CN107617351A - A kind of negative electrode of lithium ion battery stirring means, purposes and lithium ion battery - Google Patents
A kind of negative electrode of lithium ion battery stirring means, purposes and lithium ion battery Download PDFInfo
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- Y02E—REDUCTION OF GREENHOUSE GAS [GHG] EMISSIONS, RELATED TO ENERGY GENERATION, TRANSMISSION OR DISTRIBUTION
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Abstract
The invention discloses a kind of negative electrode of lithium ion battery stirring means, purposes and lithium ion battery, this method includes：Conductive agent is added in solvent and stirred in advance, while dispersant is stirred in advance；By the dispersant that mass percentage content is 50~60% and the negative active core-shell material that mass percentage content is 50~70%, while add in the pre- conductive agent for stirring to obtain, carry out first step stirring；Afterwards, the negative active core-shell material that mass percentage content is 30~50% is added, carries out second step stirring；Afterwards, the dispersant that mass percentage content is 40~50% is added, carries out the stirring of the 3rd step；Afterwards, add binding agent and carry out the stirring of the 4th step；Afterwards, defoaming treatment is carried out, and is discharged after the completion of the defoaming treatment.The solution of the present invention, lack of homogeneity, poor circulation in the prior art and the defects such as reliability is low can be overcome, realize the beneficial effect that uniformity is good, good cycle and reliability are high.
Description
Technical field
The invention belongs to cell art, and in particular to a kind of negative electrode of lithium ion battery stirring means, purposes and lithium from
Sub- battery.
Background technology
Lithium ion battery, it is a kind of secondary cell (i.e. rechargeable battery), it is general using the material conduct for containing elemental lithium
Electrode, it relies primarily on lithium ion (Li+), and movement carrys out work between a positive electrode and a negative electrode.In charge and discharge process, Li+ is at two
Insertion and deintercalation are come and gone between electrode：During charging, Li+ is embedded in negative pole, negative pole is in rich lithium shape from positive pole deintercalation by electrolyte
State；It is then opposite during electric discharge.What mobile phone and notebook computer used is all lithium ion battery.
Lithium ion battery is made up of positive pole, negative pole, barrier film, electrolyte, and both positive and negative polarity infiltrates in the electrolytic solution, and lithium ion is with electricity
Solution liquid is that medium moves between both positive and negative polarity, realizes the discharge and recharge of battery；For avoid both positive and negative polarity by contact occur short circuit, it is necessary to
Both positive and negative polarity is separated with barrier film.
Homogenate stirring is one of front end of lithium ion battery manufacture and important process, wherein, stirring with cathode size especially
Mix uncertain big, it is more difficult to control；Meanwhile whether cathode size stirring is uniformly good, directly affects later stage battery manufacturing process
Middle negative material surface forms the quality of solid electrolyte interface film (solid electrolyte interface, SEI film),
And SEI films are directly connected to cycle performance, chemical stability and heat endurance of battery etc..
The slurry that existing stirring technique is drawn is not uniform enough, and it is that can influence electricity that the later stage makes battery with uneven slurry
The cycle performance in pond etc..Such as：Publication No. CN204911355 first document discloses a kind of lithium ion cell positive homogenate
With V-mixer, Publication No. CN104549017 first document discloses a kind of stirring dress of lithium ion battery electrode sizing agent
Put, but these first documents do not improve cathode size essence, also not by improving the quality of slurry agitation, to improve electricity
The properties in pond etc..
In the prior art, lack of homogeneity, poor circulation and the defects such as reliability is low be present.
The content of the invention
It is an object of the present invention to it is directed to drawbacks described above, there is provided a kind of negative electrode of lithium ion battery stirring means, purposes and lithium
Ion battery, to solve the problems, such as the mixing uniformity difference of lithium ion battery cathode slurry in the prior art, reach lifting stirring
The effect of uniformity.
The present invention provides a kind of negative electrode of lithium ion battery stirring means, including：Step 1：Conductive agent is added in solvent
Row is stirred in advance, while dispersant is stirred in advance；Step 2：By mass percentage content be 50~60% the dispersant and
Mass percentage content is 50~70% negative active core-shell material, while adds in the pre- conductive agent for stirring to obtain, and enters
The row first step stirs；Step 3：The first step stirring after the completion of, add mass percentage content be 30~50% it is described
Negative active core-shell material, carry out second step stirring；Step 4：After the completion of second step stirring, adding mass percentage content is
40~50% dispersant, carry out the stirring of the 3rd step；Step 5：After the completion of the 3rd step stirring, add binding agent and enter
The step of row the 4th stirs；Step 6：After the completion of the 4th step stirring, defoaming treatment is carried out, and after the completion of the defoaming treatment
Discharging.
Alternatively, in addition to：Before institute's binding agent is added, obtain the mixture after the completion of the 3rd step stirs and glue
Degree；Determine whether the mixture viscosity reaches setting viscosity；When the mixture viscosity is not up to the setting viscosity, add
Diluent simultaneously continues to stir, until the mixture viscosity is adjusted to the setting viscosity.
Alternatively, in the step 1, the conductive agent is added in the solvent and stirred in advance, including：First by 10~
The mode of 30rpm rotating speed revolution, and/or 100~500rpm rotating speed rotation stirs, and stirs, until the conductive agent is dry
After powder complete wetting is in the solvent, scraper is carried out；After the completion of the scraper, then by 20~50rpm rotating speed revolution and/
Or in the way of 1000~2500rpm rotating speed rotation, stir 60~90min.
