CN108550779A - A kind of production method of the aquo-lithium ion battery electrode with high stability - Google Patents
A kind of production method of the aquo-lithium ion battery electrode with high stability Download PDFInfo
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- CN108550779A CN108550779A CN201810178524.8A CN201810178524A CN108550779A CN 108550779 A CN108550779 A CN 108550779A CN 201810178524 A CN201810178524 A CN 201810178524A CN 108550779 A CN108550779 A CN 108550779A
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- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01M—PROCESSES OR MEANS, e.g. BATTERIES, FOR THE DIRECT CONVERSION OF CHEMICAL ENERGY INTO ELECTRICAL ENERGY
- H01M4/00—Electrodes
- H01M4/02—Electrodes composed of, or comprising, active material
- H01M4/04—Processes of manufacture in general
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- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
- Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
- Y02E—REDUCTION OF GREENHOUSE GAS [GHG] EMISSIONS, RELATED TO ENERGY GENERATION, TRANSMISSION OR DISTRIBUTION
- Y02E60/00—Enabling technologies; Technologies with a potential or indirect contribution to GHG emissions mitigation
- Y02E60/10—Energy storage using batteries
Abstract
A kind of production method of the aquo-lithium ion battery electrode with high stability, includes the following steps：The dispersion of S1, PTFE；S2, mixed slurry；S3, slurry thickening；S4, PTFE fiber；It is prepared by S5, electrode.Its advantage is that：Using PTFE dispersion emulsions as the raw material of PTFE particles, after being demulsified to slurry using absolute ethyl alcohol, absolute ethyl alcohol is evaporated using water-bath evaporation mode in thickening step, magnetic stirring function is recycled to bestow shearing force to the electrode slurry of thickening, so that PTFE fiber greatly strengthens the viscosity of electrode slurry and the plasticity and elasticity of electrode batch mixing after drying, so that electrode batch mixing engages closely with collector after compacting, it is not easily to fall off, the resistance of maximum possible reduced between electrode batch mixing and collector.
Description
Technical field
The present invention relates to technical field of lithium ion, specifically a kind of aquo-lithium ion electricity with high stability
The production method of pond electrode.
Background technology
It attempts in nineteen nineties aqueous solution applying to ion for the first time from the research team of J.R.Dahn
In battery and after achieving successfully, it is contemplated that the factor of the sustainable developments such as environmental protection and economic benefit, aquo-lithium ion
The research of battery is just gradually paid attention to.
However, as electrolyte from non-water system to the change of water system environment, the structure and manufacture craft of electrode is also required to do
Corresponding adjustment.For traditional lithium ion battery, used is organic electrolyte, and oiliness bonding agent is commonly used for electricity
The preparation of pole.If but continue to continue to use oiliness bonding agent in aquo-lithium ion battery structure, then electrode active material is in water
It is chemical property in electrolyte to be shielded to a certain extent, is primarily due to oiliness binder to the affine of water
The very poor reason of property.Therefore it is very important with aqueous adhesive to replace oiliness class.PTFE is most widely used
Such aqueous binders, but the viscosity of the substance is not inherent, but needs outer bound pair it is bestowed orientation and shears
Power can embody after so that it is completed fibrosis.
After consulting document and relevant art file in relation to aquo-lithium ion battery on a large scale, do not find in electricity
Have the process that elaborates of viscosity excitation to PTFE in the preparation process of pole, if but PTFE viscosity it is poor, the stabilization of electrode
Property will be by extreme influence.To seriously affect the test of the chemical property of electrode material.Therefore, how solution is provided
The problem of above-mentioned technical problem is current urgent need to resolve.
Invention content
In order to solve above-mentioned technological deficiency, present invention offer preparation method is simple, and orients and improve PTFE (polytetrafluoroethyl-nes
Alkene) viscosity a kind of aquo-lithium ion battery electrode with high stability production method.
