CN107180961A - A kind of method of modifying of the lithium-rich manganese-based layered cathode material of alumina-coated - Google Patents
A kind of method of modifying of the lithium-rich manganese-based layered cathode material of alumina-coated Download PDFInfo
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- CN107180961A CN107180961A CN201710443835.8A CN201710443835A CN107180961A CN 107180961 A CN107180961 A CN 107180961A CN 201710443835 A CN201710443835 A CN 201710443835A CN 107180961 A CN107180961 A CN 107180961A
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- H01M4/00—Electrodes
- H01M4/02—Electrodes composed of, or comprising, active material
- H01M4/36—Selection of substances as active materials, active masses, active liquids
- H01M4/362—Composites
- H01M4/366—Composites as layered products
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- H—ELECTRICITY
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- H01M—PROCESSES OR MEANS, e.g. BATTERIES, FOR THE DIRECT CONVERSION OF CHEMICAL ENERGY INTO ELECTRICAL ENERGY
- H01M10/00—Secondary cells; Manufacture thereof
- H01M10/05—Accumulators with non-aqueous electrolyte
- H01M10/052—Li-accumulators
- H01M10/0525—Rocking-chair batteries, i.e. batteries with lithium insertion or intercalation in both electrodes; Lithium-ion batteries
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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
- H01M4/36—Selection of substances as active materials, active masses, active liquids
- H01M4/48—Selection of substances as active materials, active masses, active liquids of inorganic oxides or hydroxides
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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
- H01M4/36—Selection of substances as active materials, active masses, active liquids
- H01M4/48—Selection of substances as active materials, active masses, active liquids of inorganic oxides or hydroxides
- H01M4/50—Selection of substances as active materials, active masses, active liquids of inorganic oxides or hydroxides of manganese
- H01M4/505—Selection of substances as active materials, active masses, active liquids of inorganic oxides or hydroxides of manganese of mixed oxides or hydroxides containing manganese for inserting or intercalating light metals, e.g. LiMn2O4 or LiMn2OxFy
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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
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- H01M4/02—Electrodes composed of, or comprising, active material
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- 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 method of modifying of the lithium-rich manganese-based layered cathode material of alumina-coated, using dry ice as precipitating reagent, silicon source is used as using meta-aluminate, reacted under conditions of heating is closed, the aluminium ion in water is deposited in the surface of lithium-rich manganese-based layered cathode material, the surface of the lithium-rich manganese-based layered cathode material of alumina-coated is caused finally by calcining.The present invention has the advantages that environmental protection, abundance and cheap using dry ice as precipitating reagent.By slowly changing the pH value of precipitation reaction, the alumina layer in spherical lithium-rich manganese-based anode material coated with uniform effectively increases the coulombic efficiency first of material, while showing superior charge and discharge cycles stability.
Description
Technical field
The invention belongs to field of lithium ion battery, it is related to lithium-rich manganese-based layered cathode material, and in particular to a kind of aluminum oxide
Coat the method for modifying of lithium-rich manganese-based layered cathode material.
Background technology
Although lithium-rich positive electrode (is more than 250mAh g with very high reversible specific capacity-1), but must charge
Electrochemical activation competence exertion is carried out to more than 4.5V to come out.The electrochemical activation process is irreversible, and along with one
The problem of serial serious, for example irreversible capacity is big first, cyclical stability declines, voltage decay and voltage in cyclic process
It is delayed serious etc..In using carbon as the lithium ion battery of negative pole, if the coulombic efficiency first of positive electrode is low, illustrate in electric discharge
Some lithium ion of process can not be embedded into positive electrode.These are trapped in the lithium ion of negative pole as charge and discharge cycles can
Li dendrite can be formed on the surface of negative pole, it is easy to pierce through barrier film, cause battery short circuit and trigger safety problem.Therefore, it is
Improve the security and service life of battery, it is necessary to improve the coulombic efficiency first of positive electrode.At present, positive electrode is improved
First an effective ways of coulombic efficiency be lithium-rich positive electrode with can embedding lithium lithium ion " host " compound use, this
A little lithium ion hosts include V2O5、VO2、LiV3O8、Li4Mn5O12Deng.These can lithium intercalation compound can receive those in discharge process
The lithium ion in lithium-rich material can not be embedded into again, so as to improve the coulombic efficiency of whole composite positive pole.But,
This method can not fundamentally improve the stability of the surface texture of lithium-rich material in charge and discharge process etc.