Alternatively, in the step 2, the first step stirring, including：First by 10~30rpm rotating speed revolution and/
Or the mode of 100~500rpm rotating speed rotation, stir 30~60min；Afterwards, by 20~50rpm rotating speed revolution, and/or
In the way of 100~500rpm rotating speed rotation, 30~40min is stirred.
Alternatively, in the step 3, the second step stirring, including：First by 10~30rpm rotating speed revolution and/
Or the mode of 100~500rpm rotating speed rotation stirs, until the negative active core-shell material complete wetting；And then by 30~
50rpm rotating speed revolution, and/or the mode of 1500~2500rpm rotating speed rotation, stir 90~120min.
Alternatively, in the step 4, the 3rd step stirring, including：First by 20~50rpm rotating speed revolution and/
Or the mode of 100~500rpm rotating speed rotations, stir 10~20min；And then by 30~50rpm rotating speed revolution, and/or
The mode of 1000~2500rpm rotating speed rotation, stir 120~130min.
Alternatively, in the step 5, the 4th step stirring, including：First by 20~50rpm rotating speed revolution and/
Or the mode of 100~500rpm rotating speed rotation, stir 30~60min；And then the rotating speed rotation by 1000~2500rpm
Mode, stir 30~60min.
Alternatively, wherein, stirred in advance in described add the conductive agent in the solvent, by 10~30rpm's
When rotating speed revolves round the sun, and/or the mode of 100~500rpm rotating speed rotation stirs, mixing time is 10~30min；And/or
In the second step stirring, stirred in the way of 10~30rpm rotating speed revolution, and/or 100~500rpm rotating speed rotation
When, mixing time is 10~30min.
Alternatively, stirred in advance in described add the conductive agent in the solvent, when carry out the stirring 60~
During 90min, carry out vacuumizing setting.
Alternatively, wherein, the stirring environment of the second step stirring is vacuum environment；And/or the second step stirring
Mixing speed, more than the mixing speed of first step stirring；And/or enter in the solvent by conductive agent addition
Row is pre- to be stirred, and/or the pre- of the dispersant is stirred, and/or the first step stirs, and is carried out under non-vacuum；With/
Or, in the step 6, the defoaming treatment, including：By way of vacuumizing, the defoaming treatment before the discharging is carried out.
Alternatively, wherein, the conductive agent, including：SP series, KS-6, KS-15, Ketjen black, acetylene black, vapor phase growth
At least one of carbon fiber, CNT；And/or the solvent, including：Deionized water；And/or the dispersant, bag
Include：CMC；And/or the negative active core-shell material, including：Graphite；And/or the binding agent, including：Butadiene-styrene rubber.
Matching with the above method, further aspect of the present invention provides a kind of purposes of negative electrode of lithium ion battery stirring means,
Including：By above-described negative electrode of lithium ion battery stirring means, in the preparation technology of lithium ion battery.
Matching with the above method, another aspect of the invention also provides a kind of lithium ion battery, including：By above-described
The negative electrode of lithium ion battery that negative electrode of lithium ion battery stirring means are prepared.
The solution of the present invention, by using a kind of negative pole stirring technique, the uniformity of cathode size stirring is improved, makes conduction
Agent, binding agent are well mixed with negative electrode active material so that its surface formed SEI film dense uniforms, so as to improve battery
Cycle performance and electrochemical stability.
Further, the solution of the present invention, actual conditions are manufactured by combining, it is corresponding to devise in cathode size whipping process
The addition sequences of various materials, number and corresponding mixing speed, time etc. so that the uniformity of slurry is greatly improved,
So that the formation effect and chemical stability of later stage SEI film are strengthened, and then improve the cycle performance of battery.
Further, the solution of the present invention, by setting a kind of negative electrode of lithium ion battery stirring technique, including each component plus
Enter order, number and corresponding mixing speed and time, the uniformity of cathode size mixing can be improved, so as to improve circulating battery
Energy.
Further, the solution of the present invention, the method that negative electrode of lithium ion battery part is prepared by offer, it is chemical material group
Point, i.e. cathode size, its preparation needs the solubilizer in agitating device to stir as slurry；The uniform of cathode size can be improved
Property, make conductive agent, binding agent dispersed in major ingredient；Improve cycle performance of battery.
Thus, the solution of the present invention, addition sequence, the number to each component in negative electrode of lithium ion battery stirring technique are passed through
And corresponding mixing speed and time are configured, solves the mixing uniformity difference of lithium ion battery cathode slurry in the prior art
Problem, so as to overcome lack of homogeneity, the defects of poor circulation and reliability are low in the prior art, realize that uniformity is good, circulation
The beneficial effect that performance is good and reliability is high.
Other features and advantages of the present invention will be illustrated in the following description, also, partly becomes from specification
Obtain it is clear that or being understood by implementing the present invention.
Below by drawings and examples, technical scheme is described in further detail.
Brief description of the drawings
Fig. 1 is the process chart of the negative electrode of lithium ion battery stirring means of the present invention；Wherein, conductive agent, negative electrode active
Material, glue, binding agent etc. are the composition material of cathode size, and percentage is adds the mass fraction example of material, arrow
It show the timing node that each material adds；
Fig. 2 is the SEM using cathode size made from the negative electrode of lithium ion battery stirring means of the present invention
(SEM) figure；
Fig. 3 is following using the lithium ion battery of cathode size made from the negative electrode of lithium ion battery stirring means of the present invention
Ring performance test curve map；Wherein, the test curve includes embodiment curve and comparative example curve.
