CN109560284A - A kind of high performance doping type lithium manganate positive electrode and preparation method thereof - Google Patents
A kind of high performance doping type lithium manganate positive electrode and preparation method thereof Download PDFInfo
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- CN109560284A CN109560284A CN201811310549.5A CN201811310549A CN109560284A CN 109560284 A CN109560284 A CN 109560284A CN 201811310549 A CN201811310549 A CN 201811310549A CN 109560284 A CN109560284 A CN 109560284A
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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
- 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
- H01M4/62—Selection of inactive substances as ingredients for active masses, e.g. binders, fillers
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- H01M4/02—Electrodes composed of, or comprising, active material
- H01M4/62—Selection of inactive substances as ingredients for active masses, e.g. binders, fillers
- H01M4/628—Inhibitors, e.g. gassing inhibitors, corrosion inhibitors
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- H—ELECTRICITY
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- H01M2004/021—Physical characteristics, e.g. porosity, surface area
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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
- H01M2004/026—Electrodes composed of, or comprising, active material characterised by the polarity
- H01M2004/028—Positive electrodes
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Abstract
The present invention proposes a kind of high performance doping type lithium manganate positive electrode, at least one following element of doping in LiMn2O4: the molar ratio difference of Nb, F, B, Nb, F, the B adulterated and LiMn2O4 is as follows: 0.002-0.005,0.05-0.15,0.001-0.005.When production, including following operating procedure: MnO is weighed in proportion2、Li2CO3And the element source compound adulterated；Ball milling mixing 0.5-3h；700-900 DEG C of roasting 10-30h；It is passed through slow cooling after excessive air；Screening, sampling Detection, packaging.Doping type lithium manganate positive electrode tap density proposed by the present invention is the same as the raising at least 0.3-0.5g/cm undoped with compared with3, self discharge problem significantly improves after being assembled into lithium battery, and 1C, 55 DEG C of capacity retention ratios after high temperature circulation 300 times are still 85% or more.
Description
Technical field
The present invention relates to battery material technical field, in particular to a kind of high performance doping type lithium manganate positive electrode and
Preparation method.
Background technique
LiMn2O4 is one of very promising lithium ion anode material, compared with traditional positive electrode such as cobalt acid lithium, tool
Have the advantages that resourceful, at low cost, pollution-free, safety is good, good rate capability, be ideal power battery anode material,
But its poor cycle performance and electrochemical stability but greatly limit its industrialization.LiMn2O4 mainly includes spinel-type
LiMn2O4 and layer structure LiMn2O4, wherein lithium manganate having spinel structure stable structure, it is easy to accomplish industrialized production, nowadays market
Product is such structure.Lithium manganate having spinel structure belongs to cubic system, Fd3m space group, theoretical specific capacity 148mAh/g,
Due to three-dimensional tunnel structure, lithium ion can the reversibly deintercalation from spinel crystal lattice, collapsing for structure will not be caused, because
And there is excellent high rate performance and stability.Existing manganate lithium ion battery positive electrode is usually with MnO2/
Li2CO370-90%+LiOH 10-30% or MnO2/Li2CO3For raw material, by lithium, manganese molar ratio (0.8-1.2): 2 formulas exist
The disadvantages of self discharge is high, compacting is poor, high-temperature behavior is poor.How the formula is adjusted, to solve disadvantages mentioned above without influencing other property
Can, it is the current technical issues that need to address.
Summary of the invention
To solve the above the deficiencies in the prior art, the invention proposes a kind of high performance doping type lithium manganate positive electrodes
And preparation method thereof.
The technical scheme of the present invention is realized as follows:
A kind of high performance doping type lithium manganate positive electrode, at least one following element of doping in LiMn2O4: Nb, F, B,
The molar ratio difference of Nb, F, B and LiMn2O4 for being adulterated are as follows: 0.002-0.005,0.05-0.15,0.001-0.005.