Problem.Therefore, the cyclical stability of the composite positive pole is decayed still than more serious.
Research finds that raising of the Surface coating to the chemical property of lithium-rich positive electrode is extremely effective.Table
Roll cover is avoided that directly contacting for active electrode material and electrolyte, alleviate electrolyte to the corrosion of electrode material surface with
And the dissolving of active transition metal.Conventional covering material has Al2O3、AlF3、CeO2、ZrO2、ZnO、AlPO4Etc. no electrochemistry
The inorganic compound of activity.In fact, surface coating modification can not only reduce the irreversible capacity loss of electrode material, and
Its cyclical stability and high rate performance can be significantly improved.At present, surface coating method mainly has solid phase method and wet chemistry method.Solid phase
Method is simple to operate, cost is low, is adapted to large-scale use, but its shortcoming is that cladding is uneven, and is difficult to accomplish bag completely
Cover.But uniform complete Surface coating is very important.Although wet chemistry method can accomplish highly uniform complete cladding,
But process is complicated, cost is high, unfavorable to large-scale use.
The content of the invention
In order to solve the deficiencies in the prior art, an object of the present invention is to provide a kind of lithium-rich manganese-based layer of alumina-coated
The method of modifying of shape positive electrode, possess environmental protection, it is cheap the advantages of, while the storehouse first of material can be effectively improved
Human relations efficiency, additionally it is possible to show superior charge and discharge cycles stability.
To achieve these goals, the technical scheme is that：
A kind of method of modifying of the lithium-rich manganese-based layered cathode material of alumina-coated, using dry ice as precipitating reagent, with meta-aluminic acid
Salt reacts under conditions of heating is closed as silicon source, the aluminium ion in water is deposited in lithium-rich manganese-based layered cathode material
Surface, the surface of the lithium-rich manganese-based layered cathode material of alumina-coated is caused finally by calcining.
The present invention uses dry ice as precipitating reagent, first, compared with conventional precipitating reagent ammoniacal liquor and sodium hydroxide etc., does
Ice has the advantages that environmental protection, abundance and cheap；Secondly, using dry ice as precipitating reagent, can slowly it change
Become the pH value of precipitation reaction, so that in the alumina layer in spherical lithium-rich manganese-based anode material coated with uniform, can be effective
The coulombic efficiency first of material is improved, while showing superior charge and discharge cycles stability.3rd, because dry ice is dissolved in water
After be presented faintly acid, it is and water-soluble poor, aluminium element can not only be provided using meta-aluminate, additionally it is possible to adjust solution for alkali
Property, so that solubility of the carbon dioxide in water after gasification is added, so as to accelerate reaction rate.
The second object of the present invention is to provide the lithium-rich manganese-based layered cathode material of modification prepared by a kind of above-mentioned method of modifying.
The third object of the present invention is to provide a kind of lithium-rich manganese-based layered cathode material of above-mentioned modification in lithium ion battery
Application.
Beneficial effects of the present invention are：
The present invention is using dry ice as precipitating reagent, and compared with conventional precipitating reagent ammoniacal liquor and sodium hydroxide etc., dry ice has
There are environmental protection, abundance and cheap.By slowly changing the pH value of precipitation reaction, in spherical rich lithium manganese
Base anode material coated with uniform alumina layer, effectively increases the coulombic efficiency first of material, while showing superior
Charge and discharge cycles stability.
Brief description of the drawings
The Figure of description for constituting the part of the application is used for providing further understanding of the present application, and the application's shows
Meaning property embodiment and its illustrate be used for explain the application, do not constitute the improper restriction to the application.