Embodiment
To make the object, technical solutions and advantages of the present invention clearer, below in conjunction with the specific embodiment of the invention and
Technical solution of the present invention is clearly and completely described corresponding accompanying drawing.Obviously, described embodiment is only the present invention one
Section Example, rather than whole embodiments.Based on the embodiment in the present invention, those of ordinary skill in the art are not doing
Go out under the premise of creative work the every other embodiment obtained, belong to the scope of protection of the invention.
According to an embodiment of the invention, there is provided a kind of negative electrode of lithium ion battery stirring means.
Embodiment 1
The negative electrode of lithium ion battery stirring means of the present embodiment can include：
Step 1：Can be by the negative electrode of lithium ion battery formula of setting, the amount of each component based on setting, by the conduction
Stirred in advance in the agent addition solvent (such as：Conductive agent is added in deionized water and stirred in advance), while to described scattered
Agent is stirred in advance.
Such as：While being stirred in advance the conductive agent and the solvent, the dispersant is stirred in advance.
In an optional example, in the step 1, the conductive agent is added in the solvent and stirred in advance, can
With including：First stirred in the way of 10rpm rotating speed revolution, and/or 100rpm rotating speed rotation, until the conductive agent is dry
After powder complete wetting is in the solvent, scraper is carried out；After the completion of the scraper, then by 20rpm rotating speed revolve round the sun, and/or press
The mode of 1000rpm rotating speed rotation, stir 60min.By way of first stirring at low speed, raising speed is stirred soon again, can avoid due to
Dry powder caused by conductive agent density is small, volume is big is flown upward, and mixing uniformity is good and the feature of environmental protection is good.
Such as：Revolution, can be a bigger agitating paddle, first different powders, solvent somewhat be mixed, rotating speed leads to
It is often slower.And rotation, that rotor of soy bean milk making machine can be analogous to, it is necessary to slurry is further stirred well it is even, so general turn
Speed is also very fast.In most cases, revolution and rotation are synchronously carried out.But sometimes need only to open what revolution guarantee had been stirred
Slurry does not settle the state for just, exactly allowing slurry to keep a flowing.
Thus, by setting different revolution rotating speeds and rotation rotating speed to be stirred, mixing uniformity is good and the feature of environmental protection
It is good.
In alternatively, being stirred in advance in the solvent by conductive agent addition, revolved round the sun by 10rpm rotating speed,
And/or the mode of 100rpm rotating speed rotation is when stirring, mixing time 10min.
Thus, by setting mixing time of the dry powder complete wetting for being suitable to make conductive agent in the solvent, reliability
High and good energy saving property.
In an alternative example, in being stirred in advance in the solvent by conductive agent addition, work as progress
During the stirring 60min, carry out vacuumizing setting, so that it is carried out under vacuum conditions to the step 6.Such as：It can increase
Add and vacuumize setting, being stirred under vacuum state can make to contact more fully between slurry, mix evenly, but can slightly affected slurry
Solid content and each composition material proportioning.
Thus, by being stirred under vacuum in each whipping process after stirring in advance, mixing uniformity can be lifted, is entered
And be advantageous to lift cycle performance of battery.
Step 2：By 50% dispersant and 50% negative active core-shell material, while add described pre- stir
In the obtained conductive agent, first step stirring is carried out.
In an optional example, in the step 2, the first step stirring, it can include：First turn by 10rpm
Speed revolution, and/or the mode of 100rpm rotating speed rotation, stir 30min；Afterwards, revolved round the sun, and/or pressed by 20rpm rotating speed
The mode of 100rpm rotating speed rotation, stir 30min.
Step 3：After the completion of first step stirring, 30% negative active core-shell material is added, second step is carried out and stirs
Mix.
In an optional example, in the step 3, the second step stirring, it can include：First turn by 10rpm
The mode of speed revolution, and/or 100rpm rotating speed rotation stirs, until the negative active core-shell material complete wetting；And then press
30rpm rotating speed revolution, and/or the mode of 1500rpm rotating speed rotation, stir 90min.
Alternatively, in second step stirring, by 10rpm rotating speed revolution, and/or the side of 100rpm rotating speed rotation
When formula stirs, mixing time 10min.
Alternatively, the stirring environment of the second step stirring is vacuum environment；And/or the stirring of the second step stirring
Speed, more than the mixing speed of first step stirring.
Thus, raised speed by being stirred when second step stirs relative to the first step, be more beneficial for lifting mixing uniformity, and
It can ensure that the content of each component is accurate.
Step 4：After the completion of second step stirring, 40% dispersant is added, carries out the stirring of the 3rd step.
Such as：Stirring is caused to tie to avoid adding excessive negative active core-shell material (being used herein as second particle negative material)
Block, in step 2 to step 4, for the first time by a part of glue and a part of negative active core-shell material (such as：Graphite) add simultaneously.
After progress major ingredient stirs in advance, remaining negative active core-shell material is added, vacuum adds remaining glue after stirring soon, be further continued for carrying out major ingredient
Stirring.
In an optional example, in the step 4, the 3rd step stirring, it can include：First turn by 20rpm
Speed revolution, and/or the mode of 100rpm rotating speed rotations, stir 10min；And then by 30rpm rotating speed revolution, and/or
The mode of 1000rpm rotating speed rotation, stir 120min.
