground.
The preparation of slurry is the critical process of lithium ion battery production link, and the performance of electrode slurry is to lithium ion battery
Performance has important influence.Each component disperses more uniform in electrode slurry, and pole piece just has better processing performance, and electricity
The distribution of impedance of pole everywhere is uniform, in charge and discharge the effect of active material can play bigger, be more advantageous to promotion battery
Performance.
Traditional anode sizing agent preparation mostly uses wet-mixing greatly, and long the time required to the method, utilization rate of equipment and installations is low, production capacity phase
To relatively low, and slurry dispersibility and consistency are poor.The dry mixing process risen in the recent period has become research hotspot, which can carry
Polymolecularity and production efficiency.But current dry mixing process, there is still a need for longer time, entire blending process needs ten small
When or more than, production efficiency is relatively low, causes utilization rate of equipment and installations low;In addition, when closing slurry, the universal solid content of slurry is relatively low or inclined
Height is unfavorable for dispersibility and the improvement of consistency of slurry, is unfavorable for the promotion of the overall performance of final anode pole piece obtained.
In consideration of it, special propose the present invention.
Invention content
The first object of the present invention is to provide a kind of proportioning process of lithium ion battery anode glue size, simple for process, easy
Operation, can significantly shorten the dispensing time, improve utilization rate of equipment and installations, while batch mixing is uniform, effectively improve slurry dispersibility,
Consistency and fineness.
The second object of the present invention is to provide a kind of based lithium-ion battery positive plate, and uniformity is good, and stability is strong, qualification rate
Height has the advantages that good cycling stability, safe and at low cost.
The third object of the present invention is to provide a kind of lithium ion battery, which includes above-mentioned lithium ion battery
Positive plate has the advantages that good cycling stability, safe and at low cost.
To achieve the above object, the technical solution adopted by the present invention is:
According to an aspect of the present invention, the present invention provides a kind of proportioning process of lithium ion battery anode glue size, including
Following steps:
(a) progress of positive active material, conductive auxiliary agent, dispersant and thickener is dry-mixed, obtain mixed powder;
(b) solvent is added, mixing obtains the primary slurry that solid content is 82wt%~85wt%;
(c) solvent is added, mixing obtains the secondary slurries that solid content is 66wt%~68wt%;
(d) add solvent, mixing obtains the three-level slurry that solid content is 56wt%~59wt%, to be made lithium from
Sub- battery anode slurry.
As further preferred technical solution, in step (a), the speed of dry-mixed stirring is 15~25r/min of revolution, time
For 25~35min.
As further preferred technical solution, in step (b), 8 first are mixed with the speed for the 15~25r/min that revolves round the sun~
15min, then 110~130min is mixed with the speed for the 30~45r/min that revolves round the sun.
As further preferred technical solution, in step (c), 8 first are mixed with the speed for the 15~25r/min that revolves round the sun~
15min, then 60~100min is mixed with the speed of revolve round the sun 30~45r/min, 800~1500r/min of rotation.
As further preferred technical solution, in step (d), 8 first are mixed with the speed for the 15~25r/min that revolves round the sun~
15min, then 25~40min is mixed with the speed of revolve round the sun 30~45r/min, 800~1500r/min of rotation.
Further include the steps that de-bubble as further preferred technical solution, after obtaining three-level slurry, revolution 25~
25~35min of de-bubble is carried out under the speed of 35r/min, and lithium ion battery anode glue size is made.
As further preferred technical solution, the solid content of the primary slurry is 83wt%~84wt%;The secondary
The solid content of slurry is 67wt%~68wt%;The solid content of the three-level slurry is 57wt%~58wt%.
As further preferred technical solution, in the lithium ion battery anode glue size, positive active material, conduction help
The mass ratio of agent, dispersant and thickener is (94~97):(0.8~1.5):(0.08~0.15):(1~3);
Preferably, the positive active material includes LiFePO4;
Preferably, the conductive auxiliary agent includes conductive black, conductive carbon ball, electrically conductive graphite, carbon nanotube, conductive carbon fibre
Or at least one of graphene;
Preferably, the dispersant includes at least one of polyethylene glycol and polyvinylpyrrolidone;
Preferably, the thickener includes CMC;
Preferably, the solvent includes NMP.
According to another aspect of the present invention, the present invention also provides a kind of based lithium-ion battery positive plates, including anode collection
The slurry of body and the active material layer for being formed in the plus plate current-collecting body surface, the active material layer uses above-described lithium
The proportioning process of ion battery anode sizing agent is made.
According to another aspect of the present invention, the present invention also provides a kind of lithium ion batteries, including above-mentioned lithium-ion electric
Pond positive plate.
