CN107565120A - A kind of preparation method of polynary lithium ion battery electrode material - Google Patents
A kind of preparation method of polynary lithium ion battery electrode material Download PDFInfo
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- CN107565120A CN107565120A CN201710753368.9A CN201710753368A CN107565120A CN 107565120 A CN107565120 A CN 107565120A CN 201710753368 A CN201710753368 A CN 201710753368A CN 107565120 A CN107565120 A CN 107565120A
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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
The invention discloses a kind of polynary lithium ion battery electrode material preparation method.The formula of the electrode material is LixMOy·nAOz, active ingredient LixMOyIn M be transition metal, including at least one kind in Ni, Co, Mn, 0.5≤x≤1.2,2≤y≤3；AOyRefer to the coating for being covered in active ingredient surface, wherein, 0≤n≤0.1,1≤z≤2, the thickness of coating is nanoscale.Preparation process is：With presoma metal chloride, in the case where being not added with complexing agent and precipitating reagent, by being thermally formed presoma；Coat presoma after grinding in the same way again；After mixing lithium source in a manner of wet method, pelletized to obtain mixed powder with spray dryer；Then be sintered, cool down after through mix except magnetic obtains product.Electrode material prepared by this method has the characteristics of particle is small, high rate performance is excellent, have extended cycle life, crystallinity is high, security performance is reliable.
Description
Technical field
The present invention relates to the doping of polynary lithium ion battery electrode material, cladding, preparation method, more particularly to nickel cobalt acid
The preparation of the polynary electrode materials such as lithium, nickel ion doped, nickle cobalt lithium manganate, nickel cobalt lithium aluminate, nickel cobalt magnesium lithium and method of modifying.
Background technology
Due to the unsustainable property of primary energy, therefore with the exhaustion of limited fossil energy, and these fossil energy
Pollution of the source to environment, so it is extremely urgent to find a kind of energy of cleaning.At present in the clean energy resource of development, have nuclear energy,
Solar energy, wind energy, tide energy, power station energy etc., although nuclear energy has had a small amount of application, still have certain technology to hinder
Hinder, once there is accident, damaging range is extremely wide, duration overlength, such as Fukushima, Japan nuclear power station incident of leakage；And solar energy,
Wind energy, tide energy, power station etc. have that very big region and cycle are restricted, can only be in few area or in the time limited
The energy of correlation can be effectively collected in.Even if the collected energy is also required to store, in case making during energy peak
With.Lithium ion battery can solve the problem that above mentioned problem, both can technology cleaning, and the energy can be stored in form of electricity.
Although the cost of current lithium ion battery is still too high, development is swift and violent in recent years, has reached 1.5-2.0
Member/Wh, will be suitable with fossil energy cost after cost is down to 1 yuan/Wh, welcomes lithium battery and is widely applied market.Except
Outside cost, lithium ion battery also have two it is great the problem of be not yet fully solved, first, the cycle life of lithium ion battery is also
Fall short of, second, the security reliability of lithium ion battery does not reach a standard completely.
The cycle life and security reliability of lithium ion battery with many factors to close, including electrode material, electrolyte, every
Film, battery manufacturing process and environment, and wherein influence maximum is electrode material.Therefore, the present invention is for cycle performance and peace
A kind of the two problems of full property reliability, there is provided more simple and effective electrode material preparation method.
The content of the invention
In order to solve above technical barrier, the invention provides a kind of preparation side of polynary lithium ion battery electrode material
Method.