Fig. 1 is lithium-rich manganese-based stratified material Li prepared by embodiment 11.2Mn0.58Ni0.18Co0.04O2SEM enlarged photographs；
Fig. 2 is the lithium-rich manganese-based stratified material Li after the coated aluminum oxide of embodiment 11.2Mn0.58Ni0.18Co0.04O2SEM put
Big photo；
Fig. 3 is the lithium-rich manganese-based stratified material Li after the coated aluminum oxide of embodiment 11.2Mn0.58Ni0.18Co0.04O2Scanning
Electronic Speculum EDS energy spectrum diagrams；
Fig. 4 is the lithium-rich manganese-based stratified material Li of embodiment 11.2Mn0.58Ni0.18Co0.04O2Before and after coated aluminum oxide first
Charging and discharging curve；
Fig. 5 is lithium-rich manganese-based stratified material Li1.2Mn0.58Ni0.18Co0.04O2Charge-discharge cycle before and after coated aluminum oxide
Can curve.
Embodiment
It is noted that described further below is all exemplary, it is intended to provide further instruction to the application.Unless another
Indicate, all technologies used herein and scientific terminology are with usual with the application person of an ordinary skill in the technical field
The identical meanings of understanding.
It should be noted that term used herein above is merely to describe embodiment, and be not intended to restricted root
According to the illustrative embodiments of the application.As used herein, unless the context clearly indicates otherwise, otherwise singulative
It is also intended to include plural form, additionally, it should be understood that, when in this manual using term "comprising" and/or " bag
Include " when, it indicates existing characteristics, step, operation, device, component and/or combinations thereof.
Heretofore described lithium-rich manganese-based layered cathode material is a kind of positive electrode of lithium ion battery, its chemical formula
For xLi2MnO3·(1-x)LiMO2(0<x<1, M is one of Mn, Ni, Co or any combination).
As background technology is introduced, there is the deficiency that wet chemistry method modifying process is complicated, cost is high in the prior art,
In order to solve technical problem as above, present applicant proposes a kind of modification side of the lithium-rich manganese-based layered cathode material of alumina-coated
Method.
A kind of exemplary embodiment changing there is provided a kind of lithium-rich manganese-based layered cathode material of alumina-coated of the application
Property method, using dry ice as precipitating reagent, using meta-aluminate as silicon source, heat it is closed under conditions of react, make aluminium in water from
Son is deposited in the surface of lithium-rich manganese-based layered cathode material, causes the lithium-rich manganese-based layered cathode of alumina-coated finally by calcining
The surface of material.
The present invention uses dry ice as precipitating reagent, first, compared with conventional precipitating reagent ammoniacal liquor and sodium hydroxide etc., does
Ice has the advantages that environmental protection, abundance and cheap；Secondly, using dry ice as precipitating reagent, can slowly it change
Become the pH value of precipitation reaction, so that in the alumina layer in spherical lithium-rich manganese-based anode material coated with uniform, can be effective
The coulombic efficiency first of material is improved, while showing superior charge and discharge cycles stability.3rd, because dry ice is dissolved in water
After be presented faintly acid, it is and water-soluble poor, aluminium element can not only be provided using meta-aluminate, additionally it is possible to adjust solution for alkali
Property, so that solubility of the carbon dioxide in water after gasification is added, so as to accelerate reaction rate.
In order to prevent temperature too high, make dry ice gasification rate too fast, caused potential safety hazard, the application is preferred, heating
To 50~55 DEG C.
In order to ensure that aluminum oxide can be evenly coated at the surface of lithium-rich manganese-based layered cathode material, the application is preferred,
1~2h of stirring reaction.
Due in meta-aluminate containing other non-gasifiable metal cations, in order to reduce these metal cations to material
Expect the influence of battery performance, the application is preferred, and the product obtained after reaction is washed.Adhered in the material with removing
The foreign ions such as sodium, potassium.
Due to containing part Free water in reacted product, if the product with Free water is directly calcined, forge
Burn temperature higher, can make it that the vaporization rate of Free water in material is too fast, so that clad structure is destroyed, thus the application is further
It is preferred that, the product after washing is dried.Drying temperature is lower than calcining heat, typically not greater than 100 DEG C, can remove certainly
By water, and the boiling point due to temperature not less than water, Free water is removed based on volatilizing, and can prevent Free water vaporization rate mistake
Clad structure destruction caused by fast.The drying temperature is 75~85 DEG C.At this temperature, rate of drying is very fast.
In order to remove the combination water in reacted product, the application is preferred, and calcining heat is 300~350 DEG C.The temperature
Degree ensure that the combination water for removing product, while energy consumption can be reduced effectively.