Compared with prior art, the beneficial effects of the present invention are:
1, the proportioning process of the lithium ion battery anode glue size of offer of the invention, use is dry-mixed, solvent is added in three times
Mode, be configured to be uniformly dispersed, high-quality slurry, and can realize that the mode of fixed solid content carries out dispensing, shorten and match
Expect the time, achieves preferable mixed effect, improve the dispersing uniformity and stability of slurry, alleviate and deposit in the prior art
The dispensing time it is long, be easy reunite, be not easy uniformly mixed technical problem.
2, the present invention is simple and practicable, is not necessarily to special ancillary equipment, and easy to operate, since the dispensing time is short, batch mixing is uniform, slurry
The fineness of material is improved, and to greatly improve utilization rate of equipment and installations, improves production efficiency, reduces cost, also improves
The quality of pole piece ensures the consistency of battery performance, industrially scalable metaplasia production easy to implement.
3, not only the production time is short by the present invention, and economic efficacy is high, and slurry is mixed very uniformly, and is not easy to precipitate, be avoided
The appearance of agglomeration, improves the performance of slurry so that slurry has good homogeneity, stability and dispersibility;From
And slurry can be smoothed out when preparing positive plate, pole piece qualification rate is high, improves the uniformity of coating, and be obviously improved most
The overall performance of the anode pole piece prepared eventually.Further, the anode pole piece is applied in lithium ion battery, it can
The stability and consistency for improving battery, make lithium ion battery obtained have preferable cyclical stability, can play it is higher
Capacity has a safety feature, and extends the service life of lithium ion battery.
Specific implementation mode
Embodiment of the present invention is described in detail below in conjunction with embodiments and examples, but this field skill
Art personnel will be understood that following embodiments and embodiment are merely to illustrate the present invention, and be not construed as the model of the limitation present invention
It encloses.Based on the embodiments of the present invention, obtained by those of ordinary skill in the art without making creative efforts
Every other embodiment, shall fall within the protection scope of the present invention.The person that is not specified actual conditions, builds according to normal condition or manufacturer
The condition of view carries out.Reagents or instruments used without specified manufacturer is the conventional production that can be obtained by commercially available purchase
Product.
In a first aspect, a kind of proportioning process of lithium ion battery anode glue size is provided at least one embodiment, including
Following steps:
(a) progress of positive active material, conductive auxiliary agent, dispersant and thickener is dry-mixed, obtain mixed powder;
(b) solvent is added, mixing obtains the primary slurry that solid content is 82wt%~85wt%;
(c) solvent is added, mixing obtains the secondary slurries that solid content is 66wt%~68wt%;
(d) add solvent, mixing obtains the three-level slurry that solid content is 56wt%~59wt%, to be made lithium from
Sub- battery anode slurry.
The present invention using it is dry-mixed, solvent is added in three times by the way of, be configured to be uniformly dispersed, high-quality slurry, and energy
It realizes that the mode of fixed solid content carries out dispensing, shortens the dispensing time, achieve preferable mixed effect, improve slurry
Dispersing uniformity and stability, concretely:
First by positive active material, conductive auxiliary agent, dispersant and thickener, these dry powder carry out dry-mixing for a period of time, so
Partial solvent is added afterwards and controls solid content in 82wt%~85wt% or so, mixed state, such state are rubbed to reach dough
It is that most several dry powder can be made to reach uniformly mixed state, a period of time is mixed under such state;It is molten to add part
Agent reduces solid content to 66wt%~68wt% or so, and reaching the state of a wet mixing makes slurry be sufficiently mixed with solvent;Mixing
Partial solvent is added after stirring a period of time reduces solid content to 56wt%~59wt% or so, and tested viscosity is adjusted to work
Skill claimed range;Followed by de-bubble or viscosity is adjusted, reaches application viscosity requirement.
It is above-mentioned it is dry-mixed be by positive active material, conductive auxiliary agent, dispersant and thickener under conditions of without other solvents
It is added at one time, is directly mixed, achieves preferable mixed effect, the dispensing time can in this way shortened, and make
Slurry is more uniform, reduces the bulky grain content of slurry;The thickening dispersion that thickener and dispersant can also be given full play to is made
With.In addition, the range that solvent is added by substep, effectively controls each step solid content, also improves the dissolubility of conductive auxiliary agent,
Reduce the probability that little particle powder agglomerates into bulky grain in a solvent so that the grain size of anode sizing agent is small, it is easier to disperse
Stablize, the electrical efficiency of positive plate can be improved, is conducive to the chemical property for improving battery.Finally de-bubble or viscosity are carried out again
It adjusts, formation is uniformly dispersed, the slurry that stability is good, consistency is good ensure that battery performance while improving efficiency with slurry
Consistency.