The present invention solves the scheme of above technical problem：
A kind of preparation method of polynary lithium ion battery electrode material, the formula of the electrode material is LixMOy·nAOz, it is living
Sexual element LixMOyIn M be transition metal, including at least one kind in Ni, Co, Mn, 0.5≤x≤1.2,2≤y≤3；
AOyRefer to the coating for being covered in active ingredient surface, wherein, 0≤n≤0.1,1≤z≤2, the thickness of coating is nanometer
Level, this method comprise the following steps：
(1) presoma is prepared：Metal chloride contained by presoma is added in pure water and (if necessary to adulterate, then adulterated
Input is wherein jointly for metal chloride contained by the chloride and presoma of metal), stirring is allowed to be uniformly dissolved, be passed through air or
Heating response is carried out after nitrogen under agitation；When reactant forms viscous pasty state, stopping is stirred after adding water washing, then is stood
Ageing；After the completion of ageing plus water adjusts solid content, and material is ground in sand mill, obtains presoma；
(2) presoma (just having this step during the product that only production needs to coat) of cladding is prepared：Metal will be coated
Chloride mixes with presoma obtained by step (1), and stirring is allowed to be uniformly dissolved, and enters under agitation after being passed through air or nitrogen
Row heating response；When reactant formation viscous pasty state, stop stirring after adding water washing, then it is still aging, water is added after the completion of ageing
Adjust solid content, the presoma coated；
(3) pelletize：The lithium after crushing is added into the presoma of cladding obtained by presoma obtained by step (1) or step (2)
Source, after stirring forms the suspension of stable homogeneous, metal hydroxides presoma and lithium source are dried to obtain by spray dryer
Uniform mixed powder；
(4) finished product is prepared：Mixed powder is mounted in into feeding kiln in ceramic saggar to be sintered, passes through to crush after sintering and divides
Level, screening, mix and criticize, except the processes such as magnetic obtain that the polynary lithium ion battery electrode material that can be coated can be adulterated.
Further, the metal chloride contained by described presoma is the chlorination of one or more kinds of transition metal
It is more than one or both of thing, preferably nickel chloride, cobalt chloride, manganese chloride.
Further, described lithium source includes lithium carbonate, lithium hydroxide, lithia, lithium chloride or the organic compound containing lithium
More than one or both of thing, the ratio between amount of material of lithium and presoma metal (mol ratio) is 1-1.15.
Further, the chloride of described cladding metal includes aluminium chloride, magnesium chloride, zinc chloride, zirconium chloride, chlorination
It is more than one or both of cadmium, chromium chloride；It is 0- to coat the ratio between the amount of material of metal and presoma metal (mol ratio)
0.02。
Further, the chloride of doping metals includes aluminium chloride, magnesium chloride, zinc chloride, zirconium chloride, gallium chloride, chlorination
It is more than one or both of lithium；The ratio between amount of material of doping metals and presoma metal is 0.01-0.04；Doping metals are real
Matter is additive, and in the present invention, dopant can not have, and can be a kind of or a variety of.
Further, step (1), the heating-up temperature of step (2) are 100~300 DEG C, preferably 160~260 DEG C.
Further, step (3) spray dryer dry, inlet temperature be 180~300 DEG C, preferably 240~280 DEG C,
Outlet temperature is 100~140 DEG C, preferably 120~140 DEG C.Mixture powder is obtained by spray drying, what this mode obtained
The homogeneous mixture of metal hydroxides presoma and lithium source, not only thoroughly overcomes the problem of dry mixed is uneven, overcomes
Gel method easily lumps, fills the problem of alms bowl and clear alms bowl difficulty, and the inlet temperature being spray-dried is not higher than 300 DEG C, solves
High-temperature blocks the problem of fog-spray nozzle, while outlet temperature is not higher than 140 DEG C, can only dry out so as to reach in the process
Any change will not occur for dry purpose, metal hydroxides presoma.
Further, the hydrochloric acid that step (1), step (2) are evaporated is reclaimed by pure water, the weight not precipitated completely
Metal ion after adding alkali lye precipitation by recycling, and the hydrochloric acid regulation of the pH recovery of clear liquid is to neutrality, and water now is only
Containing sodium chloride, can directly discharge.