Step 5：After the completion of the 3rd step stirring, add the binding agent and carry out the stirring of the 4th step.
In an optional example, in the step 5, the 4th step stirring, it can include：First turn by 20rpm
Speed revolution, and/or the mode of 100rpm rotating speed rotation, stir 30min；And then the side of the rotating speed rotation by 1000rpm
Formula, stir 30min.
Thus, set by the adaptation of the different revolution rotating speed of each step, rotation rotating speed, it is ensured that mixing uniformity,
To improve the uniformity of cathode size, make conductive agent, binding agent dispersed in major ingredient；And the feature of environmental protection is good.
Step 6：After the completion of the 4th step stirring, defoaming treatment is carried out, and discharged after the completion of the defoaming treatment.
Thus, by being stirred in advance conductive agent and dispersant respectively, other components is gradually added portionwise afterwards and are stirred
Mix, the uniformity of cathode size can be improved, make conductive agent, binding agent dispersed in major ingredient；And then be advantageous to improve electricity
Pond cycle performance.
In an optional example, in the step 6, the defoaming treatment, including：By way of vacuumizing, enter
Defoaming treatment before the row discharging.Wherein, in whipping process it is all vacuumize the vacuum that need to reach can be -0.08~-
0.09Mpa。
Such as：Defoaming treatment, bubble is exactly eliminated, i.e., vacuumized when stirring, discharge gas.
Thus, defoamed by way of vacuumizing, operating process is simple, and vacuumizes reliability height.
In an optional example, to avoid vacuumizing caused solid content change, the stirring of early stage is not in vacuum shape
Carried out under state.Such as：In above step 1 into step 6, it is described the conductive agent is added in the solvent stirred in advance and/
Or to the dispersant it is pre- stir, and/or the first step stir, carried out under non-vacuum.
Thus, by being arranged to vacuum or antivacuum to stirring environment adaptation, mixing uniformity can be lifted according to demand
Or ensureing each component content accuracy, flexibility is good, and reliability is high.
In an optional embodiment, it can also include：Stirred after the completion of the 3rd step stirring, in the 4th step
Before mixing, mixture viscosity is determined and adjusted, it is specific as follows：
(1) before the binding agent is added, obtain after the completion of the 3rd step stirring mixture viscosity (such as：Pass through
The viscosity harvesters such as viscosity sensor, viscosity measurement instrument, collect the mixture after the completion of the 3rd step stirs and glue
Degree).
(2) determine whether the mixture viscosity reaches setting viscosity.
When the mixture viscosity be not up to it is described setting viscosity when, add diluent (such as：Water) adjust and continue to stir
Mix, until the mixture viscosity is adjusted to the setting viscosity.
Wherein, cathode size typically has a suitable range of viscosities, more than this scope, it is necessary to adjusts, this model
Enclose uncertain, the negative material of different model, the cathode size of different ratio are all different.Viscosity regulation is mainly by adding water
Change solid content, i.e. solid/(solid+water).The more solid contents of general water are lower, but are not linear.
Thus, can be according to setting viscosity flexible modulation mixture viscosity by the detection and regulation of viscosity, and regulation side
Formula is easy, regulation accuracy is good.
Alternatively, the conductive agent, can include：SP series, KS-6, KS-15, Ketjen black, acetylene black, vapor grown carbon
At least one of fiber, CNT.
Such as：Conductive agent can include：SP series (i.e. conductive black), KS-6 (i.e. electrically conductive graphite), KS-15 are (i.e. conductive
Graphite), Ketjen black (KB), acetylene black (AB), gas-phase growth of carbon fibre (VGCF), the one or more in CNT (CNT).
Alternatively, the solvent, can include：Deionized water.
Alternatively, the dispersant, can include：CMC (carboxymethyl cellulose).
Alternatively, the negative active core-shell material, can include：Graphite.
Alternatively, the binding agent, can include：Butadiene-styrene rubber.
Such as：Binding agent includes butadiene-styrene rubber (SBR, Styrene-butadiene rubber), a kind of chemical material.It is negative
The each component material of pole slurry is added by shared quality proportion, that is, is matched, every kind of battery it is all different.On stirring
Mode, rotating speed, mixing time of revolution and the rotation of agitating paddle in mixer, etc. are exactly set.
Thus, by each component of diversified forms, component can be chosen as needed, and then lift negative electrode of lithium ion battery
The flexibility of preparation and convenience.
Embodiment 2
Unlike the embodiments above, the negative electrode of lithium ion battery stirring means of the present embodiment can include：
In step 1, the conductive agent is added in the solvent and stirred in advance, can included：First press 30rpm rotating speed
The mode of revolution, and/or 500rpm rotating speed rotation stirs, until the dry powder complete wetting of the conductive agent is in the solvent
Afterwards, scraper is carried out；After the completion of the scraper, then the side by 50rpm rotating speed revolution, and/or the rotating speed rotation by 2500rpm
Formula, stir 90min.
In alternatively, being stirred in advance in the solvent by conductive agent addition, revolved round the sun by 30rpm rotating speed,
And/or the mode of 500rpm rotating speed rotation is when stirring, mixing time 30min.
In an alternative example, in being stirred in advance in the solvent by conductive agent addition, work as progress
During the stirring 90min, carry out vacuumizing setting, so that it is carried out under vacuum conditions to the step 6.