It should be noted that above-mentioned solid content is understood by this field conventional sense, such as it is to be understood that with
On the basis of slurry total amount, the shared mass percent of total solid substance therein is solid content.
Optionally, in operating process, positive active material, conductive auxiliary agent, dispersant first have been weighed according to mass ratio calculating
And thickener, and carry out dry-mixed;Then sequentially add solid content 82wt%~85wt% in mass ratio, 66wt%~68wt% and
56wt%~59wt% calculates required solvent, and is mixed successively, and anode sizing agent is made.
In a preferred embodiment, in step (a), the speed of dry-mixed stirring is 15~25r/min of revolution, rotation
For 0r/min, the time is 25~35min;
Preferably, the speed of dry-mixed stirring is 15~20r/min of revolution, switchs to 0r/min certainly, and the time is 28~32min;
It is further preferred that the speed of dry-mixed stirring is revolution 20r/min, switch to 0r/min, time 30min certainly.
Carry out under these conditions it is dry-mixed, i.e., when the rotating speed of dry-mixed period within the above range, can make each substance more
Add sufficient mixing, the thickening peptizaiton of thickener and dispersant can be given full play to, obtain preferable mixed effect, also
Help shorten working hour.
Particular determination is not done for the temperature of dry mixing process, for example, 15 DEG C can be greater than or equal to and be less than or equal to 35 DEG C.
The mixer used for dry mixing process does not do particular determination, for example, can be planetary motion type mixer or row
Luck dynamic formula epicyclic mixer etc..
In a preferred embodiment, in step (b), first with the speed of the 15~25r/min that revolves round the sun, rotation 0r/min
8~15min is mixed, then 110~130min is mixed with the speed of revolve round the sun 30~45r/min, rotation 0r/min;
Preferably, 9~12min is first mixed with the speed of the 15~20r/min that revolves round the sun, rotation 0r/min, then with revolution
115~125min of speed mixing of 30~35r/min, rotation 0r/min;
It is further preferred that 10min is first mixed with the speed of the 20r/min that revolves round the sun, rotation 0r/min, then with revolution
The speed mixing 120min of 35r/min, rotation 0r/min.
Carry out under these conditions dough rub it is mixed, i.e., when dough rub it is mixed during rotating speed within the above range, can make
Each substance more fully mixes, and obtains better mixed effect, helps to improve the dispersibility and stability of anode sizing agent.
Dough is rubbed and sneaks out the temperature of journey and does not do particular determination, for example, 18 DEG C can be greater than or equal to and be less than or wait
In 35 DEG C.
Dough is rubbed and sneaks out the mixer of Cheng Caiyong and does not do particular determination, for example, can be planetary motion type mixer
Or planetary motion type epicyclic mixer etc..
In a preferred embodiment, in step (c), first with the speed of the 15~25r/min that revolves round the sun, rotation 0r/min
Be mixed 8~15min, then with revolve round the sun 30~45r/min, 800~1500r/min of rotation speed be mixed 60~
100min;
Preferably, 9~12min is first mixed with the speed of the 15~20r/min that revolves round the sun, rotation 0r/min, then with revolution
60~90min of speed mixing of 30~35r/min, 900~1200r/min of rotation;
It is further preferred that 10min is first mixed with the speed of the 20r/min that revolves round the sun, rotation 0r/min, then with revolution
The speed mixing 90min of 35r/min, rotation 1000r/min.
Wet mixing is carried out under these conditions, i.e., the rotating speed during wet mixing within the above range, can make each substance more
Add sufficient mixing so that slurry is sufficiently mixed with solvent, obtains better mixed effect, helps to improve point of anode sizing agent
Dissipate property, stability and consistency.
Particular determination is not done for the temperature of wet mixing process, for example, 18 DEG C can be greater than or equal to and be less than or equal to 35 DEG C.
The mixer used for wet mixing process does not do particular determination, for example, can be planetary motion type mixer or row
Luck dynamic formula epicyclic mixer etc..
In a preferred embodiment, in step (d), first with the speed of the 15~25r/min that revolves round the sun, rotation 0r/min
Be mixed 8~15min, then with revolve round the sun 30~45r/min, 800~1500r/min of rotation speed be mixed 25~
40min;
Preferably, 9~12min is first mixed with the speed of the 15~20r/min that revolves round the sun, rotation 0r/min, then with revolution
28~35min of speed mixing of 30~35r/min, 900~1200r/min of rotation;
It is further preferred that 10min is first mixed with the speed of the 20r/min that revolves round the sun, rotation 0r/min, then with revolution
The speed mixing 30min of 35r/min, rotation 1000r/min.
