CN102064326A - Dispersing agent for positive and negative electrode materials of lithium ion battery - Google Patents
Dispersing agent for positive and negative electrode materials of lithium ion battery Download PDFInfo
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- CN102064326A CN102064326A CN2010105912034A CN201010591203A CN102064326A CN 102064326 A CN102064326 A CN 102064326A CN 2010105912034 A CN2010105912034 A CN 2010105912034A CN 201010591203 A CN201010591203 A CN 201010591203A CN 102064326 A CN102064326 A CN 102064326A
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- Y02E60/10—Energy storage using batteries
Abstract
The invention discloses a dispersing agent for positive and negative electrode materials of a lithium ion battery. A surface active agent of the dispersing agent is modified polyoxyethylene ether. Compared with the prior art, the dispersing agent has the advantages that 1) an addition method is simple; 2) the dispersing effect is good; 3) the application range is wide; 4) the electrochemical performance is stable; 5) the low-temperature performance of the battery can be improved; and 6) the safety performance of the battery can be improved, and safety tests in terms of over-charging, nail penetrating, side compression, weight impact and the like are improved.
Description
Technical field
The present invention relates to a kind of dispersant, especially a kind of dispersant that the lithium ion battery plus-negative plate material is had better dispersion effect.
Background technology
Lithium ion battery is owing to have that energy density height, operating voltage height, temperature limit are wide, advantage such as have extended cycle life, and be widely used as the power supply of various mobile devices, even conventional batteries, especially its high-energy-density of progressively replacing other in fields such as Aeronautics and Astronautics, navigation, automobile, Medical Devices have been made significant contribution for the miniaturization of mobile device especially.
Usually have the difficulties in dispersion of effective substance such as conductive carbon, active material (as graphite, cobalt acid lithium, LiMn2O4, lithium nickel cobalt manganese etc.) in the lithium ion battery preparation process, cause the performance of battery to be not in full use, influenced the application of lifting of energy content of battery density and lithium ion battery in fields such as high low temperature, safety.
In order to overcome above-mentioned defective, adopt positive and negative pole material such as offspring, carbon encapsulated material and the nano modified material etc. of better structure usually, though can improve some performance of battery like this, can not significantly improve the chemical property of battery.It is relevant with the finishing of effective dispersion of active material and active material that in fact the performance of battery improves, active material fully should be disperseed in the technical process of cell preparation, do not destroy the structure of active material itself again, more can not make active material broken in dispersion process.The particle diameter of active material such as graphite is generally several microns between tens microns, and the effective grain size of conductive carbon and CNT (carbon nano-tube) is littler, only depends on the stirring intensity of reinforcement dispersing apparatus such as high speed dispersor, mulser, planetary mixer not deal with problems.
In view of this, necessaryly provide a kind of dispersant that the lithium ion battery plus-negative plate material is had better dispersion effect.
Summary of the invention
The objective of the invention is to: provide the lithium ion battery plus-negative plate dispersion of materials agent preferably of a kind of dispersion effect, to improve the performance of lithium ion battery.
In order to realize the foregoing invention purpose, the invention provides the agent of a kind of lithium ion battery plus-negative plate dispersion of materials, the surfactant in the described dispersant is the modification APEO.
The modification group of described modification APEO is one or more of fatty alcohol, aromatic alcohol, polysiloxanes, aromatic acid.Introduce these modification groups and be used for preparing electrode paste on the one hand, need under the situation that guarantees processing characteristics, improve content of active substance as far as possible, macromolecular material such as CMC, SBR, PVDF are added in the effect that the pulp preparation stage mainly has been the suspension active material particle, the molecular weight of general polymerization thing Binder is more than 100,000, and the molecular weight of surfactant (Mw) is about 2000～10000, can in the unit addition, provide more polar group to be adsorbed on the active material particle, stability of slurry is improved.Multi-functional surfactant can improve the hydrophilic close electrolyte performance of active powder such as graphite simultaneously, after the pole piece drying, residue in the pole piece, can also bring into play the wetting property of active material and electrolyte after being prepared into electric core, thereby promote the chemical property of electric core.