Step 2：By 60% dispersant and 70% negative active core-shell material, while add described pre- stir
In the obtained conductive agent, first step stirring is carried out.
In an optional example, in the step 2, the first step stirring, it can include：First turn by 30rpm
Speed revolution, and/or the mode of 500rpm rotating speed rotation, stir 60min；Afterwards, revolved round the sun, and/or pressed by 50rpm rotating speed
The mode of 500rpm rotating speed rotation, stir 40min.
Step 3：After the completion of first step stirring, 50% negative active core-shell material is added, second step is carried out and stirs
Mix.
In an optional example, in the step 3, the second step stirring, it can include：First turn by 30rpm
The mode of speed revolution, and/or 500rpm rotating speed rotation stirs, until the negative active core-shell material complete wetting；And then press
50rpm rotating speed revolution, and/or the mode of 2500rpm rotating speed rotation, stir 125min.
Alternatively, in second step stirring, by 30rpm rotating speed revolution, and/or the side of 500rpm rotating speed rotation
When formula stirs, mixing time 30min.
Step 4：After the completion of second step stirring, 50% dispersant is added, carries out the stirring of the 3rd step.
In an optional example, in the step 4, the 3rd step stirring, it can include：First turn by 50rpm
Speed revolution, and/or the mode of 500rpm rotating speed rotations, stir 20min；And then by 50rpm rotating speed revolution, and/or
The mode of 2500rpm rotating speed rotation, stir 130min.
In the step 5, the 4th step stirring, it can include：First by 50rpm rotating speed revolution, and/or 500rpm
Rotating speed rotation mode, stir 60min；And then in the way of 2500rpm rotating speed rotation, stir 60min.
Thus, by using a kind of negative pole stirring technique, the uniformity of cathode size stirring is improved, makes conductive agent, bonding
Agent is well mixed with negative electrode active material so that its surface formed SEI film dense uniforms, so as to improve the cyclicity of battery
Energy and electrochemical stability.
Embodiment 3
Unlike the embodiments above, the negative electrode of lithium ion battery stirring means of the present embodiment can include：
In step 1, the conductive agent is added in the solvent and stirred in advance, can included：First press 20rpm rotating speed
The mode of revolution, and/or 300rpm rotating speed rotation stirs, and stirs, until the dry powder complete wetting of the conductive agent is in described
After in solvent, scraper is carried out；After the completion of the scraper, then by 35rpm rotating speed revolution, and/or the rotating speed rotation by 1750rpm
Mode, stir 75min.
In alternatively, being stirred in advance in the solvent by conductive agent addition, revolved round the sun by 20rpm rotating speed,
And/or the mode of 300rpm rotating speed rotation is when stirring, mixing time 20min.
In an alternative example, in being stirred in advance in the solvent by conductive agent addition, work as progress
During the stirring 75min, carry out vacuumizing setting, so that following step 2 is carried out under vacuum conditions to the step 6.
Step 2：By 55% dispersant and 60% negative active core-shell material, while add described pre- stir
In the obtained conductive agent, first step stirring is carried out.
In an optional example, in the step 2, the first step stirring, it can include：First turn by 20rpm
Speed revolution, and/or the mode of 300rpm rotating speed rotation, stir 45min；Afterwards, revolved round the sun, and/or pressed by 35rpm rotating speed
The mode of 300rpm rotating speed rotation, stir 30min.
Step 3：After the completion of first step stirring, 40% negative active core-shell material is added, second step is carried out and stirs
Mix.
In an optional example, in the step 3, the second step stirring, it can include：First turn by 20rpm
The mode of speed revolution, and/or 300rpm rotating speed rotation stirs, until the negative active core-shell material complete wetting；And then press
40rpm rotating speed revolution, and/or the mode of 2000rpm rotating speed rotation, stir 105min.
Alternatively, in second step stirring, by 20rpm rotating speed revolution, and/or the side of 300rpm rotating speed rotation
When formula stirs, mixing time 20min.
Step 4：After the completion of second step stirring, 45% dispersant is added, carries out the stirring of the 3rd step.
In an optional example, in the step 4, the 3rd step stirring, it can include：First turn by 35rpm
Speed revolution, and/or the mode of 300rpm rotating speed rotations, stir 15min；And then by 40rpm rotating speed revolution, and/or
The mode of 1750rpm rotating speed rotation, stir 120min.
In the step 5, the 4th step stirring, it can include：First by 35rpm rotating speed revolution, and/or 300rpm
Rotating speed rotation mode, stir 45min；And then in the way of 1750rpm rotating speed rotation, stir 45min.
Thus, adjusted by the adaptation of the addition sequence of each component and addition, can be made that stability is good, high safety
Negative electrode of lithium ion battery, and then be advantageous to lifted lithium ion battery cycle performance.
Various embodiments above, the test effect that can at least reach can include：After being stirred using various embodiments above Slurry is uniformly dispersed, and without obvious aberration, viscosity is suitable, and good cyclicity is shown in follow-up battery testing Can, illustrate that the SEI films formation effect of negative terminal surface is good, improve stable charge/discharge of battery etc..
Such as：Arbitrarily match cathode size (such as：Cathode size each group distribution ratio is：Negative electrode active material：It is conductive
Agent：Dispersant：Binding agent=96：1.5：1.2：1.3) in stirring technique, after the stirring means stirring of the present embodiment, slurry
Material is uniformly dispersed, without obvious aberration；And the cycle performance in further battery test is good.