The fusing point of Nb is up to 2468 DEG C, and for boiling point up to 4742 DEG C, other refractory metals of density ratio are low, is 8.57g/cm3.Nb
Architectural characteristic it is more stable, and under low-temperature condition present superconductor property, at normal atmospheric pressure, the critical-temperature of Nb is
9.2K is highest in all simple substance superconductors.Its magnetic penetration depth is also highest in all elements.Mangaic acid lithium doping Nb member
After element, material structure is remained unchanged, and unit cell volume increases, and can effectively expande the transmission channel of lithium ion, can rock-steady structure, raising
Ionic diffusion energy, improve compactibility, solve lithium manganate material structural instability, thermal stability in cyclic process it is poor, press
Real poor defect, makes it have higher specific capacity and good compactibility, cyclical stability and high rate performance.In addition, Nb is also
Various erosions can be resisted, dielectric oxide layer is formed, manganate cathode material for lithium is preferably protected and guarantees its normal operation.Together
When, Nb is relatively conventional, and price is lower.Modification is doped using niobium, is conducive to save production cost.B ion ratio Mn ion
Ionic radius it is much smaller, the intensity of B-O key ratio Mn-O key is much larger, and the practical oxidation state of Mn in LiMn2O4 can be promoted by mixing B,
The oxidation state for delaying Mn is lower than+3.5 process, mitigates the Jahn-Teller distortion of Mn ion, slows down structural stability decline,
Improve the stability and self discharge of sample structure in charge and discharge process.The doping of B can also increase lithium manganate particle, change
Kind agglutinating property.After adulterating F, the crystal property of material is good, chemical stability is high, can be effective in charge and discharge process repeatedly
The structural stability for keeping adulterated lithium manganate material, promotes its multiplying power and high temperature cyclic performance.
Preferably, at least one following element: Al, Mg, Li, O is also adulterated.Al, Mg can further stable doping mangaic acids
The structural stability of lithium, Li can further improve the cyclicity of adulterated lithium manganate, and oxygenating can reduce the production of the co-melting body of anoxic
It is raw, improve the cycle life of adulterated lithium manganate.
It is further preferred that doping type lithium manganate positive electrode is Li1+xMn2-x-yAlxMgyFxO4-x, wherein 0.1≤x≤
0.12,0.01≤y≤0.1.
It is further preferred that doping type lithium manganate positive electrode is Li1+xMn2-2xNbxBxO4, wherein 0.001≤x≤
0.01。
The present invention also proposes a kind of preparation method of high performance doping type lithium manganate positive electrode, including operates step as follows
It is rapid:
(1) MnO is weighed in proportion2、Li2CO3And the element source compound adulterated；
(2) ball milling mixing 0.5-3h；
(3) 700-900 DEG C of roasting 10-30h；
(4) slow cooling；
(5) screening, sampling Detection, packaging.
Mg source compound includes but is not limited to Mg (OH)2, MgO and MgF2One of or it is a variety of, Nb source compound include but
It is not limited to Nb2O5、(CH3COO)5Nb and Nb2(C2O4)5One of or it is a variety of, Al source compound includes but is not limited to Al (OH)3、
Al2O3、KAlF4One of or it is a variety of, B source compound includes but is not limited to H3BO3。
Preferably, in step (4), slow cooling for 24 hours after, temperature is down to 500 DEG C, needs to be continually fed into excess during this period
Air；It is naturally cooling to room temperature from 500 DEG C again later, air can be passed through in this temperature descending section, it can not also blowing air.
Doping type lithium manganate positive electrode tap density proposed by the present invention improves, at least in 1.7g/cm3More than；Assembling
It is significantly improved at self discharge after lithium battery, 1C, 55 DEG C of capacity retention ratios after high temperature circulation 300 times are still 85% or more.Moreover,
The preparation method step of doping type lithium manganate positive electrode proposed by the present invention is few, it is easy to operate, be easily industrialized.