The central principle of this preparation method has dependence following three：
(1) metal chloride heats the corresponding hydroxide of generation in water：
MClx+H2O→M(OH)x+HCl↑
Presoma processed (including doping presoma) and the principle coated are in this way, and the hydroxide that precipitates when coating
Thing can just be attached to the surface of presoma；
(2) mode of spray drying only comes out water evaporation, and gel is formed without being to continue with evaporation, is due to i, sprays and do
Dry to form fine powder, convenience fills alms bowl, and directly depression formation gel will lump, not civilian dress alms bowl；Ii, depression formation gel
When, the material of bottom can include more clads, uneven so as to cause, and make uniformity poor；Iii, do not have metal chlorination
Thing enters spray dryer, and hydrogen chloride gas would not be so contained in the outlet of spray dryer, so as to avoid pollution empty
The problem of gas.
(3) after oversintering forms li-ion electrode materials, doped chemical is distributed in crystals, forms the whole of unification
Body, and coating then uniform fold inside electrode material surface is without entrance.
The beneficial effects of the present invention are：
(1) uniformity of products obtained therefrom of the present invention is high, and the method mixed relative to dry mixed, micron order significantly improves,
So as to improve the performance of product.
(2) complexing agents such as ammoniacal liquor, sodium hydroxide and precipitating reagent are not needed in course of reaction of the present invention, not only reduce cost,
And the step of removing ammonia nitrogen can be saved in waste water.
(3) method that the present invention uses, because the content of each metal hydroxides in presoma accumulates not of uniform size, Er Qieqing
Nickel oxide solubility product is minimum, cobalt hydroxide secondly, manganous hydroxide it is minimum, so in the mixed precipitation formed, the most manganese of interior nickel
Minimum, the concentration gradient of nickel, cobalt, manganese from high to low from inside to outside was formed just now, so as to significantly improve the circulation longevity of target product
Life and security reliability.
(4) present invention doping step is completed in presoma preparatory phase, and this wet method forerunner doping is most uniformly, with reference to most
Good mode.
(5) present invention reaches benign and recycled in product process is prepared.The hydrochloric acid that reactive evaporation comes out is by returning
Receive, for two aspects, be on the one hand used for the redissolution for reclaiming precipitation, on the other hand the pH value for wash water is adjusted.
(6) technique of the invention is green, in the industrial water discharged, containing only the sodium chloride of no any harm.
(7) cladding of the invention is also that wet processing is completed, and this directly heat to form precipitation and be attached to forerunner surface
Mode, homogeneous coating film can be both formed on presoma surface, while the thickness of film also allows for controlling.
(8) products obtained therefrom granularity of the present invention reaches Nano grade, and obtained product monocrystalline little particle is reunited less, for making
In terms of electrokinetic cell, high rate performance is more preferably.
(9) when method of the invention thoroughly solves dry process nickelic product, the viscous wall of raw material mixing and cause dispensing not
The problem of quasi-, it is especially suitable for the preparation of nickelic product.
(10) the oxide cladding layers energy high temperature resistant that the present invention obtains, excellent stability, excellent insulating property, therefore compare
It is also obvious more preferable in common material, the cycle life and safety and reliability of this covering material.
Brief description of the drawings
Fig. 1 is the structural representation of products obtained therefrom of the present invention.
Fig. 2 is the XRD spectrum of the resulting materials of embodiment 1.
Fig. 3 is the electron microscope that the resulting materials of embodiment 1 amplify 3000 times.
Fig. 4 is the resulting materials of the embodiment 1 specific capacity-voltage curve of the 20th week.
Embodiment
With reference to specific embodiment, the detailed elaboration of system is done to the present invention, but the present invention is not restricted to this.