A kind of production method of the aquo-lithium ion battery electrode with high stability, includes the following steps：
The dispersion of S1, PTFE：After absolute ethyl alcohol is added in PTFE dispersion emulsions, ultrasonic disperse stays in nothing in mixed liquor
When method observes apparent milky aggregate or precipitation, PTFE dispersions are completed；
Preferably, in step S1, PTFE is 60wt% in PTFE dispersion emulsions, and mixes 50 in every 1gPTFE dispersion emulsions
~200ml absolute ethyl alcohols；
Preferably, in step S1, the ultrasonic disperse time is 30~45min, and changes water every 15min during ultrasonic disperse
Once, prevent water temperature in ultrasonic machine from overheating；
Further, in step S1, PTFE dispersion emulsions are mixed with absolute ethyl alcohol, for being demulsified to PTFE；
S2, mixed slurry：It will be stirred on substance merging magnetic stirring apparatus in step S1 after ultrasound, and stir one on one side
Conductive agent and electrode active material is added in side, is persistently stirred overnight again after sealing, obtains slurry；
In step S2, the dispersion PTFE dosage that is obtained in the dosage of electrode active material and conductive agent and step S1 according to,
Electrode active material：Conductive agent：PTFE is 15:3:2 mass ratio calculates；
Further, in step S2, the conductive agent is acetylene black, and the electrode active material is intercalation materials of li ions；
S3, slurry thickening：By in the slurry merging water bath device by step S2 processing, one side magnetic agitation adds on one side
In hot water bath apparatus water to boil, wait for slurry to toothpaste-like stop heat, take out, seal it is spare；
In step S3, the speed of magnetic agitation is 5r/s；
Preferably, in step S3, when magnetic agitation, water heats in water bath device, to evaporate absolute ethyl alcohol in slurry；
S4, PTFE fiber：The step S3 slurries obtained are placed on magnetic stirring apparatus, are stirred with the rotating speed of 30~40r/s
It mixes, until slurry stops stirring to butyrous, PTFE fiberization is completed；
Preferably, in step S1~S4, slurry is placed in same sealing container and is operated；
It is prepared by S5, electrode：Slurry drying prepared by step S4 obtains electrode batch mixing and is collected in standby in sample box
With；Take collector acetone and absolute ethyl alcohol ultrasonic oil removal treatment 15min respectively, then dry up pack after collector it is spare；Take electricity
Pole batch mixing is shaped through rotary push, then stereotyped electrode batch mixing is squeezed into using pressurize mode in collector one side, will be loaded with
The collector of electrode batch mixing is bent and observes whether electrode batch mixing is tightly combined, if electrode batch mixing edges of regions is without departing from collector
And the side that electrode batch mixing is not contacted with collector is glossy smooth, and the collector for being loaded with electrode batch mixing is restored shape, then 60
DEG C dry 2h, electrode fabrication are completed.
Preferably, in step S5, when collector is bent so that the interior angle of collector bending is 135-150 °；
Preferably, in step S5, the container equipped with slurry is placed in 80 DEG C of baking ovens, dries slurry.
A kind of production method of the aquo-lithium ion battery electrode with high stability of the present invention, its advantage is that：
(1), it using PTFE dispersion emulsions as the raw material of PTFE particles, is demulsified to slurry using absolute ethyl alcohol
Afterwards, absolute ethyl alcohol is evaporated using water-bath evaporation mode in thickening step, recycles electrode of the magnetic stirring function to thickening
Slurry bestows shearing force so that PTFE fiber greatly strengthen electrode slurry viscosity and electrode batch mixing after drying it is plastic
Property and elasticity so that electrode batch mixing engages with collector after compacting close, not easily to fall off, maximum possible reduces electricity
Resistance between pole batch mixing and collector；
(2), traditional electrode, which is often taken, makes wet slurry coated on the mode being compacted after being dried on collector, still
The content of the active material of the electrode made in this way is often depending on the thickness and area of electrode active material layer, so
And the uniformity coefficient of thickness and the size of area are with dependence on coating, roll-in and the stability requirement of punching equipment height.However, for
For small-scale laboratory, purchases these equipment and need certain economic base support, therefore, the method for the present invention is made compared to tradition
Preparation Method has low-cost advantage, and easy to operate, no additional additive, environmentally protective.
