CN102064326B - The agent of lithium ion battery plus-negative plate dispersion of materials - Google Patents
The agent of lithium ion battery plus-negative plate dispersion of materials Download PDFInfo
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Abstract
The invention discloses the agent of a kind of lithium ion battery plus-negative plate dispersion of materials, the surfactant in described dispersant is modification APEO.Relative to prior art, dispersant of the present invention has the following advantages: 1) adding method is simple; 2) dispersion effect is good; 3) applied range; 4) stable electrochemical property; 5) cryogenic property of battery can be improved; 6) can improve the security performance of battery, to overcharging, drift bolt, side pressure, the safety test such as heavy impact be all improved.
Description
Technical field
The present invention relates to a kind of dispersant, especially a kind of dispersant lithium ion battery plus-negative plate material being had to better dispersion effect.
Background technology
Lithium ion battery is owing to having the advantages such as energy density is high, operating voltage is high, temperature limit is wide, have extended cycle life, and be widely used as the power supply of various mobile device, in the fields such as Aeronautics and Astronautics, navigation, automobile, Medical Devices, even progressively replace other conventional batteries, especially its high-energy-density is especially for significant contribution has been made in the miniaturization of mobile device.
Usually the difficulties in dispersion of effective substance as conductive carbon, active material (as graphite, cobalt acid lithium, LiMn2O4, lithium nickel cobalt manganese etc.) is had in lithium ion battery preparation process, cause the performance of battery to be not in full use, have impact on battery energy density and promote and the application of lithium ion battery in the field such as high/low temperature, safety.
In order to overcome above-mentioned defect, usually adopting the positive and negative pole material of better structure as offspring, carbon encapsulated material and nano modified material etc., although some performance of battery can be improved like this, significantly can not improve the chemical property of battery.The performance of battery improves in fact relevant with effective dispersion of active material and the finishing of active material, active material fully should be disperseed in technical process prepared by battery, do not destroy the structure of active material itself again, active material more can not be made broken in dispersion process.The particle diameter of active material as graphite is generally between several micron to tens micron, and the effective grain size of conductive carbon and CNT (carbon nano-tube) is less, only can not deal with problems by strengthening dispersing apparatus such as the stirring intensity of high speed dispersor, mulser, planetary mixer.
In view of this, necessaryly a kind of dispersant lithium ion battery plus-negative plate material being had to better dispersion effect is provided.
Summary of the invention
The object of the invention is to: provide the agent of a kind of dispersion effect good lithium ion battery plus-negative plate dispersion of materials, to improve the performance of lithium ion battery.
In order to realize foregoing invention object, the invention provides the agent of a kind of lithium ion battery plus-negative plate dispersion of materials, the surfactant in described dispersant is modification APEO.
The modified group of described modification APEO be fatty alcohol, aromatic alcohol, polysiloxanes, aromatic acid one or more.Introduce these modified groups on the one hand in electrode slurry preparation, need the content as far as possible improving active material when ensureing processing characteristics, the be added in stock preparation stage of macromolecular material as CMC, SBR, PVDF mainly plays suspended active compounds 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 unit addition, provide more polar group to be adsorbed on active material particle, the stability of slurry is improved.Multi-functional surfactant can improve the hydrophilic close electrolyte performance of active powder material as graphite simultaneously, when residuing in pole piece after pole piece drying, the wetting property of active material and electrolyte can also be played after being prepared into battery core, thus promote the chemical property of battery core.
The molecular weight of described modification APEO is 2000 ~ 10000, modification APEO is as well narrower with molecular weight distribution, the surfactant of this sized molecules amount and the intermiscibility of solvent good, more easily be adsorbed on the surface of active material simultaneously, play the effect of stable slurry, use its CMC value (critical micelle concentration) of surfactant of narrow molecular weight distribution less, the addition of dispersant can be reduced as far as possible.
In described modification APEO, the molecular weight of modified group segment is 200 ~ 5000, and the best is 1000 ~ 2000.APEO segment its flow regime long, to responsive to temperature, all has adverse effect to storage and transport; The too short then chemical property of segment is unstable, can not be applicable to the operation window voltage (3.0 ~ 4.2V) that lithium ion battery is wide.
Solvent, mould inhibitor and rust inhibitor is also comprised in described dispersant.