Embodiment 1：Prepare and not only undoped but also do not coated LNCMO
(1) presoma prepared.Nickel chloride, cobalt chloride, manganese chloride are pressed into n (Ni):n(Co):N (Mn)=5:2:3 ratio
Example is dissolved in the reactor A equipped with pure water, and the total concentration for making metal ion is 120g/L, after stirring and dissolving, in nitrogen atmosphere
The middle solution by reactor is warming up to 200 DEG C, continues the nitrogen being passed through, and brings the hydrogen chloride evaporated into together with steam
Hydrochloric acid is obtained in absorption cell, until solution stops heating in scattered paste shape, is cooled to room temperature under agitation, after standing 3 hours, use is pure
For water washing presoma until chloride ion content reaches below 100ppm, regulation solid content is 40%, by sand mill by presoma
It is ground, then is pumped into reactor B.
(2) pelletize.With n (Li):The lithium carbonate that n (metal ion)=1.05 ratio is added into B reactors after crushing,
After stirring forms the suspension of stable homogeneous, the EAT for setting spray dryer is 240 DEG C, and leaving air temp is 140 DEG C, is passed through
Spray dryer obtains mixed powder.
(3) finished product is prepared.Mixed powder is mounted in into feeding kiln in ceramic saggar to sinter 13 hours with 950 DEG C of temperature,
After the product cooling burnt till, D50=14.2um product is obtained by crushing.
The powder diffraction spectrum of product is as shown in Figure 2 in the present embodiment.
The exterior appearance under an electron microscope of product is as shown in Figure 3 in the present embodiment.
By the assembling product in the present embodiment into CR2032 button cells, charge and discharge is carried out with 1C multiplying power at a temperature of 25 DEG C
Electrical testing, capacity is 160.8mAh/g first, and the capacity of the 20th circulation volume is 151.8mAh/g, 20 weeks specific capacity-voltage
Curve is as shown in Figure 4.
Embodiment 2：Prepare the LNCAO for only adulterating and not coating
(1) presoma prepared.Nickel chloride, cobalt chloride, aluminium chloride are pressed into n (Ni):n(Co):N (Al)=80：15：5
Ratio is dissolved in the reactor A equipped with pure water, and the total concentration for making metal ion is 135g/L, after stirring and dissolving, in air gas
The solution in reactor is warming up to 260 DEG C in atmosphere, continues the air being passed through, the hydrogen chloride band that will be evaporated together with steam
Enter and hydrochloric acid is obtained in absorption cell, until solution stops heating in scattered paste shape, be cooled to room temperature under agitation, after standing 4 hours, adjust
It is 42% to save solid content, is ground presoma by sand mill, then be pumped into reactor B.
(2) pelletize.With n (Li):The lithium carbonate that n (metal ion)=1.06 ratio is added into B reactors after crushing
It is 42% to adjust solid content, and after stirring forms the suspension of stable homogeneous, the EAT for setting spray dryer is 270 DEG C, is gone out
Air temperature is 130 DEG C, and mixed powder is obtained by spray dryer；
(3) finished product is prepared.Mixed powder is mounted in into feeding kiln in ceramic saggar to sinter 18 hours with 800 DEG C of temperature,
After the product cooling burnt till, D50=6.8um product is obtained by crushing；
By the assembling product in the present embodiment into CR2032 button cells, charge and discharge is carried out with 1C multiplying power at a temperature of 25 DEG C
Electrical testing, capacity is 195.2mAh/g first.
Embodiment 3：Prepare the LNCMAO for undoping and only coating
(1) presoma prepared.Nickel chloride, cobalt chloride, manganese chloride are pressed into n (Ni):n(Co):N (Mn)=6:2:2 ratio
Example is dissolved in the reactor A equipped with pure water, and the total concentration for making metal ion is 130g/L, after stirring and dissolving, in nitrogen atmosphere
The middle solution by reactor is warming up to 300 DEG C, continues the nitrogen being passed through, and brings the hydrogen chloride evaporated into together with steam
Hydrochloric acid is obtained in absorption cell, until solution stops heating in scattered paste shape, room temperature is cooled under agitation, after standing 3.4 hours, adjusts
It is 37% to save solid content, is ground presoma by sand mill, then be pumped into reactor B.