The molecular weight of described modification APEO is 2000～10000, the modification APEO is narrower for well with molecular weight distribution, the surfactant of this sized molecules amount and the intermiscibility of solvent are good, on the simultaneously easier surface that is adsorbed in active material, play the effect of stable slurry, use its CMC value (critical micelle concentration) of surfactant of narrow molecular weight distribution less, can reduce the addition of dispersant as far as possible.
The molecular weight of modification group segment is 200～5000 in the described modification APEO, and the best is 1000～2000.Long its flow regime of APEO segment all has adverse effect to responsive to temperature to storing and transporting; The too short then chemical property of segment instability can not be applicable to the operation window voltage (3.0～4.2V) that lithium ion battery is wide.
Also comprise solvent, mould inhibitor and rust inhibitor in the described dispersant.
The mass content of four kinds of materials is in the dispersant: modification APEO 15%～90%; Solvent 5%～80%; Mould inhibitor 1%～2%; Rust inhibitor 1%～4%.
Described solvent is one or more in deionized water, N-methyl pyrrolidone, alcohols or the ethers, also can be the straight or branched hydroxyl of amino or 6～10 carbon of the aromatic radical that contains 6～8 carbon, 3～6 nitrogen.
Described mould inhibitor is long-acting multispectral mould inhibitor.
Described rust inhibitor is organic acid sodium salt.
With respect to prior art, dispersant of the present invention has the following advantages: 1) adding method is simple, has avoided the replacing to original battery preparation technique and equipment; 2) dispersion effect is good, all can reach splendid dispersion effect to conductive agent, active material, shortens the jitter time of above-mentioned active material; 3) applied range, just can be applicable to/negative material preparation in, and all can be suitable for water-based system and solvent borne system; 4) stable electrochemical property is stable in 0～4.5V voltage; 5) can improve the cryogenic property of battery; 6) can improve the security performance of battery, to overcharge, safety test such as drift bolt, side pressure, heavy impact all has improvement.
Description of drawings
Below in conjunction with Figure of description and each specific embodiment, the present invention and useful technique effect thereof are elaborated, wherein:
The slurry that Fig. 1 prepares for various embodiments of the present invention is painted ESEM (SEM) picture behind the pole piece.
Fig. 2 is cyclic voltammetric (CV) curve of embodiment of the invention dispersant in negative pole.
Fig. 3 is the partial enlarged drawing of Fig. 2.
Fig. 4 is cyclic voltammetric (CV) curve of embodiment of the invention dispersant in positive pole.
Embodiment
Modification polyethenoxy ether class dispersant among the present invention is a class all has the fine dispersion effect to the battery plus-negative plate material a dispersant, has good electrochemical, it is that the structure as the modification APEO of dispersant Main Ingredients and Appearance is adjustable on the one hand, thereby can form the product that satisfies the different technologies requirement; The 2nd, dispersant is as a kind of component of electrode material, and it does not influence other active component of battery or has certain improved action, thereby satisfies more demand.Again on the one hand, lithium ion battery is because reduction potential is low, and a lot of auxiliary agents can decompose under low reduction potential, thereby can cause the deterioration of battery performance, can effectively address the aforementioned drawbacks by adding modified poly-epoxy ethene ethers dispersant, the chemical property of battery is optimized.
Reagent and supplier that this specification is related are as shown in table 1.