Detailed description of the invention
In order to more clearly explain the embodiment of the invention or the technical proposal in the existing technology, to embodiment or will show below
There is attached drawing needed in technical description to be briefly described, it should be apparent that, the accompanying drawings in the following description is only this
Some embodiments of invention without any creative labor, may be used also for those of ordinary skill in the art
To obtain other drawings based on these drawings.
Fig. 1 is that the SEM of 1 products obtained therefrom of embodiment schemes；
Fig. 2 is the XRD diagram of 1 products obtained therefrom of embodiment；
The SEM figure that a is the SEM figure of the LiMn2O4 to undope in Fig. 3, b is 4 products obtained therefrom of embodiment.
Specific embodiment
Technical solution of the present invention is clearly and completely described below in conjunction with the embodiment of the present invention.Obviously, described
Embodiment is only a part of the embodiment of the present invention, instead of all the embodiments.Based on the embodiments of the present invention, this field
Those of ordinary skill's every other embodiment obtained without creative efforts, belongs to protection of the present invention
Range.
Embodiment 1
A kind of high performance doping type lithium manganate positive electrode, chemical formula Li1.1Mn1.8Al0.1Mg0.1F0.1O3.9。
The preparation method of the positive electrode includes following operating procedure:
(1) MnO is weighed in proportion2、Li2CO3And the source compound of doped chemical, the source Li are LiF, the source Al is Al (OH)3,
The source Mg is Mg (OH)2, the source F is LiF；
(2) ball milling mixing 0.5h；
(3) 900 DEG C of roasting 10h；
(4) slow cooling under natural conditions；
(5) screening, sampling Detection, packaging.
Embodiment 2
A kind of high performance doping type lithium manganate positive electrode, chemical formula Li1.12Mn1.87Al0.12Mg0.01F0.12O3. 88.Preparation method is similar to Example 1, ball milling mixing 3h, 700 DEG C of roasting 10h, remaining operating condition is same as Example 1.
Embodiment 3
A kind of high performance doping type lithium manganate positive electrode, chemical formula Li1.11Mn1.84Al0.11Mg0.05F0.11O3. 84.Preparation method is similar to Example 1, ball milling mixing 2h, 800 DEG C of roasting 2h, remaining operating condition is same as Example 1.
Embodiment 4
A kind of high performance doping type lithium manganate positive electrode, chemical formula Li1.001Mn1.998Nb0.001B0.001O4。
(1) MnO is weighed in proportion2、Li2CO3And the source compound of doped chemical, the source Nb are Nb2(C2O4)5, the source B is
H3BO3；
(2) ball milling mixing 0.5h；
(3) 900 DEG C of roasting 10h；
(4) be continually fed into excessive air, slow cooling for 24 hours after, temperature is down to 500 DEG C, drops naturally from 500 DEG C again later
It warms to room temperature；
(5) screening, sampling Detection, packaging.
Embodiment 5
A kind of high performance doping type lithium manganate positive electrode, chemical formula Li1.005Mn1.99Nb0.005B0.005O4.It is made
Preparation Method is similar to Example 4, ball milling mixing 3h, 700 DEG C of roasting 30h, remaining operating condition is same as Example 4.
Embodiment 6
A kind of high performance doping type lithium manganate positive electrode, chemical formula Li1.01Mn1.98Nb0.01B0.01O4.It is prepared
Method is similar to Example 4, ball milling mixing 2h, 800 DEG C of roasting 2h, remaining operating condition is same as Example 4.
Embodiment 7
A kind of high performance doping type lithium manganate positive electrode, chemical formula Li1.1Mn1.8Al0.1Mg0.1F0.1O4。
The preparation method of the positive electrode includes following operating procedure:
(1) MnO is weighed in proportion2、Li2CO3And the source compound of doped chemical, the source Li are LiF, the source Al is Al (OH)3,
The source Mg is Mg (OH)2, the source F is LiF；
(2) ball milling mixing 0.5h；
(3) 900 DEG C of roasting 10h；
(4) be continually fed into excessive air, slow cooling for 24 hours after, temperature is down to 500 DEG C, drops naturally from 500 DEG C again later
It warms to room temperature；
(5) screening, sampling Detection, packaging.