In dispersant, the mass content of four kinds of materials is: modification APEO 15% ~ 90%; Solvent 5% ~ 80%; Mould inhibitor 1% ~ 2%; Rust inhibitor 1% ~ 4%.
Described solvent is one or more in deionized water, 1-METHYLPYRROLIDONE, alcohols or ethers, also can be the straight or branched hydroxyl containing the aromatic radical of 6 ~ 8 carbon, the amino of 3 ~ 6 nitrogen or 6 ~ 10 carbon.
Described mould inhibitor is long-acting multispectral mould inhibitor.
Described rust inhibitor is organic acid sodium salt.
Relative to prior art, dispersant of the present invention has the following advantages: 1) adding method is simple, avoids 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, can be applicable in the preparation of positive/negative material, 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) cryogenic property of battery can be improved; 6) can improve the security performance of battery, to overcharging, drift bolt, side pressure, the safety test such as heavy impact be all improved.
Accompanying drawing explanation
Below in conjunction with Figure of description and each specific embodiment, the present invention and Advantageous Effects thereof are described in detail, wherein:
Fig. 1 is ESEM (SEM) picture after pole piece painted by slurry prepared by various embodiments of the present invention.
Fig. 2 is the cyclic voltammetric of embodiment of the present invention dispersant in negative pole (CV) curve.
Fig. 3 is the partial enlarged drawing of Fig. 2.
Fig. 4 is the cyclic voltammetric of embodiment of the present invention dispersant in positive pole (CV) curve.
Embodiment
Modification polyethenoxy ether class dispersant in the present invention is that a class all has the dispersant of fine dispersion effect to battery plus-negative plate material, there is good chemical property, it is on the one hand be adjustable as the structure of the modification APEO of dispersant Main Ingredients and Appearance, thus can form the product meeting different technologies requirement; Two is dispersant a kind of components as electrode material, and it does not affect other active component of battery or have certain improved action, thus meets more demand.Again on the one hand, lithium ion battery due to reduction potential low, a lot of auxiliary agent can decompose under low reduction potential, thus can cause the deterioration of battery performance, effectively can address the aforementioned drawbacks by adding modified poly-epoxy ethene ethers dispersant, the chemical property of battery is optimized.
Reagent involved by this specification and supplier as shown in table 1.
Table 1, agents useful for same and supplier are detailed
| 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 |
| 1-METHYLPYRROLIDONE | 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
Taking 20kg polyvinyl alcohol joins in 100L stainless steel cauldron, takes 10kg toluene or the less solvent of other polarity adds in reactor as bottoming solvent simultaneously.Close charge door nitrogen (N
2) (494kPa) replace 3 times, to get rid of the air in still, start to be heated to 110 DEG C-120 DEG C, vacuumize 2-3 time and carry out vacuum dehydration, the time is about 10min simultaneously, and then to inflated with nitrogen (N in still
2) to a little higher than normal pressure.Add and analyze pure caustic soda (NaOH) or caustic soda (KOH), and pass into appropriate dehydration ethylene oxide gas, until intake reaches pre-provisioning request.Period, need to remove by cooling the refluxing toluene that volatilizes and carrying out oil water separator a small amount of water generated in reaction, controlled the molecular weight of product by the viscosity measuring product.When molecular weight close to 200 ~ 5000 time, close oxirane inlet valve, continue to add about 15kg hydrogenating methyl silicone oil or amido silicon oil and add a small amount of catalyst and continue reaction to molecular weight and be about 1000-8000; Meanwhile, take circumfluence method to slough most solvent and moisture, after gas remaining in 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, period needs the acid number constantly removing moisture and monitoring reaction system, and adds a small amount of base catalyst.After reaction terminates, product is neutralized to neutrality, and takes circumfluence method to slough most solvent, finally obtain the modification polyoxyethylene ether surface active agent that molecular weight is 2000 ~ 10000.
(3) preparation of dispersant
Obtained surfactant is got the amount of surfactant of 15 ~ 90 parts by quality, 5 ~ 80 parts of deionized waters or organic solvent are poured in mixer, open mixer above-mentioned solution is mixed evenly, and then add the mould inhibitor of 1 ~ 2 part and the rust inhibitor of 1 ~ 4 part mixes, namely prepare qualified dispersant for subsequent use.