Description of the drawings
Fig. 1 is electrode front in embodiment one；
Fig. 2 is in embodiment one, and the SEM of electrode batch mixing schemes；
Fig. 3 to 5 is in embodiment two, and active material is the ultrathin electrodes of cobalt acid lithium in voltage window in different PH electrolyte
Mouth is the Cyclic voltamogram curve of 0~0.92V (vs SCE)；
Fig. 6 is 0.5M Li of the lithium cobaltate cathode material in PH=7 in embodiment three2SO4Cycle characteristics in solution is bent
Line；
Fig. 7 is 0.5M Li of the lithium cobaltate cathode material in PH=7 in embodiment three2SO4First lap charge and discharge in solution
Characteristic curve.
Specific implementation mode
With regard to specific embodiment, the invention will be further described below：
Embodiment one
A kind of production method of the aquo-lithium ion battery electrode with high stability, includes the following steps：
The dispersion of S1, PTFE：0.0445g PTFE dispersion emulsions, 20ml absolute ethyl alcohols are weighed respectively, first disperse PTFE
Lotion is placed in beaker, then absolute ethyl alcohol is instilled with dropper in the beaker equipped with PTFE dispersion emulsions, meanwhile, beaker is shaken,
So that absolute ethyl alcohol enters demulsification to PTFE dispersion emulsions, then with preservative film by after the sealing of beaker mouth, ultrasonic disperse 35min is
It prevents water temperature in ultrasonic machine from overheating, a water is changed per 15min, wait for that solution is uniformly dispersed and can not observe apparent milky white in beaker
When color aggregate or precipitation, complete PTFE dispersions；
S2, mixed slurry：Scattered PTFE in step S1 is placed in magnetic stirrer together with beaker, while to burning
0.20025g cobalt acid lithiums, 0.04005 acetylene black is added in cup one by one, then beaker is closed with preservative film, is persistently stirred overnight；
S3, slurry thickening：By in the beaker merging water bath device equipped with slurry by step S2 processing, open on beaker
The preservative film of sealing, is slowly stirred, simultaneously so that water is heated to boiling in water bath device, waits for that absolute ethyl alcohol evaporates (institute in beaker
Absolute ethyl alcohol is stated by the absolute ethyl alcohol that is added in step S1), slurry becomes thick therewith, until stop heating in toothpaste-like,
Beaker is taken out, is again sealed beaker with preservative film, thickening terminates at this time；
S4, PTFE fiber：The beaker equipped with slurry that step S3 is obtained is placed on magnetic stirring apparatus, with 30r/s's
Rotating speed stirs, until in container after slurry to butyrous exquisiteness, stops stirring, PTFE fiberization is completed；
It is prepared by S5, electrode：The preservative film sealed on beaker is opened, and the beaker equipped with slurry is put into 80 DEG C of baking oven
Slurry is dried, that is, obtain electrode batch mixing and is collected in spare in sample box；
It takes 403 stainless (steel) wire of collector to be cut into the rectangle of 50mm*30mm, is then surpassed respectively with acetone and absolute ethyl alcohol
Sound oil removal treatment 15min, the collector after then taking out cleaning with tweezers are quickly dried up with hair-dryer, and it is standby to be hidden in sealed sample bag
With；
Spare electrode batch mixing 0.04g is weighed, it is fixed then to carry out rotary push to electrode batch mixing with the metal grinding tool of polishing
Type, the electrode batch mixing sheet surface to be observed to sizing in grinding tool slot are smooth standby without electrode batch mixing thin slice is taken out after apparent slight crack
With；The side that electrode batch mixing thin slice is contacted with metal grinding tool slot bottom can be called thin slice reverse side, otherwise be front, electrode is mixed
Material thin slice is placed in clean polishing metal plane and thin slice face down, then collector is placed on thin slice reverse side, together
Sample is on a current collector just vertically downward squeezed into thin slice reverse side with the pressure of 10MPa using the polishing metal plane of a clean surface
In netted collector, the collector for being loaded with electrode batch mixing is taken out after pressurize 1min, bending collector be (collector bending at this time
Interior angle is 145 °) observe whether electrode batch mixing engages closely, if electrode batch mixing edges of regions is without departing from collector and electrode batch mixing
Front is glossy smooth, and the collector for being loaded with electrode batch mixing is taken out, and observation electrode batch mixing region, is the circle of a diameter of 13.3mm