Be diluted adjusting viscosity under these conditions, i.e., the rotating speed during dilution adjusts viscosity within the above range,
Each substance can be made more fully to mix, obtain better mixed effect, be conducive to the adjusting of viscosity, while helping to carry
Dispersibility, storage stability and the consistency of high anode sizing agent.
The temperature that viscosity process is adjusted for dilution does not do particular determination, for example, can be greater than or equal to 18 DEG C and be less than
Or it is equal to 35 DEG C.
The mixer that viscosity process uses is adjusted for dilution and does not do particular determination, for example, can be mixed for planetary motion type
Clutch or planetary motion type epicyclic mixer etc..
In a preferred embodiment, further include the steps that de-bubble, after obtaining three-level slurry, revolution 25~
25~35min of de-bubble is carried out under the speed of 35r/min, and lithium ion battery anode glue size is made.
Preferably, the speed of de-bubble is 25~30r/min of revolution, switchs to 0r/min certainly, and the time is 28~32min;
It is further preferred that the speed of de-bubble is revolution 30r/min, switch to 0r/min, time 30min certainly.
De-bubble is carried out under these conditions, can make mixing evenly, ensures that slurry has better electrical property and Painting effect.
Particular determination is not done for the temperature and pressure of de-bubble, such as can be froth in vacuum, temperature can be more than or wait
In 20 DEG C and it is less than or equal to 35 DEG C.
Under the operating conditions described above, the dispensing time can significantly be shortened, the dispensing time phase with existing 8-10 hour
Than the dispensing time is foreshortened to 4-5 hour, 2 times of improving productivity by the present invention.
In a preferred embodiment, the solid content of the primary slurry is 83wt%~84wt%;The secondary
The solid content of slurry is 67wt%~68wt%;The solid content of the three-level slurry is 57wt%~58wt%;
Preferably, the solid content of primary slurry is 84wt% or so;The solid content of the secondary slurries is 67wt% or so;
The solid content of the three-level slurry is 58wt% or so.
By effectively controlling or fixing the solid content of the slurry of each step, i.e., when the solid content of each step is in above range
It is interior, the mixing uniformity of each step slurry is helped to improve, the dissolubility of conductive auxiliary agent is also contributed to, reduces little particle
Powder easily agglomerates into the probability of bulky grain in a solvent, improves the fineness of slurry, improves the performance of slurry, ensures lithium-ion electric
The performances such as the good cycle in pond, multiplying power, safety, consistent.
In a preferred embodiment, in the lithium ion battery anode glue size, positive active material, conduction help
The mass ratio of agent, dispersant and thickener is (94~97):(0.8~1.5):(0.08~0.15):(1~3);
Preferably, the positive active material includes LiFePO4;
Preferably, the conductive auxiliary agent includes conductive black, conductive carbon ball, electrically conductive graphite, carbon nanotube, conductive carbon fibre
Or at least one of graphene;
Preferably, the dispersant includes at least one of polyethylene glycol and polyvinylpyrrolidone;
Preferably, the thickener includes CMC;
Preferably, the solvent includes NMP.
Excessive restriction is not done for the ratio of each substance in slurry, if the additive amount of each substance meet slurry can
Balance between coating and bond property;Such as can be positive active material, conductive auxiliary agent, dispersant and thickening
The mass ratio of agent is (94~97):(0.8~1.5):(0.08~0.15):(1~3);Can also be positive active material, conduction
The mass ratio of auxiliary agent, dispersant and thickener is (94.5~96.5):(1.0~1.2):(0.1~0.12):(1.5~2);Match
During system, it is added each substance according to actually required ratio, and the content of solvent then can be according to each step in slurry
Determining solid content is added required quantity of solvent.
Optionally, the viscosity of anode sizing agent obtained is 2000~8000mPas.In operating process, can testing size it is viscous
Degree also can adjust viscosity by adjusting the additive amount of solvent, and be adjusted to technological requirement range.
It is understood that the present invention is for each positive active material, solvent, thickener, conductive auxiliary agent and dispersant
Source does not have special limitation, using each raw material well-known to those skilled in the art;Its commercial goods such as may be used,
It can also voluntarily be prepared using preparation method well known to those skilled in the art.
It is further described below for each composition material in slurry:
Positive active material:Positive active material is not done it is specifically limited, as long as active material be can be used for lithium ion
The typical activity substance of the anode of secondary cell.Positive active material is preferably LiFePO4.