Two, dispersant formulation embodiment
Table 2, dispersant formulation embodiment
Three, application of dispersant is in the experiment of cathode size
Blank Example 3-1: weigh 20kg deionized water and add in agitator tank, then 200g sodium carboxymethylcellulose dispersing and dissolving is added, add carbonaceous conductive agent more successively as Super " p " Li etc., active material is as graphite, and butadiene-styrene rubber, finally be prepared into solids content 45%, the qualified cathode size of viscosity 3000 ~ 10000mpas is for subsequent use.
Dispersant prepared by Application Example 3-2: weighing 40g embodiment 2-1 joins in the agitator tank filling 20kg deionized water, dispersed with stirring is even, then 200g sodium carboxymethylcellulose dispersing and dissolving is added, add carbonaceous conductive agent successively again, active material is as graphite, and butadiene-styrene rubber, be finally prepared into solids content 45%, the qualified cathode size of viscosity 3000 ~ 10000mpas is for subsequent use.
Dispersant prepared by Application Example 3-3: weighing 40g embodiment 2-3 joins in the agitator tank filling 20kg deionized water, dispersed with stirring is even, then 200g sodium carboxymethylcellulose dispersing and dissolving is added, add conductive nano agent more successively as carbon nano-tube, 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 for subsequent use.
Four, application of dispersant is in the experiment of anode sizing agent
Blank Example 4-1: take 600kgN-methyl pyrrolidone solvent and join in agitator tank, then carbonaceous conductive agent is added, add cobalt acid lithium after Kynoar fully disperses, dispersion is prepared into solid content 65% further, and the qualified anode sizing agent of viscosity 3000 ~ 5000mpas is for subsequent use.
Dispersant prepared by Application Example 4-2: weighing 150g embodiment 2-2 joins dispersion in the agitator tank filling 600kgN-methyl pyrrolidone and stirs, then carbonaceous conductive agent is added, cobalt acid lithium is added after Kynoar or other bonding agent fully disperse, further dispersion is prepared into solid content 65%, the qualified anode sizing agent of viscosity 2000 ~ 10000mpas.
Dispersant prepared by Application Example 4-3: weighing 180g embodiment 2-4 joins dispersion in the agitator tank filling 600kgN-methyl pyrrolidone and stirs, then carbonaceous conductive agent is added, LiMn2O4 is added after Kynoar or other bonding agent fully disperse, further dispersion is prepared into solid content 70%, the qualified anode sizing agent of viscosity 2000 ~ 5000mpas.
Dispersant prepared by Application Example 4-4: weighing 130g embodiment 2-5 joins dispersion in the agitator tank filling 600kgN-methyl pyrrolidone and stirs, then carbonaceous conductive agent is added, lithium nickel cobalt manganese is added after Kynoar bonding agent or other bonding agent fully disperse, further dispersion is prepared into solid content 65%, the qualified anode sizing agent of viscosity 2000 ~ 5000mpas.
Dispersant prepared by Application Example 4-5: weighing 90g embodiment 2-7 joins dispersion in the agitator tank filling 600kgN-methyl pyrrolidone and stirs, then CNT (carbon nano-tube) is added, Zinc-lithium alloy material (lithium antimony alloy is added after Kynoar bonding agent or other bonding agent fully disperse, Li-Si alloy), further dispersion is prepared into solid content 50%%, the qualified anode sizing agent of viscosity 2000 ~ 5000mpas.
Prepared by battery core
The designing requirement of above-mentioned accepted stock being pressed Model (as 383450 square batteries, 053448 square battery, 18650 cylindrical batteries etc.) coats qualified positive/negative pole piece on coating machine.
By the model of design, above-mentioned pole piece is assembled into battery core, and pour into electrolyte and carry out chemical membrane, aging, detect the chemical property of battery core, and test (CV) with electrochemical impedance spectroscopy (EIS) and cyclic voltammetry scan and scan pole piece and carry out performance evaluation.
Five, beneficial effect experiment
Above-mentioned battery core is carried out high temperature storage, detects battery core security performance by UL1642 lithium battery safety standard.By New Energy Corporation's quality control standard, high temperature performance detection is carried out to battery core.