In an optional example, as shown in Figure 2 using the SEM of cathode size made from stirring means of the present invention
Figure, conductive agent, binding agent etc. are uniformly dispersed, and do not occur obvious agglomeration, and be uniformly distributed between negative pole major ingredient.Show to bear
The uniformity of pole slurry is preferable, is advantageous to the formation of later stage SEI film and the stability of cycle charge-discharge.
In an optional example, the lithium using cathode size made from stirring means of the present invention is illustrated in figure 3
The cycle performance test curve figure (embodiment and comparative example) of ion battery.Under particular cycle mechanism, embodiment follows in Fig. 3
Ring performance is substantially better than comparative example, and overall circulation volume conservation rate attenuation trend is gentle, and does not occur the diving phenomenon of comparative example,
Illustrate that such a stirring means can be effectively improved the uniformity of cathode size and the chemical stability of later stage lithium ion battery and follow
Ring performance.
In figure 3, cycle is exactly to circulate, and can refer to the charge and discharge cycles test of battery, for characterizing the discharge and recharge of battery
Performance；For example, sometimes mobile phone has used a period of time to find can not filling electricity, or even if fully charged, can also use soon
Complete, here it is poor circulation, and this is the important performance evaluation index of a battery.RT, which is represented, to be carried out in normal temperature environment ,@
Nothing particularly looks like, and is exactly individual bound symbol.Fig. 3 is by being test curve to the normal-temperature circulating performance of lithium ion battery
Figure.
The processing and function realized by the method for the present embodiment essentially correspond to the embodiment of aforementioned formula, principle and
Example, therefore not detailed part in the description of the present embodiment, may refer to the related description in previous embodiment, do not do herein superfluous
State.
Through substantial amounts of verification experimental verification, using technical scheme, actual conditions are manufactured by combining, it is corresponding to devise
The addition sequence of various materials in cathode size whipping process, number and corresponding mixing speed, time etc. so that slurry it is equal
Even property is greatly improved, so that the formation effect and chemical stability of later stage SEI film are strengthened, and then improves electricity
The cycle performance in pond.
According to an embodiment of the invention, a kind of lithium-ion electric corresponding to negative electrode of lithium ion battery stirring means is additionally provided
The purposes of pond negative pole stirring means.The purposes of the negative electrode of lithium ion battery stirring means can include：By lithium as described above
Ion battery negative pole stirring means, in the preparation technology of lithium ion battery.
In an optional example, negative electrode of lithium ion battery stirring means that the present embodiment uses can improve cathode size
The uniformity of mixing, so as to improve cycle performance of battery.Concrete technical scheme is：
Step 1, first progress conductive agent stirs in advance, meanwhile, the synchronous stirring for carrying out glue.
Wherein, conductive agent can include：SP series (i.e. conductive black), KS-6 (i.e. electrically conductive graphite), KS-15 are (i.e. conductive
Graphite), Ketjen black (KB), acetylene black (AB), gas-phase growth of carbon fibre (VGCF), the one or more in CNT (CNT).
Step 2, then glue adds at twice.Wherein, glue and negative active core-shell material add at twice respectively, from Fig. 1
It is exactly glue that middle arrow, which adds the dispersant that node can be seen that in Fig. 1,.
For the first time by mass parts be 50%~60% (such as：50 powder, 55%, 60% etc. can be selected) glue and quality
Part for 50%~70% (such as：50%, 60%, 70% etc. can be selected) negative active core-shell material (such as：Graphite) add simultaneously
Enter.
After progress major ingredient stirs in advance, remaining negative active core-shell material is added, vacuum adds remaining glue, is further continued for after stirring soon
Carry out major ingredient stirring.
Wherein, what major ingredient referred to is exactly agitated those material before this step, is used as differentiation, is not that certain is specific
Material.Cathode size includes those in Fig. 1：Conductive agent, solvent (such as：Deionized water), dispersant, negative active core-shell material
Or negative electrode active material, binding agent.It is exactly the node location that arrow points to from Fig. 1 to the addition sequence of each composition, from upper
Lower addition.
Step 3, add afterwards if it need to adjust viscosity diluent (such as：Water) regulation to suitable, be eventually adding binding agent and enter
Row stirring, discharges after defoaming, treats that subsequent processing uses, using the battery of such a stirring technique, conductive agent, binding agent are in major ingredient
It is uniformly dispersed, improves cycle performance positive effect.
In an optional example, as shown in figure 1, the negative electrode of lithium ion battery stirring means of the present embodiment, can include：
(1) conductive agent is added in deionized water first and stirred in advance, the another synchronous stirring for carrying out glue；Due to conductive agent
Density is small, and volume is big, to avoid dry powder from flying upward, first with revolve round the sun and 10~30rpm (such as：Can select 10rpm, 20rpm,
30rpm etc.), 100~500rpm of rotation (such as：100rpm, 300rpm, 500rpm etc. can be selected) the slow-speed of revolution stirring 10~
30min (such as：10min, 20min, 30mi etc. can be selected), after dry powder complete wetting scraper (such as：Vulcanite scraper can be used
Plate etc. scrapes materials and parts, and the powder not being completely dissolved on agitating paddle, and/or on stirring top tank structure, solidliquid mixture etc. are wiped off), then
By revolution 20~50rpm (such as：20rpm, 35rpm, 50rpm etc. can be selected), 1000~2500rpm of rotation (such as：Can be with
Selection 1000rpm, 1750rpm, 2500rpm etc.) stir soon 60~90min (such as：60min, 75min, 90min can be selected
Deng).