Conductive auxiliary agent:Conductive auxiliary agent is not done it is specifically limited, as long as conductive auxiliary agent, which has, electronic conductivity and improves electricity
The conductibility of pole.Conductive auxiliary agent includes carbon material, and conductive auxiliary agent can be for example conductive black, acetylene black, Ketjen black, lead
Electrical carbon ball, electrically conductive graphite, carbon nanotube, conductive carbon fibre or graphene, and the graphite with specific activity substance particle ruler
Very little smaller graphite, these conductive auxiliary agents can be used alone or being applied in combination with their two or more.
Dispersant:Dispersant is not done it is specifically limited, as long as dispersant be used for improve anode sizing agent dispersing uniformity,
Coatability.Such as can be polyethylene glycol, polyvinylpyrrolidone, polyethylene glycol therein may include gathering dispersant
Ethylene glycol 200, polyethylene glycol 400, Macrogol 600, cetomacrogol 1000 etc., polyvinylpyrrolidone may include polyethylene pyrrole
Pyrrolidone K15, PVP K30, polyvinylpyrrolidone K40, polyvinylpyrrolidone K60 etc.;These dispersants
It can be used alone or being applied in combination with their two or more.
Thickener:Thickener is not done it is specifically limited, as long as thickener is used to improve the coatability of anode sizing agent i.e.
It can.Thickener includes water-soluble polymer, and thickener for example can be cellulose-based polymer, such as carboxymethyl cellulose, first
Base cellulose and hydroxy propyl cellulose and their ammonium salt and metal salt.Thickener is preferably sodium carboxymethylcellulose, i.e.,
CMC (Sodium carboxymethlycellulose), appearance are white or yellowish fibrous powder or white powder,
It is odorless, it is tasteless, it is nontoxic, it derives from a wealth of sources, it is at low cost.
Solvent:Solvent is not done it is specifically limited, as long as can dissolve above-mentioned substance, contribute to improve thickener dispersion
Property, the contact between active material and conductive auxiliary agent will not be hindered.The solvent, such as can be N- crassitudes
Ketone, i.e. NMP (N-methyl-2-pyrrolidone), with viscosity is low, chemical stability and thermal stability are good, volatility
Low feature, at low cost, source is wide, and slurry fluidity obtained is good.
Second aspect, provides a kind of based lithium-ion battery positive plate at least one embodiment, including plus plate current-collecting body and
It is formed in the active material layer on the plus plate current-collecting body surface, the slurry of the active material layer uses above-described lithium ion
The proportioning process of battery anode slurry is made.
The third aspect provides a kind of lithium ion battery, including above-mentioned lithium ion battery at least one embodiment
Positive plate.The lithium ion battery further includes negative plate, diaphragm and electrolyte.
It is understood that the present invention does not have the concrete type of plus plate current-collecting body, negative plate, diaphragm and electrolyte
Especially limitation, according to this field conventional selection.
The generation type of active material layer for being formed in plus plate current-collecting body surface is also not particularly limited, using normal
Slurry obtained is coated by the painting process of rule.
There is good homogeneity, stability and dispersibility by anode sizing agent made from the above method, improve slurry
Fineness, can improve the uniformity of painting process, alleviate the prior art easy cracked, pole in battery pole piece coating process
The low technical problem of piece qualification rate, to help to promote the overall performance of the anode pole piece finally prepared.Further,
The positive plate is applied in lithium ion battery, the stability and consistency of battery can be improved, make lithium-ion electric obtained
Pond has preferable cyclical stability, can play higher capacity, have a safety feature, and high rate performance is high, extends lithium-ion electric
The service life in pond has expanded the scope of application of lithium ion battery.
With reference to specific embodiment and comparative example, the invention will be further described.
Embodiment 1
A kind of proportioning process of lithium ion battery anode glue size, includes the following steps:
(a) LiFePO4, conductive black, polyethylene glycol and CMC have been weighed according to mass ratio calculating, and with the 20r/ that revolves round the sun
The speed dry-mixed 30min of progress of min, rotation 0r/min, obtain mixed powder;
(b) NMP is added, 10min is first mixed with the speed of the 20r/min that revolves round the sun, rotation 0r/min, then with the 35r/ that revolves round the sun
The speed mixing 120min of min, rotation 0r/min, obtain the primary slurry that solid content is 83.8wt%, the addition of NMP
By solid content for 83.8wt% based on;
(c) NMP is added, 10min is first mixed with the speed of the 20r/min that revolves round the sun, rotation 0r/min, then with revolution
The speed mixing 90min of 35r/min, rotation 1000r/min, obtain the secondary slurries that solid content is 67.4wt%, NMP's
Addition by solid content for 67.4wt% based on;
(d) NMP is added, 10min is first mixed with the speed of the 20r/min that revolves round the sun, rotation 0r/min, then with revolution
The speed mixing 30min of 35r/min, rotation 1000r/min, obtain the three-level slurry that solid content is 57.9wt%, NMP's
Addition by solid content for 57.9wt% based on;
Then de-bubble is carried out with the speed stirring 30min of the 30r/min that revolves round the sun, rotation 0r/min, is obtaining lithium ion battery just
Pole slurry;
Wherein, the mass ratio of LiFePO4, conductive black, polyethylene glycol and CMC are 96.9:1.0:0.1:2.