Table 1, agents useful for same and supplier's detail
| Reagent name | Supplier |
| Polyethylene glycol (600) | Amperex?Technology?Co.，Ltd |
| Graphite | Amperex?Technology?Co.，Ltd |
| Cobalt acid lithium | Amperex?Technology?Co.，Ltd |
| Lithium nickel cobalt manganese | Amperex?Technology?Co.，Ltd |
| LiFePO4 | Amperex?Technology?Co.，Ltd |
| Alloy material | Amperex?Technology?Co.，Ltd |
| Super“p”Li | Timical?Company |
| Carbon nano-tube | Amperex?Technology?Co.，Ltd |
| Kynoar | Amperex?Technology?Co.，Ltd |
| Styrene-butadiene latex | Amperex?Technology?Co.，Ltd |
| Dispersant | Amperex?Technology?Co.，Ltd |
| The N-methyl pyrrolidone | Amperex?Technology?Co.，Ltd |
| PVDF-HEP(PVDF) | Amperex?Technology?Co.，Ltd |
| Electrolyte | Amperex?Technology?Co.，Ltd |
| Sodium carboxymethylcellulose | Amperex?Technology?Co.，Ltd |
One, the preparation of dispersant:
(1) preparation of APEO
Take by weighing the 20kg polyvinyl alcohol and join in the 100L stainless steel cauldron, take by weighing the less solvent of 10kg toluene or other polarity simultaneously and add in the reactor as the bottoming solvent.Close charge door nitrogen (N
2) (494kPa) displacement 3 times, to get rid of the air in the still, begin heat temperature raising to 110 ℃-120 ℃ simultaneously, vacuumize 2-3 time and carry out vacuum dehydration, about 10min of time, and then in still inflated with nitrogen (N
2) to a little higher than normal pressure.Add and analyze pure caustic soda (NaOH) or caustic soda (KOH), and feed an amount of dehydration ethylene oxide gas, reach pre-provisioning request until the feeding amount.During this time, the backflow toluene that need volatilize by cooling also carries out oil water separator and removes the low amounts of water that generates in the reaction, the molecular weight of the viscosity control product by measuring product.When molecular weight near 200～5000 the time, closed loop oxidative ethane inlet valve continues to add about 15kg hydrogenation methyl-silicone oil or amido silicon oil and adds little amount of catalyst and continue to react to molecular weight and be about 1000-8000; Simultaneously, take circumfluence method to slough most solvent and moisture, behind the interior remaining gas of venting still, obtain the intermediate reaction thing of polyoxyethylene ether structure.
(2) preparation of modification polyoxyethylene ether surface active agent
Continue to add about 20kg aliphatic acid and carry out esterification, during the acid number that needs constantly to remove moisture and monitor reaction system, and add a spot of base catalyst.After reaction finishes product is neutralized to neutrality, and takes circumfluence method to slough most solvent, finally obtain molecular weight and be 2000～10000 modification polyoxyethylene ether surface active agent.
(3) preparation of dispersant
Resulting surfactant got 15～90 parts amount of surfactant by quality, 5～80 parts of deionized waters or organic solvent are poured in the mixer, it is evenly mixed with above-mentioned solution to open mixer, and then add 1～2 part mould inhibitor and 1～4 part rust inhibitor mixes, it is standby promptly to prepare qualified dispersant.
Two, dispersant formulation Example
Table 2, dispersant formulation Example
Three, dispersant is applied to the experiment of cathode size
Blank embodiment 3-1: weighing 20kg deionized water adds in the agitator tank, add 200g sodium carboxymethylcellulose dispersing and dissolving then, add carbonaceous conductive agent such as Super " p " Li etc. more successively, active material such as graphite, and butadiene-styrene rubber, finally be prepared into solids content 45%, the qualified cathode size of viscosity 3000～10000mpas is standby.
Application Example 3-2: the dispersant of weighing 40g embodiment 2-1 preparation joins in the agitator tank that fills the 20kg deionized water, dispersed with stirring is even, add 200g sodium carboxymethylcellulose dispersing and dissolving then, add the carbonaceous conductive agent more successively, active material such as graphite, and butadiene-styrene rubber, finally being prepared into solids content 45%, the qualified cathode size of viscosity 3000～10000mpas is standby.
Application Example 3-3: the dispersant of weighing 40g embodiment 2-3 preparation joins in the agitator tank that fills the 20kg deionized water, dispersed with stirring is even, add 200g sodium carboxymethylcellulose dispersing and dissolving then, add conductive nano agent such as carbon nano-tube more successively, active material such as graphite and butadiene-styrene rubber are prepared into solid content 45%, and the qualified cathode size of viscosity 2000～5000mpas is standby.
Four, dispersant is applied to the experiment of anode sizing agent
Blank embodiment 4-1: take by weighing 600kgN-crassitude ketone solvent and join in the agitator tank, add the carbonaceous conductive agent then, Kynoar fully disperses the back to add cobalt acid lithium, further disperses to be prepared into solid content 65%, and the qualified anode sizing agent of viscosity 3000～5000mpas is standby.