(2) presoma of cladding is prepared.By AlCl3With n (Al):N (Ni+Co+Mg)=0.018:1 ratio input reaction
In kettle B, stirring is allowed to be uniformly dissolved, and the solution in reactor is warming up into boiling in air atmosphere, continues the air being passed through,
Hydrochloric acid is obtained in absorption cell with bringing the hydrogen chloride evaporated into together with steam, until solution in scattered paste shape stop heating,
Room temperature is cooled under stirring, after standing 2 hours, with pure water presoma until chloride ion content reaches below 60ppm, is imported
Into reactor C；
(3) pelletize.With n (Li):The lithium carbonate that n (metal ion)=1.09 ratio is added into C reactors after crushing
It is 42% to adjust solid content, and after stirring forms the suspension of stable homogeneous, the EAT for setting spray dryer is 260 DEG C, is gone out
Air temperature is 135 DEG C, and mixed powder is obtained by spray dryer；
(4) finished product is prepared.Mixed powder is mounted in into feeding kiln in ceramic saggar to sinter 17 hours with 850 DEG C of temperature,
After the product cooling burnt till, D50=10.4um product is obtained by crushing；
By the assembling product in the present embodiment into CR2032 button cells, charge and discharge is carried out with 1C multiplying power at a temperature of 25 DEG C
Electrical testing, capacity is 178.1mAh/g first.
Embodiment 4：Prepare the LNCMgZrO for not only having mixed but also having coated
(1) presoma prepared.Nickel chloride, cobalt chloride, magnesium chloride are pressed into n (Ni):n(Co):N (Mg)=80:16:4
Ratio is dissolved in the reactor A equipped with pure water, and the total concentration for making metal ion is 110g/L, after stirring and dissolving, in air gas
The solution in reactor is warming up to 160 DEG C in atmosphere, continues the air being passed through, the hydrogen chloride band that will be evaporated together with steam
Enter and hydrochloric acid is obtained in absorption cell, stop heating in scattered paste shape until liquid is molten, be cooled to room temperature under agitation, after standing 2.5 hours,
It is 30% to adjust solid content, is ground presoma by sand mill, then be pumped into reactor B.
(2) presoma of cladding is prepared.By ZrCl4 with n (Zr):N (Ni+Co+Mg)=0.02:1 ratio input reaction
In kettle B, stirring is allowed to be uniformly dissolved, and the solution in reactor is warming up into boiling in air atmosphere, continues the air being passed through,
Hydrochloric acid is obtained in absorption cell with bringing the hydrogen chloride evaporated into together with steam, stops heating in scattered paste shape until liquid is molten,
Room temperature is cooled under stirring, after standing 3.5 hours, with pure water presoma until chloride ion content reaches below 80ppm, is led
Enter into reactor C；
(3) pelletize.With n (Li):The hydroxide that n (metal ion)=1.08 ratio is added into C reactors after crushing
Lithium regulation solid content is 32%, and after stirring forms the suspension of stable homogeneous, the EAT for setting spray dryer is 280 DEG C,
Leaving air temp is 120 DEG C, and mixed powder is obtained by spray dryer；
(4) finished product is prepared.Mixed powder is mounted in into feeding kiln in ceramic saggar to sinter 20 hours with 750 DEG C of temperature,
After the product cooling burnt till, D50=7.2um product is obtained by crushing；
By the assembling product in the present embodiment into CR2032 button cells, charge and discharge is carried out with 1C multiplying power at a temperature of 25 DEG C
Electrical testing, capacity is 188.9mAh/g first.