Shape, trimming electrode length is to 27mm, width to 13.3mm, after subsequent 60 DEG C dry 2h, electrode fabrication completion.(as shown in Figure 1)
Observe electrode batch mixing SEM figures (as shown in Figure 2), it is known that the nanofiber formed by PTFE fiber is in electrode batch mixing
Inner Constitution space three-dimensional reticular structure, the structure is included by electrode active material and conductive agent spooling, to press down
Made the dusting of electrode batch mixing, largely enhanced the plasticity and viscosity of electrode batch mixing, thus can and collector
It is tightly engaged into form a stable entirety, is unlikely to that showing for electrode batch mixing disengaging occurs in the various test process to electrode
As.In addition, PTFE chemical inertness, does not influence any Electrochemical results；PTFE fiber reticular structure distribution simultaneously is equal
Even sparse, when system existing for electrode has been applied to electrolyte, more conducively infiltration of the electrolyte to electrode substantially increases
The wetting ability of electrode, the activity cycle of reduce electrode phase before testing.
Embodiment two
With embodiment one the difference is that：To cater to cyclic voltammetry environment, the batch mixing layer of electrode should be as far as possible
It is thin；
Therefore, the electrode batch mixing layer for the electrode made is not squeezed to embedded netted collection completely with clean metal plectrum
The part of fluid is completely exfoliated, and then the remaining part of electrode is again placed under 10Mpa pressure and is compacted simultaneously pressurize 1 minute, complete
The electrode batch mixing layer thickness ultrathin electrodes equal with afflux body thickness are obtained at rear, then by electrode and Pt to electrode and saturation
Calomel reference electrode is assembled into three-electrode structure and is immersed in the 0.5M Li for filling PH=112SO4In the electrolytic cell of solution, and one
Sweep speed is the cyclic voltammetry (as shown in Figures 3 to 5) of 1mV/s in constant voltage window.
When due to cobalt acid lithium as aquo-lithium ion battery positive electrode, electrochemical stability is related with PH, works as pH value
When less than 11, the H in electrolyte+Content is relatively higher, H+It can be embedded in cobalt acid lithium layer structure in the deep discharge stage, by
It is an irreversible procedure to be embedded in hydrogen ion, so that follow-up lithium ion deintercalation process will undergo the electrochemistry pole of bigger
Change, leads to cobalt acid lithium cyclicity severe exacerbation.In addition no matter in charging or discharge process, as lithium ion is in cobalt acid lithium crystalline substance
Deintercalation in lattice, material will undergo phase transformation three times, and should correspond to three pairs of redox peaks pair respectively in cyclic voltammetry curve.From
Corresponding curve can see in Fig. 5 to Fig. 7, three pairs of apparent redox peaks pair, and with the increase of cycle-index, envelope
Closed curve area contraction trend increases with pH value and is slowed down, and demonstrates and reduces H in electrolyte by the way that pH value to be turned up+The side of concentration
Formula is inhibited by the phenomenon that hydrogen ion insertion caused cyclicity deterioration；
In addition, cobalt acid lithium, as a kind of positive layer structure removal lithium embedded combination materials, deep charge can destroy its space knot
Structure, in order to observe its complete triple phase transformation, goes out to can also deteriorate its cyclicity to a certain extent in the positive half-turn section of curve
Just mean to enter deep charge state when double phase transformation after now, in the cyclic voltammetry curve that pH value is 11 still may be used
To see certain curve shrinkage trend, however it is caused by electrode is unstable that it, which is not,.To cater to test, thickness of electrode is controlled
Very little is made, suitable with afflux body thickness, electrode batch mixing bearing capacity is very low, therefore it is required that being engaged between electrode batch mixing and collector
Secure rigid, it is seen that electrode stability is required very high.From test result it can be seen that the electrode made by the method for the invention
It has good stability, the variation of the chemical property of electrode active material can be showed completely and embodies external environment to material property
Influence.