(2) then cause to stir to avoid adding excessive negative active core-shell material (being used herein as second particle negative material)
Caking, first add mass parts 50%~60% (such as：50%, 55%, 60% etc. can be selected) glue, and only add quality
Part 50%~70% (such as：50%, 60%, 70% etc. can be selected) negative active core-shell material carry out major ingredient and stir in advance, set public
Turn 10~30rpm (such as：10rpm, 20rpm, 30rpm etc. can be selected), 100~500rpm of rotation (such as：It can select
100rpm, 300rpm, 500rpm etc.) 30~60min of stirring (such as：30min, 45min, 60min etc. can be selected) after, it will stir
Speed raising extremely 20~50rpm of revolution (such as：20rpm, 35rpm, 50rpm etc. can be selected), 100~500rpm of rotation (such as：
100rpm, 300rpm, 500rpm etc. can be selected) stirring 35min, while to avoid vacuumizing caused solid content change, it is preceding
The stirring of phase is not carried out under vacuum conditions.
After add remaining negative active core-shell material, by revolution 10~30rpm (such as：Can select 10rpm,
20rpm, 30rpm etc.), 100~500rpm of rotation (such as：100rpm, 300rpm, 500rpm etc. can be selected) stir 10 slowly~
30min (such as：10min, 20min, 30min etc. can be selected), now negative active core-shell material complete wetting, then carries rotating speed
Up to 30~50rpm of revolution (such as：Can select), 1500~2500rpm of rotation (such as：Can select 1500rpm,
2000rpm, 2500rpm etc.), and stir soon under vacuum conditions 90~120min (such as：Can select 90min, 105min,
120min etc.).
After add remaining glue, first by revolution 20~50rpm (such as：20rpm, 35rpm, 50rpm can be selected
Deng), 100~500rpm of rotation (such as：100rpm, 300rpm, 500rpm etc. can be selected) stir in advance after 10min again by revolution 30
~50rpm (such as：30rpm, 40rpm, 50rpm etc. can be selected), 1000~2500rpm of rotation (such as：It can select
1000rpm, 1750rpm, 2500rpm etc.) 120min is stirred soon, step stirring need to such as adjust viscosity after terminating, then add diluent (example
Such as：Water) regulation, as viscosity is suitable, be then directly added into binder solution, according to 20~50rpm of revolution (such as：It can select
20rpm, 35rpm, 50rpm etc.), 100~500rpm of rotation (such as：100rpm, 300rpm, 500rpm etc. can be selected) stirring
30~60min (such as：30min, 45min, 60min etc. can be selected), after rotation is improved to 1000~2500rpm (examples again
Such as：1000rpm, 1750rpm, 2500rpm etc. can be selected) stir soon 30~60min (such as：Can select 30min, 45min,
60min etc.), while the defoaming treatment before being discharged is vacuumized, negative pole stirring is completed, and the later stage can carry out preparing lithium ion battery
Finished product.
Alternatively, the addition mass fraction of each material described in above-described embodiment can replace with it according to actual processing conditions
His numerical value.
Alternately, in above-described embodiment conductive agent stir 60~90min (such as：Can select 60min, 75min,
90min etc.) when, it can increase and vacuumize setting, being stirred under vacuum state can make to contact more fully between slurry, mix evenly,
But can the solid content of slightly affected slurry and the proportioning of each composition material.
Thus, by using a kind of negative pole stirring technique, the uniformity of cathode size stirring is improved, makes conductive agent, bonding
Agent is well mixed with negative electrode active material so that its surface formed SEI film dense uniforms, so as to improve the cyclicity of battery
Energy and electrochemical stability.
The processing and function realized by the purposes of the present embodiment essentially correspond to the embodiment of preceding method, principle and
Example, therefore not detailed part in the description of the present embodiment, may refer to the related description in previous embodiment, do not do herein superfluous
State.
Through substantial amounts of verification experimental verification, using technical scheme, by setting a kind of negative electrode of lithium ion battery to stir
Technique, including the addition sequence of each component, number and corresponding mixing speed and time, can improve the uniform of cathode size mixing
Property, so as to improve cycle performance of battery.
According to an embodiment of the invention, a kind of lithium-ion electric corresponding to negative electrode of lithium ion battery stirring means is additionally provided
Pond.The lithium ion battery can include：The lithium-ion electric being prepared by above-described negative electrode of lithium ion battery stirring means
Pond negative pole.
The processing and function realized by the battery of the present embodiment essentially correspond to the embodiment of preceding method, principle and
Example, therefore not detailed part in the description of the present embodiment, may refer to the related description in previous embodiment, do not do herein superfluous
State.
Through substantial amounts of verification experimental verification, using technical scheme, negative electrode of lithium ion battery part is prepared by offer
Method, be chemical material component, i.e. cathode size, it is slurry that its preparation, which needs the solubilizer stirring in agitating device,；Can be with
The uniformity of cathode size is improved, makes conductive agent, binding agent dispersed in major ingredient；Improve cycle performance of battery.
To sum up, it will be readily appreciated by those skilled in the art that on the premise of not conflicting, above-mentioned each advantageous manner can be certainly
Combined, be superimposed by ground.