Claims (9)
1. a kind of preparation method of polynary lithium ion battery electrode material, it is characterised in that comprise the following steps：
(1) presoma is prepared：Metal chloride contained by presoma is added in pure water, stirring is allowed to be uniformly dissolved, and is passed through sky
Heating response is carried out after gas or nitrogen under agitation；When reactant formation viscous pasty state, stop stirring after adding water washing, then
It is still aging；After the completion of ageing plus water adjusts solid content, and material is ground in sand mill, obtains presoma；
(2) presoma of cladding is prepared：After the chloride for coating metal is uniformly dissolved, mixed with step (1) gained presoma,
It is passed through after air or nitrogen and carries out heating response under agitation；When reactant formation viscous pasty state, stop after adding water washing
Stirring, then it is still aging, after the completion of ageing plus water adjusts solid content, the presoma coated；
(3) pelletize：The lithium source after crushing is added into the presoma of cladding obtained by presoma obtained by step (1) or step (2), is stirred
Mix after forming the suspension of stable homogeneous, metal hydroxides presoma is dried to obtain by spray dryer and the uniform of lithium source mixes
Close powder；
(4) finished product is prepared：Mixed powder is sintered, after sintering by crushing and classification, screening, mixed batch, except magnetic obtain it is polynary
Lithium ion battery electrode material.
2. the preparation method of polynary lithium ion battery electrode material according to claim 1, it is characterised in that also include mixing
It is miscellaneous, it is described to be doped to put into the metal chloride of the chloride of doping metals and presoma jointly in step (1).
3. the preparation method of polynary lithium ion battery electrode material according to claim 1 or 2, it is characterised in that described
Presoma contained by metal chloride for one or more kinds of transition metal chloride.
4. the preparation method of polynary lithium ion battery electrode material according to claim 1 or 2, it is characterised in that described
Lithium source include more than one or both of lithium carbonate, lithium hydroxide, lithia, lithium chloride or organic compound containing lithium,
The ratio between amount of material of lithium and presoma metal is 1-1.15.
5. the preparation method of polynary lithium ion battery electrode material according to claim 1 or 2, it is characterised in that described
The chloride of cladding metal include aluminium chloride, magnesium chloride, zinc chloride, zirconium chloride, caddy, one or both of chromium chloride
More than；It is 0-0.02 to coat the ratio between amount of material of metal and presoma metal.
6. the preparation method of polynary lithium ion battery electrode material according to claim 2, it is characterised in that described mixes
The chloride of miscellaneous metal include aluminium chloride, magnesium chloride, zinc chloride, zirconium chloride, gallium chloride, one or both of lithium chloride with
On；The ratio between amount of material of doping metals and presoma metal is 0.01-0.04.
7. the preparation method of polynary lithium ion battery electrode material according to claim 1 or 2, it is characterised in that step
(1), the heating-up temperature of step (2) is 100~300 DEG C.
8. the preparation method of polynary lithium ion battery electrode material according to claim 1 or 2, it is characterised in that step
(3) spray dryer is dried, and inlet temperature is 200~300 DEG C, and outlet temperature is 100~140 DEG C.
9. the preparation method of polynary lithium ion battery electrode material according to claim 1 or 2, it is characterised in that step
(1), the hydrochloric acid that step (2) is evaporated is reclaimed by pure water, and the heavy metal ion not precipitated completely is by adding alkali lye
Recycled after precipitation, the hydrochloric acid regulation of the pH recovery of clear liquid comprises only sodium chloride, can directly arranged to neutrality, water now
Put.
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN106025179A (en) * | 2016-06-30 | 2016-10-12 | 湖南桑顿新能源有限公司 | Method for preparing cathode material lithium nickel cobalt aluminate for lithium ion battery by spray drying |
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2017
- 2017-08-28 CN CN201710753368.9A patent/CN107565120A/en active Pending
Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN106025179A (en) * | 2016-06-30 | 2016-10-12 | 湖南桑顿新能源有限公司 | Method for preparing cathode material lithium nickel cobalt aluminate for lithium ion battery by spray drying |
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Application publication date: 20180109 |