Application Example 4-2: the dispersant of weighing 150g embodiment 2-2 preparation joins and disperses in the agitator tank that fills 600kg N-methyl pyrrolidone to stir, add the carbonaceous conductive agent then, Kynoar or other bonding agent fully disperse the back to add cobalt acid lithium, further disperse to be prepared into solid content 65%, the qualified anode sizing agent of viscosity 2000～10000mpas.
Application Example 4-3: the dispersant of weighing 180g embodiment 2-4 preparation joins and disperses in the agitator tank that fills 600kg N-methyl pyrrolidone to stir, add the carbonaceous conductive agent then, Kynoar or other bonding agent fully disperse the back to add LiMn2O4, further disperse to be prepared into solid content 70%, the qualified anode sizing agent of viscosity 2000～5000mpas.
Application Example 4-4: the dispersant of weighing 130g embodiment 2-5 preparation joins and disperses in the agitator tank that fills 600kg N-methyl pyrrolidone to stir, add the carbonaceous conductive agent then, Kynoar bonding agent or other bonding agent fully disperse the back to add lithium nickel cobalt manganese, further disperse to be prepared into solid content 65%, the qualified anode sizing agent of viscosity 2000～5000mpas.
Application Example 4-5: the dispersant of weighing 90g embodiment 2-7 preparation joins and disperses in the agitator tank that fills 600kg N-methyl pyrrolidone to stir, add CNT (carbon nano-tube) then, Kynoar bonding agent or other bonding agent fully disperse the back to add Zinc-lithium alloy material (lithium antimony alloy, the lithium silicon alloy), further disperse to be prepared into solid content 50%%, the qualified anode sizing agent of viscosity 2000～5000mpas.
The preparation of electricity core
The designing requirement that above-mentioned accepted stock is pressed Model (as 383450 square batteries, 053448 square battery, 18650 cylindrical batteries etc.) on coating machine, coat qualified just/cathode pole piece.
Model by design is assembled into electric core with above-mentioned pole piece, and pours into electrolyte and carry out chemical membrane, and is aging, detects the chemical property of electric core, and carries out performance evaluation with electrochemical impedance spectroscopy (EIS) and cyclic voltammetry scan test (CV) scanning pole piece.
Five, beneficial effect experiment
Above-mentioned electric core is carried out high temperature storage, detect electric core security performance by UL 1642 lithium battery safety standards.By new forms of energy company quality control criterion electric core being carried out high temperature performance detects.
1, dispersion effect evaluation
The diaphragm of embodiment 3-1 to 4-5 preparation is carried out analyzing and testing with ESEM (SEM) to the surface and the section of diaphragm.As seen from Figure 1, the diaphragm distribution of particles wherein of not adding dispersant is extremely inhomogeneous, and all there is the phenomenon of uniting in variable grain, and wherein conductive carbon material is united especially obvious; The diaphragm that has added dispersant then be can't see the phenomenon of particle agglomeration, illustrates that the Dispersion of Particles effect is very good.
2, coating performance evaluation
Generally, the problem that occurs in coating process of negative material is less.For positive electrode, because the granule-morphology and the granular size of material itself are different, positive electrode itself contains impurity such as unreacted lithium carbonate and lithium hydroxide in addition, directly causes anode sizing agent gelatin phenomenon can occur in whipping process, and serious gel can cause whole jar of slurry to be scrapped.In addition, slight gel can cause slurry hangover, the cut phenomenon of filming to occur in coating process, like this when being coated with second, the laser head of indication coating operation need find first face starting point of filming just can carry out second coating on the coating machine, if first hangover occurs then entanglement can appear in the position of second coating, can cause the bad bad product of filming.
In addition; for automatic assembly line and manual production line, owing to be to differentiate qualified product and non-qualified product by machine, in case cut occurs; then need to shut down and the 5-10 silver before and after this pole piece disposed to connect again again and reel, can have a strong impact on production capacity and acceptance rate like this.