Embodiment 2
A kind of proportioning process of lithium ion battery anode glue size, includes the following steps:
(a) LiFePO4, conductive black, polyethylene glycol and CMC have been weighed according to mass ratio calculating, and with the 20r/ that revolves round the sun
The speed dry-mixed 35min of progress of min, rotation 0r/min, obtain mixed powder;
(b) NMP is added, 12min is first mixed with the speed of the 20r/min that revolves round the sun, rotation 0r/min, then with the 35r/ that revolves round the sun
The speed mixing 115min of min, rotation 0r/min, obtain the primary slurry that solid content is 83wt%, the addition of NMP is pressed
Solid content is counted for 83wt%;
(c) NMP is added, 15min is first mixed with the speed of the 20r/min that revolves round the sun, rotation 0r/min, then with revolution
The speed mixing 60min of 35r/min, rotation 1000r/min, obtain the secondary slurries that solid content is 67wt%, and NMP's adds
Enter amount by solid content for 67wt% based on;
(d) NMP is added, 8min is first mixed with the speed of the 20r/min that revolves round the sun, rotation 0r/min, then with revolution
The speed mixing 40min of 35r/min, rotation 1000r/min, obtain the three-level slurry that solid content is 57wt%, and NMP's adds
Enter amount by solid content for 57wt% based on;
Then de-bubble is carried out with the speed stirring 25min of the 30r/min that revolves round the sun, rotation 0r/min, is obtaining lithium ion battery just
Pole slurry;
Wherein, the mass ratio of LiFePO4, conductive black, polyethylene glycol and CMC are 95.85:1.5:0.15:2.5.
Embodiment 3
A kind of proportioning process of lithium ion battery anode glue size, includes the following steps:
(a) LiFePO4, conductive carbon fibre, polyvinylpyrrolidone and CMC have been weighed according to mass ratio calculating, and with public affairs
The speed dry-mixed 30min of progress for turning 25r/min, rotation 0r/min, obtains mixed powder;
(b) NMP is added, 10min is first mixed with the speed of the 15r/min that revolves round the sun, rotation 0r/min, then with the 45r/ that revolves round the sun
The speed mixing 120min of min, rotation 0r/min, obtain the primary slurry that solid content is 85wt%, the addition of NMP is pressed
Solid content is counted for 85wt%;
(c) NMP is added, 10min is first mixed with the speed of the 15r/min that revolves round the sun, rotation 0r/min, then with revolution
The speed mixing 90min of 30r/min, rotation 1500r/min, obtain the secondary slurries that solid content is 68wt%, and NMP's adds
Enter amount by solid content for 68wt% based on;
(d) NMP is added, 10min is first mixed with the speed of the 25r/min that revolves round the sun, rotation 0r/min, then with revolution
The speed mixing 30min of 45r/min, rotation 800r/min, obtain the three-level slurry that solid content is 59wt%, and NMP's adds
Enter amount by solid content for 59wt% based on;
Then de-bubble is carried out with the speed stirring 35min of the 25r/min that revolves round the sun, rotation 0r/min, is obtaining lithium ion battery just
Pole slurry;
Wherein, the mass ratio of LiFePO4, conductive carbon fibre, polyvinylpyrrolidone and CMC are 95.72:1.2:0.08:3.
Embodiment 4
A kind of proportioning process of lithium ion battery anode glue size, with embodiment 1 difference lies in:
(b) NMP is added, 10min is first mixed with the speed of the 15r/min that revolves round the sun, rotation 0r/min, then with the 30r/ that revolves round the sun
The speed mixing 125min of min, rotation 0r/min, obtain the primary slurry that solid content is 83.8wt%, the addition of NMP
By solid content for 83.8wt% based on;
(c) NMP is added, 10min is first mixed with the speed of the 25r/min that revolves round the sun, rotation 0r/min, then with revolution
The speed mixing 80min of 40r/min, rotation 1000r/min, obtain the secondary slurries that solid content is 67.4wt%, NMP's
Addition by solid content for 67.4wt% based on;
(d) NMP is added, 10min is first mixed with the speed of the 20r/min that revolves round the sun, rotation 0r/min, then with revolution
The speed mixing 25min of 30r/min, rotation 1500r/min, obtain the three-level slurry that solid content is 57.9wt%, NMP's
Addition by solid content for 57.9wt% based on;
Remaining is same as Example 1.