Due to the carbon dioxide that dry ice is solid-state, its boiling point is relatively low, and reaction is airtight condition, in order to prevent dry ice from adding
Amount is excessive, makes the hypertonia in reaction system, so as to produce potential safety hazard, and the application is preferred, and the amount for adding dry ice causes
Pressure in confined reaction system is no more than 1MPa.
Because lithium-rich manganese-based layered cathode material is a kind of brand-new material, it is not commercialized, so the application provides one
The preparation method of lithium-rich manganese-based layered cathode material is planted, manganese salt, nickel salt, cobalt salt mixed solution is configured to, into mixed solution
Carbonate is added, and adjusts pH for 8.2~8.5, heating response is dried after reaction, then by dried product and carbonic acid
Lithium is well mixed, and is then carried out calcining and is obtained lithium-rich manganese-based layered cathode material, the calcination process be first be warming up to 500 ±
10 DEG C of calcining a period of times, it is further continued for being warming up to 900 ± 10 DEG C of calcining a period of times.
Present invention also provides the lithium-rich manganese-based layered cathode material of modification prepared by a kind of above-mentioned method of modifying.
Present invention also provides a kind of application of above-mentioned lithium-rich manganese-based layered cathode material of modification in lithium ion battery.
In order that the technical scheme of the application can clearly be understood by obtaining those skilled in the art, below with reference to tool
The embodiment of body describes the technical scheme of the application in detail with comparative example.
Embodiment
By manganese sulfate, nickel sulfate and cobaltous sulfate proportionally (29:9:2) mixed solution that total concentration is 2M is configured to,
In the homemade reactors of 2L, 200mL 0.1mol L are added-1Sodium carbonate liquor, add acetic acid regulation 8.3 or so, be heated to 60
℃.Under stirring, by nickel, cobalt, the sulfate of manganese and 2.1mol L-1Sodium carbonate precipitating reagent cocurrent be added in reactor react,
The mixing speed for controlling precipitation process is that 100-1000rpm, pH value are that 8.2~8.5, charging rate is 250mL h-1, overall reaction
Time is 12 hours.Reaction terminates, and is washed precipitated product to close to neutrality with hot water, then 110 DEG C of dryings 12 hours, are obtained
Nickel cobalt manganese precipitates presoma.Resulting persursor material is calcined 8 hours at 500 DEG C and is converted into complex oxide, then root
According to ratio (Li/M=(1+x)/(1-x), by lithium carbonate and complex oxide of lithium ion in target product and transition metal
(according to mol ratio 1.5:2) it is well mixed.First 500 DEG C of precalcinings 2 hours, are then calcined 1 hour at 900 DEG C in Muffle furnace,
Programming rate is 2 DEG C of min-1, target product material Li is obtained after cooling1.2Mn0.58Ni0.18Co0.04O2Electrode material, material shakes
Real density is in 2.4g/cm-3, the material of acquisition is as shown in figure 1, the Li prepared1.2Mn0.58Ni0.18Co0.04O2Electrode material is ball
Shape, and it is this it is spherical be second particle, be to be formed by the accumulation of nano particle.
0.2 gram of spherical lithium-rich manganese-based layered cathode material is distributed in 50 milliliters of 3mmol/L sodium metaaluminate aqueous solution, turned
Move on in 100 milliliters of reactors.Then 1 gram of dry ice is added, reactor is sealed, at 50 DEG C, stirring reaction 1 hour.Will be anti-
The product that should be obtained is washed with deionized totally, 80 DEG C of drying.Finally in Muffle furnace 300 DEG C sinter 4 hours, obtain surface
The lithium-rich manganese-based layered cathode material of coated aluminum oxide, is designated as 3wt%Al2O3- 500, its pattern are as shown in Fig. 2 according to Fig. 3 institutes
The spectral information shown further proves alumina-coated on the surface of the material.