In actual production, positive plate is coated on the aluminium foil, because aluminium foil is an amphoteric metal, not only can with acid reaction but also can with alkali reaction, because contain considerable residual lithium carbonate and lithium hydroxide in the positive electrode, in storage process, lithium carbonate or lithium hydroxide can absorb airborne moisture, and and then react with metal aluminum foil and to cause diaphragm to come off or the bubbling phenomenon, strong more easy more this class phenomenon that occurs of the alkalescence of material.
Find according to experiment, in anode sizing agent, add a spot of dispersant, can reduce even stop above-mentioned anomaly, the acceptance rate of pole piece is greatly improved.
For further research the present invention reduces the reason of bad product rate, to batch powder add and do not add the slurry that dispersant is prepared into 100kg respectively and test, obtain experimental result as table 3.
Table 3, slurry coating cut situation statistics
As can be seen from Table 3, the slurry viscosity in storage process that does not add dispersant constantly rises, and the slurry viscosity in storage process that has added dispersant constantly descends.Illustrate that the adding of dispersant can effectively control the viscosity of slurry, thereby avoided the generation of gelatin phenomenon from the source.
3, dispersion effect evaluation
Adopting electrochemical impedance spectroscopy (EIS) is 10mm with 1000Hz～1Hz frequency test contact area
2The membrane resistance of identical compacted density, obtain result as shown in table 4.
Table 4 membrane resistance measurement result
By table 4 as seen, under the situation of same coating quality and identical compacted density, the pole piece that has added additive is because electric conducting material and active material are uniformly dispersed, and its pairing membrane resistance obviously reduces, and helps improving the chemical property of battery.
4, to the influence of positive and negative pole material chemical property
With 1480 electrochemical workstations to not adding dispersant (embodiment 3-1) and having added the circular button half-cell that the cathode membrane (embodiment 3-2) of dispersant is prepared into and carried out CV scanning, button cell model: 2032, scanning voltage: 0-2.5V, sweep speed: 20uv/s obtains result shown in Figure 2.In order to observe the influence of dispersant better, the part of Fig. 2 amplified obtain result shown in Figure 3.By Fig. 2 and Fig. 3 as seen, the irreversibility of pole piece oxidation reaction in first CV of having added dispersant is stronger, but overlap fully with the cyclic voltammetry scan curve of normal pole piece after second week, the character that shows surfactant in the pole piece that has added surfactant tends towards stability, and illustrates that dispersant does not have influence to the chemical property of electric core.
Same with 1480 electrochemical workstations the anodal diaphragm (embodiment 4-2) that does not add dispersant (embodiment 4-1) and added dispersant be prepared into circular button half-cell and carry out CV and scan, button cell model: 2032, scanning voltage: 0-4.5V, sweep speed: 20uv/s obtains result as shown in Figure 4.
As seen from Figure 4, for anodal, except that first circulation, the pole piece that has added dispersant is basic the same with the pole piece that does not add dispersant after second week, and do not have how extra redox peak and occur, show that this dispersant can add in the positive electrode system equally.
5, to the influence of full battery performance
The electric core that assembles is changed into, and contrast the electric core that does not add dispersant, the result is as shown in table 5.
The full battery performance of table 5
By table 5 as seen, in electric core pole piece, add a spot of dispersant, the main chemical property of electric core is all had no side effect as coulombic efficiency, positive electrode capacity performance, high low temperature circulation etc. first.In addition, the internal resistance and the high rate performance of electric core had a certain upgrade, illustrate to add the chemical property that dispersant helps to improve electric core.
6, to the influence of battery high temperature performance
Press UL 1642 standards respectively at-20 ℃ ,-10 ℃, 0 ℃, 25 ℃, 45 ℃, embodiment 3-1 to 4-5 is carried out high low temperature volume test under 60 ℃, be that benchmark is investigated the capability retention of electric core under different temperatures with the capacity under 25 ℃, the result is as shown in table 6.
The high temperature performance of table 6, electric core
By table 6 as seen, added the high-temperature behavior not influence of dispersant, the performance electric core low temperature has under been improved, and in positive pole and negative pole, all can reach identical effect, shown that this dispersant has some improvement to the cryogenic property of electric core electric core.
7, to the influence of battery safety
By UL 1642 standards the electric core that embodiment 3-1 to 4-5 prepares has been carried out the test of secure context, the result is as shown in table 7.