Embodiment 5
A kind of proportioning process of lithium ion battery anode glue size, with embodiment 1 difference lies in:
Step (b), (c) and the solid content in (d) are respectively 82.1wt%, 66.2wt% and 56.0wt%;
Remaining is same as Example 1.
Comparative example 1
A kind of proportioning process of lithium ion battery anode glue size, with embodiment 1 difference lies in:
Step (b), (c) and (d) are replaced with:NMP is added, it is mixed with the speed of the 35r/min that revolves round the sun, rotation 1000r/min
Close stirring 150min, obtain the slurry that solid content is 70wt%, the addition of NMP by solid content for 70wt% based on;
Difference lies in NMP is disposably all added this comparative example with embodiment 1.
Comparative example 2
A kind of proportioning process of lithium ion battery anode glue size, with embodiment 1 difference lies in:
Step (b), (c) and the solid content in (d) are respectively 72wt%, 62wt% and 50wt%;
This comparative example with embodiment 1 difference lies in the present invention do not protect by step (b), (c) and the solid content in (d)
In the range of.
Comparative example 3
A kind of proportioning process of lithium ion battery anode glue size, with embodiment 1 difference lies in:
(a) LiFePO4, conductive black, polyethylene glycol and CMC have been weighed according to mass ratio calculating, and with the 35r/ that revolves round the sun
The speed dry-mixed 40min of progress of min, rotation 0r/min, obtain mixed powder;
(b) NMP is added, 5min is first mixed with the speed of the 40r/min that revolves round the sun, rotation 0r/min, then with the 50r/ that revolves round the sun
The speed mixing 150min of min, rotation 0r/min, obtain the primary slurry that solid content is 83.2wt%, the addition of NMP
By solid content for 83.2wt% based on;
(c) NMP is added, 120min is mixed with the speed of the 20r/min that revolves round the sun, rotation 1500r/min, admittedly contained
Amount is the secondary slurries of 66.4wt%, the addition of NMP by solid content for 66.4wt% based on;
(d) NMP is added, 60min is mixed with the speed of the 20r/min that revolves round the sun, rotation 500r/min, obtains solid content
For the three-level slurry of 57.5wt%, the addition of NMP by solid content for 57.5wt% based on;
Difference lies in the rotating speed of each step and operating time be not in the model of the invention protected with embodiment 1 for this comparative example
In enclosing.
Performance test
The test of viscosity and fineness is carried out to anode sizing agent made from embodiment 1-5 and comparative example 1-3 respectively, wherein
Fineness is measured by fineness, and viscosity is the 3.4s at 20 DEG C by Brookfield viscometer- 1Shear rate under measure;So
Each slurry is opened wide at room temperature afterwards and is placed 3 days, the viscosity of each slurry of re-test, and it is calculate by the following formula rate of change in viscosity:
Rate of change in viscosity (%)=(viscosity -1 before viscosity/placement 3 days after placing 3 days) × 100;
Slurry obtained by each embodiment and comparative example is coated on copper foil, positive plate is made by roll-in, cross cutting, it will be positive
Piece winds with diaphragm and negative plate, enters shell, fluid injection, sealing, lithium ion battery is made, each embodiment and comparative example respectively takes 10
Battery, tests its capacity and cycle life, and test result is as shown in table 1.
1 the performance test results of table
As can be seen from Table 1, the obtained size performance performances of 1-5 of the embodiment of the present invention are substantially better than comparative example 1-3 and are starched
Expect performance, the embodiment of the present invention improve anode slurry fineness, viscosity is good, viscosity within the scope of technological requirement, according to
For the preparation-obtained anode sizing agent viscosity of the method for the present invention in 3 days, viscosity change very little maintains the property of original slurry substantially
Matter, is not in sedimentation phenomenon, and size performance is more stable;Meanwhile slurry obtained being coated on plus plate current-collecting body, it is made just
Pole piece is prepared into lithium ion battery by pole piece according still further to prior art, since the lithium ion battery and its pole piece of the present invention use
Above-mentioned slurry, above-mentioned slurry has good electric conductivity and dispersion effect and stability are good so that lithium ion battery obtained
Higher capacity and preferable cyclical stability are played, the service life of lithium ion battery is extended.