Embodiment 2
The present embodiment is same as Example 1, and difference is, by 0.2 gram of spherical lithium-rich manganese-based layered cathode material point
It is scattered in 50 milliliters of 2mmol/L sodium metaaluminate aqueous solution, obtains the lithium-rich manganese-based layered cathode material note of surface-coated aluminum oxide
For 2wt%Al2O3-500。
Embodiment 3
The present embodiment is same as Example 1, and difference is, by 0.2 gram of spherical lithium-rich manganese-based layered cathode material point
It is scattered in 50 milliliters of 1mmol/L sodium metaaluminate aqueous solution, obtains the lithium-rich manganese-based layered cathode material note of surface-coated aluminum oxide
For 1wt%Al2O3-500。
Charge-discharge performance is carried out to embodiment 1~3 to be characterized as below：
To Li before and after coated aluminum oxide1.2Mn0.58Ni0.18Co0.04O2Electrode material carries out first charge-discharge experiment and characterized, its
As a result as shown in figure 4, wherein the voltage range of discharge and recharge is 4.5~2.0V, current density is 20mA g-1.Fig. 4 shows, coats
The specific discharge capacity of aluminum oxide rear electrode material has raising (~10mAh g by a small margin-1), but coulombic efficiency is substantially carried first
It is high：85% (3wt%Al is brought up to from original 67%2O3)。
To Li before and after coated aluminum oxide1.2Mn0.58Ni0.18Co0.04O2Electrode material carries out charge-discharge performance test, its
As a result as shown in figure 5, electrode material is circulated between 4.8~2.0V, current density is 20mA g-1。
Comparative example
The preparation method of this comparative example is identical with the preparation method of embodiment 1, and difference is, by the spherical rich lithiums of 0.2g
Manganese base layered cathode material is distributed in 50 milliliters of 3mmol/L aluminum chloride aqueous solutions, is transferred in reactor.Then 10 millis are added
0.045mol/L ammoniacal liquor is risen, reactor is sealed, at 50 DEG C, stirring reaction 1 hour.Obtained product deionization will be reacted
Water washing is clean, 80 DEG C of drying.Finally in Muffle furnace 300 DEG C sinter 4 hours, obtain the lithium-rich manganese-based of surface-coated aluminum oxide
Layered cathode material.
Carry out first charge-discharge experiment to the material to characterize, its result shows that this method is only capable of carrying coulombic efficiency first
Up to 75%.
The preferred embodiment of the application is the foregoing is only, the application is not limited to, for the skill of this area
For art personnel, the application can have various modifications and variations.It is all within spirit herein and principle, made any repair
Change, equivalent substitution, improvement etc., should be included within the protection domain of the application.
Claims (10)
1. a kind of method of modifying of the lithium-rich manganese-based layered cathode material of alumina-coated, it is characterized in that, using dry ice as precipitating reagent, with
Meta-aluminate reacts under conditions of heating is closed as silicon source, the aluminium ion in water is deposited in lithium-rich manganese-based layered cathode
The surface of material, the surface of the lithium-rich manganese-based layered cathode material of alumina-coated is caused finally by calcining.
2. method of modifying as claimed in claim 1, it is characterized in that, it is heated to 50~55 DEG C.
3. method of modifying as claimed in claim 1, it is characterized in that, 1~2h of stirring reaction.
4. method of modifying as claimed in claim 1, it is characterized in that, the product obtained after reaction is washed.
5. method of modifying as claimed in claim 4, it is characterized in that, the product after washing is dried；It is preferred that, it is described to dry
Dry temperature is 75~85 DEG C.
6. method of modifying as claimed in claim 1, it is characterized in that, calcining heat is 300~350 DEG C.
7. method of modifying as claimed in claim 1, it is characterized in that, the amount of addition dry ice causes the pressure in confined reaction system
No more than 1MPa.
8. method of modifying as claimed in claim 1, it is characterized in that, the preparation method of the lithium-rich manganese-based layered cathode material,
Manganese salt, nickel salt, cobalt salt are configured to mixed solution, carbonate is added into mixed solution, and it is 8.2~8.5 to adjust pH, heating
Reaction, is dried after reaction, then dried product is well mixed with lithium carbonate, is then carried out calcining and is obtained lithium-rich manganese-based
Layered cathode material, the calcination process is first to be warming up to 500 ± 10 DEG C of calcining a period of times, is further continued for being warming up to 900 ± 10
DEG C calcining a period of time.
9. the lithium-rich manganese-based layered cathode material of modification prepared by a kind of any described method of modifying of claim 1~8.
10. application of the lithium-rich manganese-based layered cathode material of modification in lithium ion battery described in a kind of claim 9.
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