Embodiment 8
A kind of high performance doping type lithium manganate positive electrode, chemical formula Li1.12Mn1.87Al0.12Mg0.01F0.12O4。
Preparation method is similar to Example 7, ball milling mixing 3h, 700 DEG C of roasting 3h, remaining operating condition is same as Example 7.
Embodiment 9
A kind of high performance doping type lithium manganate positive electrode, chemical formula Li1.11Mn1.84Al0.11Mg0.05F0.11O4。
Preparation method is similar to Example 7, ball milling mixing 2h, 800 DEG C of roasting 2h, remaining operating condition is same as Example 7.
The resulting material of embodiment 1 is subjected to SEM (as shown in Figure 1) and XRD test (as shown in Figure 2), is mixed as shown in Figure 2
There is no miscellaneous peak appearance in lithium manganate material XRD spectrum after miscellaneous, material still keeps spinel structure after doping, but spinelle knot
Structure is rounded cunning, to increase mobility, improve compacted density.The smooth rigid surface that the structure has, which can effectively reduce, to be filled
Dissolution of the discharge process micro-moisture to bivalent manganese, improves high-temperature behavior and cycle performance.
Lithium battery is assembled into the LiMn2O4 of obtained doping Al, Li, Mg, the F of embodiment 1-3 and carries out chemical property survey
Examination, including 1C capacity retention ratio after discharge capacity and 55 DEG C, 300 circulations for the first time.Test result is shown: doping Al, Li, Mg, F
LiMn2O4 1C discharge for the first time gram volume from embodiment 1-3 be respectively 134.2mAh/g, 133.4mAh/g, 135.6mAh/g, 1C,
55 DEG C, capacity retention ratio is respectively 87%, 86%, 88% after 300 circulations, and under the same test condition of LiMn2O4 to undope
Conservation rate is only 40% or so.
By the progress SEM test of the resulting material of embodiment 4, the LiMn2O4 of Nb, B as shown in figure 3, a undopes, b doping Nb,
The LiMn2O4 of B.It is obvious that the pattern of LiMn2O4 is substantially change after doping Nb, B, changed by the irregular block before adulterating
For the chondritic of comparison rule, particle diameter distribution also tends to uniform.The test result of tap density meter is shown: embodiment 4-6's
Tap density is in 1.9g/cm3More than, than undoped raising 0.3-0.5g/cm2.By the obtained material of embodiment 4-6 and
Undoped LiMn2O4 is assembled into lithium battery respectively as positive electrode.Constant-current charge is carried out to above-mentioned lithium battery with 0.2C, is filled
Constant-voltage charge is carried out to battery after to 4.2V, current limliting 0.2C is until electric current is reduced to 0.02C.Battery is put respectively at 60 DEG C
It sets one, two, three day and tests its capacitance loss.Test result is as follows for self discharge shown in table:
| Battery | It is shelved at 60 DEG C one day | It is shelved at 60 DEG C two days | It is shelved at 60 DEG C three days |
| Embodiment 4 | 11.2 | 11.0 | 11.3 |
| Embodiment 5 | 10.8 | 10.5 | 10.7 |
| Embodiment 6 | 10.4 | 10.2 | 10.3 |
| Any doping is not carried out | 14.9 | 14.1 | 14.0 |
As seen from the above table: the lithium manganate cell volume loss of doping Nb, B substantially reduce, and self discharge significantly improves, table
It is bright its stability is good in the electrolytic solution, the side reaction at positive electrode and electrolyte interface can be inhibited to occur.
The LiMn2O4 of doping Al, Li, Mg, F, O that embodiment 7-9 is obtained are assembled into lithium battery and carry out chemical property survey
Examination, 1C, 55 DEG C, 300 times circulation after capacity retention ratio be respectively 95%, 96%, 94%.Compared respectively with embodiment 1-3 it is found that
The generation for reducing the co-melting body of anoxic by oxygenating, improves cycle life.