In addition, solvent once addition is unfavorable for slurry it can be seen from the comparative analysis of comparative example 1 and embodiment 1
Mixing, the dispersibility of slurry and consistency can be caused to be deteriorated, the bad stability of slurry is susceptible to sedimentation phenomenon;Meanwhile
By comparative example 2 and 3 and embodiment 1 comparative analysis it is found that change operating parameter such as solid content, rotating speed set by each step and
Time etc., said effect is can not achieve, the performance of obtained slurry can be reduced.
Result above can illustrate that proportioning process good mixing effect of the invention, the fineness of slurry is small, and stability is good, no
Easily precipitation, improves the quality of pole piece, ensure that the consistency of battery performance, while also shortening working hour, improves production effect
Rate.
Finally it should be noted that:The above embodiments are only used to illustrate the technical solution of the present invention., rather than its limitations;To the greatest extent
Present invention has been described in detail with reference to the aforementioned embodiments for pipe, it will be understood by those of ordinary skill in the art that:Its according to
So can with technical scheme described in the above embodiments is modified, either to which part or all technical features into
Row equivalent replacement;And these modifications or replacements, various embodiments of the present invention technology that it does not separate the essence of the corresponding technical solution
The range of scheme.
Claims (10)
1. a kind of proportioning process of lithium ion battery anode glue size, which is characterized in that include the following steps:
(a) progress of positive active material, conductive auxiliary agent, dispersant and thickener is dry-mixed, obtain mixed powder;
(b) solvent is added, mixing obtains the primary slurry that solid content is 82wt%~85wt%;
(c) solvent is added, mixing obtains the secondary slurries that solid content is 66wt%~68wt%;
(d) solvent is added, mixing obtains the three-level slurry that solid content is 56wt%~59wt%, to which lithium-ion electric be made
Pond anode sizing agent.
2. the proportioning process of lithium ion battery anode glue size according to claim 1, which is characterized in that in step (a), do
The speed that puddling is mixed is 15~25r/min of revolution, and the time is 25~35min.
3. the proportioning process of lithium ion battery anode glue size according to claim 1, which is characterized in that in step (b), first
8~15min is mixed with the speed for the 15~25r/min that revolves round the sun, then 110 are mixed with the speed for the 30~45r/min that revolves round the sun
~130min.
4. the proportioning process of lithium ion battery anode glue size according to claim 1, which is characterized in that in step (c), first
8~15min is mixed with the speed for the 15~25r/min that revolves round the sun, then with 30~45r/min, the 800~1500r/ of rotation of revolving round the sun
60~100min is mixed in the speed of min.
5. the proportioning process of lithium ion battery anode glue size according to claim 1, which is characterized in that in step (d), first
8~15min is mixed with the speed for the 15~25r/min that revolves round the sun, then with 30~45r/min, the 800~1500r/ of rotation of revolving round the sun
25~40min is mixed in the speed of min.
6. the proportioning process of lithium ion battery anode glue size according to claim 1, which is characterized in that further include de-bubble
Step after obtaining three-level slurry, carries out 25~35min of de-bubble under the speed for the 25~35r/min that revolves round the sun, lithium-ion electric is made
Pond anode sizing agent.
7. according to the proportioning process of claim 1~6 any one of them lithium ion battery anode glue size, which is characterized in that institute
The solid content for stating primary slurry is 83wt%~84wt%;The solid content of the secondary slurries is 67wt%~68wt%;It is described
The solid content of three-level slurry is 57wt%~58wt%.
8. according to the proportioning process of claim 1~6 any one of them lithium ion battery anode glue size, which is characterized in that institute
State in lithium ion battery anode glue size, positive active material, conductive auxiliary agent, dispersant and thickener mass ratio be (94~
97):(0.8~1.5):(0.08~0.15):(1~3);
Preferably, the positive active material includes LiFePO4;
Preferably, the conductive auxiliary agent includes conductive black, conductive carbon ball, electrically conductive graphite, carbon nanotube, conductive carbon fibre or stone
At least one of black alkene;
Preferably, the dispersant includes at least one of polyethylene glycol and polyvinylpyrrolidone;
Preferably, the thickener includes CMC;
Preferably, the solvent includes NMP.
9. a kind of based lithium-ion battery positive plate, including plus plate current-collecting body and the active material for being formed in the plus plate current-collecting body surface
Layer, which is characterized in that the slurry of the active material layer uses claim 1~8 any one of them lithium ion cell positive
The proportioning process of slurry is made.
10. a kind of lithium ion battery, which is characterized in that including the based lithium-ion battery positive plate described in claim 9.
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