1, dispersion effect evaluation
To the surface of diaphragm and section, analyzing and testing is carried out to diaphragm ESEM (SEM) prepared by embodiment 3-1 to 4-5.As seen from Figure 1, the diaphragm distribution of particles wherein of not adding dispersant is extremely uneven, and variable grain all exists phenomenon of uniting, and wherein conductive carbon material is united especially obvious; The diaphragm that with the addition of dispersant then can't see the phenomenon of particle agglomeration, illustrates that Granular composite effect is very good.
2, coating performance evaluation
Under normal circumstances, negative material produced problem in coating process is less.For positive electrode, due to the granule-morphology of material itself and granular size different, positive electrode itself is containing the impurity such as unreacted lithium carbonate and lithium hydroxide in addition, and directly cause anode sizing agent in whipping process, there will be gelatin phenomenon, serious gel can cause whole tank slurry to be scrapped.In addition, slight gel can cause slurry in coating process, occur hangover, film cut phenomenon, like this when painting second, coating machine indicate the laser head of painting work need to find first surface film starting point just can carry out second coating, if hangover appears in first surface, the position of second coating there will be entanglement, can cause the bad bad product of film.
In addition; for automatic assembly line and manual production line, owing to being by machine to differentiate qualified product and non-qualified product, once there is cut; then need to shut down and the 5-10 silver before and after this pole piece is disposed again to connect again to reel, production capacity and acceptance rate can be had a strong impact on like this.
In actual production, positive plate is coated on aluminium foil, because aluminium foil is amphoteric metal, not only can with acid reaction but also can with alkali reaction, owing to containing considerable residual lithium carbonate and lithium hydroxide in positive electrode, in storage process, lithium carbonate or lithium hydroxide can absorb the moisture in air, and and then react with metal aluminum foil and cause diaphragm to come off or bubbling phenomenon, more easily there is this kind of phenomenon more by force in the alkalescence of material.
Experimentally find, in anode sizing agent, add a small amount of dispersant, can reduce and even stop above-mentioned anomaly, the acceptance rate of pole piece is greatly improved.
Reduce the reason of bad product rate to study the present invention further, to batch powder add and do not add the slurry that dispersant is prepared into 100kg respectively and test, obtain the 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 not adding dispersant constantly rises, and the slurry viscosity in storage process that with the addition of dispersant constantly declines.What dispersant was described adds the viscosity that effectively can control slurry, thus avoids the generation of gelatin phenomenon from source.
3, dispersion effect evaluation
Adopt electrochemical impedance spectroscopy (EIS) with 1000Hz ~ 1Hz frequency test contact area for 10mm
2the membrane resistance of identical compacted density, obtain result as shown in table 4.
Table 4 membrane resistance measurement result
From table 4, when same coating quality is with identical compacted density, the pole piece adding additive is uniformly dispersed due to electric conducting material and active material, and the membrane resistance corresponding to it obviously reduces, and is conducive to the chemical property improving battery.
4, on the impact of positive and negative pole material chemical property
With 1480 electrochemical workstations, CV scanning is carried out to the circular button half-cell that the cathode membrane (embodiment 3-2) of not adding dispersant (embodiment 3-1) and with the addition of dispersant is prepared into, button cell model: 2032, scanning voltage: 0-2.5V, sweep speed: 20uv/s, obtains the result shown in Fig. 2.In order to observe the impact of dispersant better, the local of Fig. 2 is amplified to the result obtained shown in Fig. 3.From Fig. 2 and Fig. 3, the irreversibility that with the addition of pole piece oxidation reaction in first CV of dispersant is stronger, but overlap completely with the cyclic voltammetry scan curve of normal pole piece after second week, the character showing to the addition of surfactant in the pole piece of surfactant tends towards stability, and illustrates that the chemical property of dispersant on battery core is without impact.
Same use 1480 electrochemical workstation is prepared into circular button half-cell to the positive pole diaphragm (embodiment 4-2) not adding dispersant (embodiment 4-1) and with the addition of dispersant and carries out CV scanning, 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 positive pole, except first circulation, the pole piece second week that with the addition of dispersant is later basic the same with the pole piece not adding dispersant, and occur without how extra redox peak, show that this dispersant can add in positive electrode system equally.
5, on the impact of full battery performance
Change into the battery core assembled, and the battery core of dispersant is not added in contrast, result is as shown in table 5.