The assembling mode of battery involved in above-mentioned test is as follows: binder PVDF (gathering inclined fluorine vinyl chloride) is dissolved in
In solvent NMP (N-Methyl pyrrolidone), the product that later obtains above-described embodiment (or the mangaic acid of any doping is not carried out
Lithium) with conductive agent CNT (carbon nanotube), binder PVDF 96.5:1:2.5 in mass ratio be mixed to form uniform anode sizing agent,
The quality of the solvent NMP of binder PVDF is product (or the LiMn2O4 for not carrying out any doping) quality that above-described embodiment obtains
80%.Anode sizing agent is coated on plus plate current-collecting body aluminium foil and forms anode.Carbon material used as anode and conductive agent SP, binder
CMC (sodium carboxymethylcellulose), SBR (butadiene-styrene rubber), water are made after mixing according to mass ratio 92:1:1.5:5.5:130
Negative electrode slurry.Negative electrode slurry is coated on the copper foil of 10 μ m-thick of negative current collector and forms cathode.By anode, cathode and diaphragm
It is assembled into battery core, is packed into shell, is then injected into lithium battery electrolytes, seals, is assembled into battery.
The foregoing is merely illustrative of the preferred embodiments of the present invention, is not intended to limit the invention, all in essence of the invention
Within mind and principle, any modification, equivalent replacement, improvement and so on be should all be included in the protection scope of the present invention.
Claims (6)
1. a kind of high performance doping type lithium manganate positive electrode, it is characterised in that: adulterate at least one following member in LiMn2O4
Element: the molar ratio difference of Nb, F, B, Nb, F, the B adulterated and LiMn2O4 is as follows: 0.002-0.005,0.05-0.15,0.001-
0.005。
2. high performance doping type lithium manganate positive electrode according to claim 1, it is characterised in that: also adulterate at least one
The following element of kind: Al, Mg, Li, O.
3. high performance doping type lithium manganate positive electrode according to claim 2, it is characterised in that: the doping type manganese
Sour lithium anode material is Li1+xMn2-x-yAlxMgyFxO4-x, wherein 0.1≤x≤0.12,0.01≤y≤0.1.
4. high performance doping type lithium manganate positive electrode according to claim 2, it is characterised in that: the doping type manganese
Sour lithium anode material is Li1+xMn2-2xNbxBxO4, wherein 0.001≤x≤0.01.
5. a kind of preparation method of high performance doping type lithium manganate positive electrode according to any one of claims 1-4,
It is characterized in that: including following operating procedure:
(1) MnO is weighed in proportion2、Li2CO3And the element source compound adulterated；
(2) ball milling mixing 0.5-3h；
(3) 700-900 DEG C of roasting 10-30h；
(4) slow cooling；
(5) screening, sampling Detection, packaging.
6. the preparation method of high performance doping type lithium manganate positive electrode according to claim 5, it is characterised in that: step
Suddenly in (4), slow cooling for 24 hours after, temperature is down to 500 DEG C, needs to be continually fed into excessive air during this period；Later again from
500 DEG C are naturally cooling to room temperature.
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| CN110921720A (en) * | 2019-12-03 | 2020-03-27 | 江南大学 | High-voltage lithium ion battery positive electrode material and preparation method thereof |
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| CN110921720A (en) * | 2019-12-03 | 2020-03-27 | 江南大学 | High-voltage lithium ion battery positive electrode material and preparation method thereof |
| CN110921720B (en) * | 2019-12-03 | 2022-02-15 | 江南大学 | High-voltage lithium ion battery positive electrode material and preparation method thereof |
| CN113178558A (en) * | 2021-04-27 | 2021-07-27 | 安徽锂桥新材料有限公司 | Composite manganese-based positive electrode material and preparation method thereof |
| WO2023197240A1 (en) * | 2022-04-14 | 2023-10-19 | 宁德时代新能源科技股份有限公司 | Positive electrode active material, secondary battery, battery module, battery pack, and electric device |
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