Embodiment three
With embodiment one the difference is that：
By prepared electrode mechanical energy constant current charge-discharge test：By electrode and Pt to electrode and saturated calomel reference electrode
It is assembled into three-electrode structure and is immersed in the 0.5M Li for filling PH=72SO4Constant current charge-discharge test is carried out in the electrolytic cell of solution；
Be illustrated in figure 6 lithium cobaltate cathode material PH=7 0.5M Li2SO4Cycle characteristics curve in solution, voltage
Window is 0~0.9V (vs SCE), current density 71.5mA/g, and the cycle number of turns 100 is enclosed；Fig. 7 is that lithium cobaltate cathode material exists
The 0.5M Li of PH=72SO4First lap charge-discharge characteristic curve in solution.
Constant current charge-discharge curve characterization is a kind of long-range cycle performance of electrode active material, and it is special to be different from cyclic voltammetric
Property, the latter is a kind of opposite short distance means of testing, primarily to probing into the chemical property and stability of material.
As can see from Figure 6 the coulombic efficiency of material experienced most start less than ten circle after, numerical value is protected
It holds 100%, stablizes extend to the 100th circle always, specific discharge capacity line smoothing, without apparent fluctuation.Before being indicated above electrode
The problem of phase soak time is short, and test midway falls off there is no electrode batch mixing.
The coulomb effect of the relatively low mainly test first lap of cobalt acid lithium entirety specific capacity value in Fig. 6 is caused as seen from Figure 7
Caused by rate is relatively low, reason is that electrolytic solution cell pH value is too low (PH=7), causes in test first lap charging stage hydrogen
Ion is largely embedded among cobalt acid lithium lattice, is caused activation polarization to increase, is reduced discharge capacity for the first time.Right curve electric discharge is flat
Platform is apparent, illustrates that lower specific discharge capacity is not that bad the caused ohmic polarization of Fabrication Technology of Electrode is too big caused
's.
In conjunction with above-described embodiment one to three, surface makes electrode by the method for the invention, and fabrication cycle is short, green ring
It protects, of low cost, stable structure, and all kinds of electrochemical property tests can be competent at.
The foregoing is merely presently preferred embodiments of the present invention, is not intended to limit the invention, it is all the present invention spirit and
Within principle, any modification, equivalent replacement, improvement and so on should all be included in the protection scope of the present invention.
Claims (7)
1. a kind of production method of the aquo-lithium ion battery electrode with high stability, it is characterised in that：Include the following steps
The dispersion of S1, PTFE：After absolute ethyl alcohol is added in PTFE dispersion emulsions, ultrasonic disperse, staying in mixed liquor can not see
When measuring apparent milky aggregate or precipitation, PTFE dispersions are completed；
S2, mixed slurry：It will stir on substance merging magnetic stirring apparatus in step S1 after ultrasound, and add while stirring
Enter conductive agent and electrode active material, be persistently stirred overnight again after sealing, obtains slurry；
S3, slurry thickening：By in the slurry merging water bath device by step S2 processing, one side magnetic agitation heats water on one side
In bath apparatus water to boil, wait for slurry to toothpaste-like stop heat, take out, seal it is spare；
S4, PTFE fiber：The step S3 slurries obtained are placed on magnetic stirring apparatus, are stirred with the rotating speed of 30~40r/s, directly
To slurry to butyrous, stop stirring, PTFE fiberization is completed；
It is prepared by S5, electrode：Slurry drying prepared by step S4 obtains electrode batch mixing and is collected in spare in sample box；It takes
Collector acetone and the ultrasonic oil removal treatment 15min of absolute ethyl alcohol difference, then packed after drying up spare；Take electrode batch mixing through rotation
Pressing sizing, then stereotyped electrode batch mixing is squeezed into using pressurize mode in collector one side, the collection of electrode batch mixing will be loaded with
Fluid is bent and observes whether electrode batch mixing is tightly combined, if electrode batch mixing edges of regions without departing from collector and electrode batch mixing not
The side contacted with collector is glossy smooth, and the collector for being loaded with electrode batch mixing is restored shape, then 60 DEG C of dry 2h, electrode
It completes.