The electrochemistry security performance of table 7, electric core
By table 7 as seen, the electric core that has added dispersant is compared with the electric core that does not add dispersant has identical security performance, shows the not influence of security performance of the interpolation of dispersant to electric core.
In sum, dispersant of the present invention has the following advantages: 1) adding method is simple, has avoided the replacing to original battery preparation technique and equipment; 2) dispersion effect is good, and to conductive agent, active material all can reach splendid dispersion effect, shortens the jitter time of above-mentioned active material; 3) applied range, just can be applicable to/negative material preparation in, and all can be suitable for water-based system and solvent borne system; 4) stable electrochemical property is stable in 0～4.5V voltage; 5) can improve the cryogenic property of battery; 6) can improve the security performance of battery, to overcharge, the safety test such as drift bolt, side pressure, heavy impact all is improved.
Claims (10)
1. lithium ion battery plus-negative plate dispersion of materials agent is characterized in that: the surfactant in the described dispersant is the modification APEO.
2. lithium ion battery plus-negative plate dispersion of materials according to claim 1 agent is characterized in that: the modification group of described modification APEO is one or more of fatty alcohol, aromatic alcohol, polysiloxanes, aromatic acid.
3. lithium ion battery plus-negative plate dispersion of materials according to claim 1 agent is characterized in that: the molecular weight of described modification APEO is 2000～10000.
4. lithium ion battery plus-negative plate dispersion of materials according to claim 1 agent is characterized in that: the molecular weight of described modification APEO modification group segment is 200～5000.
5. lithium ion battery plus-negative plate dispersion of materials according to claim 4 agent is characterized in that: molecular weight the best of described modification APEO modification group segment is 1000～2000.
6. according to each described lithium ion battery plus-negative plate dispersion of materials agent in the claim 1 to 5, it is characterized in that: also comprise solvent, mould inhibitor and rust inhibitor in the described dispersant.
7. lithium ion battery plus-negative plate dispersion of materials according to claim 6 agent is characterized in that: the quality percentage composition of each composition is in the dispersant: modification APEO 15%～90%; Solvent 5%～80%; Mould inhibitor 1%～2%; Rust inhibitor 1%～4%.
8. lithium ion battery plus-negative plate dispersion of materials according to claim 6 agent, it is characterized in that: described solvent is one or more in deionized water, N-methyl pyrrolidone, alcohols or the ethers, or contains the straight or branched hydroxyl of amino or 6～10 carbon of the aromatic radical of 6～8 carbon, 3～6 nitrogen.
9. lithium ion battery plus-negative plate dispersion of materials according to claim 6 agent is characterized in that: described mould inhibitor is long-acting multispectral mould inhibitor.
10. lithium ion battery plus-negative plate dispersion of materials according to claim 6 agent is characterized in that: described rust inhibitor is organic acid sodium salt.
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| CN108428865A (en) * | 2018-03-05 | 2018-08-21 | 天臣新能源研究南京有限公司 | A kind of preparation method of lithium ion battery anode slurry |
| CN111129594A (en) * | 2019-12-25 | 2020-05-08 | 宁德新能源科技有限公司 | Electrochemical device and electronic device comprising same |
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| CN113161513A (en) * | 2021-06-13 | 2021-07-23 | 中南大学 | Overcharge-resistant negative electrode, preparation method thereof and lithium ion battery |
| CN114899400A (en) * | 2022-05-11 | 2022-08-12 | 厦门海辰新能源科技有限公司 | Positive electrode slurry, positive electrode plate and lithium battery |
| CN114899400B (en) * | 2022-05-11 | 2023-09-08 | 厦门海辰储能科技股份有限公司 | Positive electrode slurry, positive electrode plate and lithium battery |
| CN115141376A (en) * | 2022-08-01 | 2022-10-04 | 深圳市皓飞实业有限公司 | Dispersing agent for lithium ion battery anode slurry and application thereof |
| CN115141376B (en) * | 2022-08-01 | 2023-12-22 | 深圳市皓飞实业有限公司 | Dispersing agent for lithium ion battery anode slurry and application thereof |
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