The full battery performance of table 5
From table 5, in battery core pole piece, add a small amount of dispersant, main chemical property such as initial coulomb efficiency, positive electrode capacity performance, the high/low temperature circulation etc. of battery core are all had no side effect.In addition, the internal resistance of battery core and high rate performance are had a certain upgrade, the chemical property adding dispersant and contribute to improving battery core is described.
6, on the impact of battery high temperature performance
By UL1642 standard respectively at-20 DEG C ,-10 DEG C, 0 DEG C, 25 DEG C, 45 DEG C, carry out high/low temperature volume test at 60 DEG C to embodiment 3-1 to 4-5, with the capacity at 25 DEG C for benchmark investigates battery core capability retention at different temperatures, result is as shown in table 6.
The high temperature performance of table 6, battery core
From table 6, with the addition of the high-temperature behavior of dispersant on battery core does not affect, and improves, and all can reach identical effect to the performance under battery core low temperature in positive pole and negative pole, shows that the cryogenic property of this dispersant to battery core has some improvement.
7, on the impact of battery safety
Carried out the test of secure context by UL1642 standard to battery core prepared by embodiment 3-1 to 4-5, result is as shown in table 7.
The electrochemistry security performance of table 7, battery core
From table 7, the battery core that with the addition of dispersant has identical security performance compared with the battery core of not adding dispersant, shows that the security performance of the interpolation of dispersant on battery core does not affect.
In sum, dispersant of the present invention has the following advantages: 1) adding method is simple, avoids 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, can be applicable in the preparation of positive/negative material, 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) cryogenic property of battery can be improved; 6) can improve the security performance of battery, to overcharging, drift bolt, side pressure, the safety test such as heavy impact be all improved.
Claims (5)
1. a lithium ion battery plus-negative plate dispersion of materials agent, is characterized in that: the surfactant in described dispersant is modification APEO, and the molecular weight of described modification APEO is 2000 ~ 10000; The modified group of described modification APEO be fatty alcohol, aromatic alcohol, polysiloxanes, aromatic acid one or more, the molecular weight of modified group segment is 1000 ~ 2000; Solvent, mould inhibitor and rust inhibitor is also comprised in described dispersant.
2. lithium ion battery plus-negative plate dispersion of materials according to claim 1 agent, is characterized in that: in dispersant, the mass percentage of each composition is: modification APEO 15% ~ 90%; Solvent 5% ~ 80%; Mould inhibitor 1% ~ 2%; Rust inhibitor 1% ~ 4%.
3. lithium ion battery plus-negative plate dispersion of materials according to claim 1 agent, is characterized in that: described solvent is one or more in deionized water, 1-METHYLPYRROLIDONE, alcohols or ethers.
4. lithium ion battery plus-negative plate dispersion of materials according to claim 1 agent, is characterized in that: described mould inhibitor is long-acting multispectral mould inhibitor.
5. lithium ion battery plus-negative plate dispersion of materials according to claim 1 agent, is characterized in that: described rust inhibitor is organic acid sodium salt.
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| CN104143633B (en) * | 2014-07-31 | 2017-06-30 | 深圳市振华新材料股份有限公司 | The positive electrode that element microemulsified cladding process is made, preparation method and application |
| CN107978728A (en) * | 2017-10-31 | 2018-05-01 | 旭成（福建）科技股份有限公司 | A kind of lithium ion battery coating material and coating method |
| 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 |
| CN110265627B (en) | 2018-09-28 | 2020-09-29 | 宁德时代新能源科技股份有限公司 | Positive electrode plate and lithium ion secondary battery |
| CN117059876A (en) * | 2019-12-25 | 2023-11-14 | 宁德新能源科技有限公司 | Electrochemical device and electronic device comprising same |
| CN113161513A (en) * | 2021-06-13 | 2021-07-23 | 中南大学 | Overcharge-resistant negative electrode, preparation method thereof and lithium ion 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 |
| 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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Effective date of registration: 20180614 Address after: 352100 Xingang Road, Zhangwan Town, Jiaocheng District, Ningde, Fujian 1 Patentee after: Ningde Amperex Technology Ltd. Address before: 523080 new energy technology park, Baima management area, Nancheng District, Dongguan, Guangdong Patentee before: Dongguan New Energy Source Electronic Sci-Tech Co., Ltd. |
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