2. method according to claim 1, it is characterised in that：In step S1, PTFE is 60wt% in PTFE dispersion emulsions, and
50~200ml absolute ethyl alcohols are mixed in per 1gPTFE dispersion emulsions.
3. method according to claim 1, it is characterised in that：In step S1, the ultrasonic disperse time is 30~45min, and super
It is primary that every 15min water is changed in sound dispersion process.
4. method according to claim 1, it is characterised in that：In step S2, the dosage of electrode active material and conductive agent with
The dispersion PTFE dosage obtained in step S1, according to electrode active material：Conductive agent：PTFE is 15:3:2 mass ratio calculates.
5. method according to claim 1, it is characterised in that：In step S2, the conductive agent is acetylene black, the electrode active
Property material be intercalation materials of li ions.
6. method according to claim 1, it is characterised in that：In step S1~S4, slurry be placed in same sealing container into
Row operation.
7. method according to claim 1, it is characterised in that：In step S5, when collector is bent so that collector bending
Interior angle is 135-150 °.
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Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN109742316A (en) * | 2018-11-27 | 2019-05-10 | 湖北大学 | A kind of water system sodium-ion battery electrode and the preparation method and application thereof |
| CN109768329A (en) * | 2018-12-04 | 2019-05-17 | 湖北大学 | The construction method of mixed aquo-lithium ion battery system based on cobalt acid lithium and active carbon |
| CN110176573A (en) * | 2019-04-28 | 2019-08-27 | 湖北大学 | A kind of modification method of lithium ion cell electrode production |
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| CN101685710A (en) * | 2008-09-26 | 2010-03-31 | 通用电气公司 | Methods for preparing composition and sheet containing composition as well as electrode containing sheet |
| CN105304906A (en) * | 2015-09-24 | 2016-02-03 | 山东润昇电源科技有限公司 | Flexible lithium ion battery cathode and manufacturing method thereof |
| CN106784857A (en) * | 2017-01-06 | 2017-05-31 | 深圳市德方纳米科技股份有限公司 | A kind of lithium ion battery water system primary coat collector and its preparation method and application |
| CN107134563A (en) * | 2017-06-13 | 2017-09-05 | 中国电子新能源（武汉）研究院有限责任公司 | Sodium-ion battery positive plate and preparation method thereof |
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| CN101685710A (en) * | 2008-09-26 | 2010-03-31 | 通用电气公司 | Methods for preparing composition and sheet containing composition as well as electrode containing sheet |
| CN105304906A (en) * | 2015-09-24 | 2016-02-03 | 山东润昇电源科技有限公司 | Flexible lithium ion battery cathode and manufacturing method thereof |
| CN106784857A (en) * | 2017-01-06 | 2017-05-31 | 深圳市德方纳米科技股份有限公司 | A kind of lithium ion battery water system primary coat collector and its preparation method and application |
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| Publication number | Priority date | Publication date | Assignee | Title |
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| CN109742316A (en) * | 2018-11-27 | 2019-05-10 | 湖北大学 | A kind of water system sodium-ion battery electrode and the preparation method and application thereof |
| CN109742316B (en) * | 2018-11-27 | 2021-09-21 | 湖北大学 | Water system sodium ion battery electrode and preparation method and application thereof |
| CN109768329A (en) * | 2018-12-04 | 2019-05-17 | 湖北大学 | The construction method of mixed aquo-lithium ion battery system based on cobalt acid lithium and active carbon |
| CN109768329B (en) * | 2018-12-04 | 2021-12-10 | 太原科技大学 | Construction method of mixed type water system lithium ion battery system based on lithium cobaltate and active carbon |
| CN110176573A (en) * | 2019-04-28 | 2019-08-27 | 湖北大学 | A kind of modification method of lithium ion cell electrode production |
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