Embodiments of the invention are the foregoing is only, are not intended to limit the invention, for those skilled in the art
For member, the present invention can have various modifications and variations.Any modification within the spirit and principles of the invention, being made,
Equivalent substitution, improvement etc., should be included within scope of the presently claimed invention.
Claims (13)
- A kind of 1. negative electrode of lithium ion battery stirring means, it is characterised in that including：Step 1：Conductive agent is added in solvent and stirred in advance, while dispersant is stirred in advance；Step 2：It is 50~70% by the dispersant and mass percentage content that mass percentage content is 50~60% Negative active core-shell material, while add in the pre- conductive agent for stirring to obtain, carry out first step stirring；Step 3：After the completion of first step stirring, the negative electrode active material that mass percentage content is 30~50% is added Material, carry out second step stirring；Step 4：After the completion of second step stirring, the dispersant that mass percentage content is 40~50% is added, is entered The step of row the 3rd stirs；Step 5：After the completion of the 3rd step stirring, add binding agent and carry out the stirring of the 4th step；Step 6：After the completion of the 4th step stirring, defoaming treatment is carried out, and discharged after the completion of the defoaming treatment.
- 2. according to the method for claim 1, it is characterised in that also include：Before institute's binding agent is added, the mixture viscosity after the completion of the 3rd step stirring is obtained；Determine whether the mixture viscosity reaches setting viscosity；When the mixture viscosity is not up to the setting viscosity, solubilizer simultaneously continues to stir, until the mixture is glued Degree is adjusted to the setting viscosity.
- 3. method according to claim 1 or 2, it is characterised in that in the step 1, the conductive agent is added into institute State in solvent and stirred in advance, including：First stir, stir in the way of 10~30rpm rotating speed revolution, and/or 100~500rpm rotating speed rotation, until institute After the dry powder complete wetting of conductive agent is stated in the solvent, scraper is carried out；After the completion of the scraper, then the side by 20~50rpm rotating speed revolution, and/or the rotating speed rotation by 1000~2500rpm Formula, stir 60~90min.
- 4. according to the method described in one of claim 1-3, it is characterised in that in the step 2, the first step stirring, Including：First in the way of 10~30rpm rotating speed revolution, and/or 100~500rpm rotating speed rotation, 30~60min is stirred；Afterwards, by 20~50rpm rotating speed revolution, and/or in the way of 100~500rpm rotating speed rotation, stirring 30~ 40min。
- 5. according to the method described in one of claim 1-4, it is characterised in that in the step 3, the second step stirring, Including：First stirred in the way of 10~30rpm rotating speed revolution, and/or 100~500rpm rotating speed rotation, until the negative pole Active material complete wetting；And then in the way of 30~50rpm rotating speed revolution, and/or 1500~2500rpm rotating speed rotation, stirring 90~ 120min。
- 6. according to the method described in one of claim 1-5, it is characterised in that in the step 4, the 3rd step stirring, Including：First in the way of 20~50rpm rotating speed revolution, and/or 100~500rpm rotating speed rotations, 10~20min is stirred；And then in the way of 30~50rpm rotating speed revolution, and/or 1000~2500rpm rotating speed rotation, stirring 120~ 130min。
- 7. according to the method described in one of claim 1-6, it is characterised in that in the step 5, the 4th step stirring, Including：First in the way of 20~50rpm rotating speed revolution, and/or 100~500rpm rotating speed rotation, 30~60min is stirred；And then in the way of 1000~2500rpm rotating speed rotation, stir 30~60min.
- 8. according to the method described in one of claim 5-7, it is characterised in that wherein,In being stirred in advance in the solvent by conductive agent addition, by 10~30rpm rotating speed revolution, and/or 100 When the mode of~500rpm rotating speed rotation stirs, mixing time is 10~30min；And/orIn second step stirring, in the way of 10~30rpm rotating speed revolution, and/or 100~500rpm rotating speed rotation During stirring, mixing time is 10~30min.
- 9. according to the method described in one of claim 3-8, it is characterised in that the conductive agent is added into the solvent described It is middle to be stirred in advance, when carrying out 60~90min of the stirring, carry out vacuumizing setting.
- 10. according to the method described in one of claim 1-8, it is characterised in that wherein,The stirring environment of the second step stirring is vacuum environment；And/or the mixing speed of the second step stirring, more than institute State the mixing speed of first step stirring；And/orDescribed add the conductive agent in the solvent is stirred, and/or the pre- of the dispersant is stirred, and/or described in advance The first step stirs, and is carried out under non-vacuum；And/orIn the step 6, the defoaming treatment, including：By way of vacuumizing, carry out at the defoaming before the discharging Reason.
- 11. according to the method described in one of claim 1-10, it is characterised in that wherein,The conductive agent, including：In SP series, KS-6, KS-15, Ketjen black, acetylene black, gas-phase growth of carbon fibre, CNT At least one of；And/orThe solvent, including：Deionized water；And/orThe dispersant, including：CMC；And/orThe negative active core-shell material, including：Graphite；And/orThe binding agent, including：Butadiene-styrene rubber.
- A kind of 12. purposes of negative electrode of lithium ion battery stirring means, it is characterised in that including：Will be as appointed in claim 1-11 Negative electrode of lithium ion battery stirring means described in one, in the preparation technology of lithium ion battery.
- A kind of 13. lithium ion battery, it is characterised in that including：As the lithium-ion electric as any one of claim 1-11 The negative electrode of lithium ion battery that pond negative pole stirring means are prepared.
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