CN103178260A - Lithium manganate anode material, and preparation method and application thereof - Google Patents
Lithium manganate anode material, and preparation method and application thereof Download PDFInfo
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Abstract
The invention discloses lithium manganate anode material, and a preparation method and the application of the lithium manganate anode material. The chemical formula of the lithium manganate anode material is Li1+xMn2-x-yMyO4; the lithium manganate anode material is powdery; M in the chemical formula is selected from one or more elements in Ni, Co, Mg, Al, Cr and Ti; x is larger than or equal to 0.03 and smaller than or equal to 0.15; and y is larger than or equal to 0 and smaller than or equal to 0.20. The invention also comprises the preparation method and the application of the lithium manganate anode material. The lithium manganate anode material can enhance the energy density of batteries, and can simultaneously improve the multiplying power and the high-temperature cycle performance of the batteries.
Description
Technical field
The present invention relates to a kind of lithium ion battery manganate cathode material for lithium and preparation method thereof and application.
Background technology
Lithium ion battery is the most competitive battery of a new generation, is called as " the environmental protection energy ", is the one preferred technique that solves Contemporary Environmental pollution problem and energy problem.In recent years, lithium ion battery has been obtained immense success in the high-energy battery field, emerge but the consumer still expects the better battery of combination property, and this depends on the research and development to new electrode material and electrolyte system.Anode material for lithium-ion batteries as the lithium ion battery important component part, is the essential critical material of lithium ion battery, and its performance quality has material impact to the performance of lithium ion battery.
In order to seek the material of high-energy-density, be mainly to realize by the compacted density and the capacity that improve material.As everyone knows, compacted density generally is subjected to the impact of real density and material appearance structure.According to the descending arrangement of real density, the order of four kinds of materials is as follows: cobalt acid lithium〉ternary〉LiMn2O4〉LiFePO4, this is also in full accord with the trend of present compacted density, and as seen, real density is maximum effect factor of a kind of material compaction of impact.But for same material, the smooth surface degree of material, particle diameter distributes, the size of second particle internal voids, the alignment degree of material, these are all the factors that affects material compacted density.It is the factor of more complicated that particle diameter distributes, and reasonably particle diameter distributes and can suitably improve compacted density.
Positive electrode can damage battery performance when improving compacted density, for example improve compacted density, can reduce capacity, multiplying power and high temperature cyclic performance.
CN101841018A discloses a kind of single crystal lithium manganese oxide for lithium ion battery and preparation method thereof on September 22nd, 2010, the multiplying power of this battery and high temperature cyclic performance are excellent, but monocrystalline lithium manganese oxide calcining heat used is high, and energy consumption is large, and compacted density remains further to be improved simultaneously.
Summary of the invention
Technical problem to be solved by this invention is, provides a kind of and can promote energy content of battery density, can improve manganate cathode material for lithium and preparation method thereof and the application of battery multiplying power and high temperature cyclic performance simultaneously.
The technical scheme that the present invention solves its technical problem employing is:
The present invention's manganate cathode material for lithium, chemical formula are Li
1+xMn
2-x-yM
yO
4, for Powdered;
In described chemical formula, M is one or more the element that is selected from Ni, Co, Mg, Al, Cr, Ti, 0.03≤x≤0.15,0≤y≤0.20.
The preparation method of the present invention's manganate cathode material for lithium comprises the following steps: with average grain diameter D
50Be the granule manganese compound of 0.1～10 μ m, average grain diameter D
50Be bulky grain manganese compound, the average grain diameter D of 12～30 μ m
50Be the lithium compound of 2～12 μ m and the doped compound that contains the M element, press chemical formula Li
1+xMn
2-x-yM
yO
4Metering is than weigh batching, and the ball grinder batch mixing of packing into, batch mixing ball are alumina balls, ball material mass ratio (0.5～1): 1, mix 1～5h; The material pine burning alms bowl of packing into after mixing, the Muffle furnace sintering first is warming up to 600 ± 5 ℃, and constant temperature 1～10h(preferred 2～6h), be warming up to again 750～1000 ℃ (preferred 800～900 ℃), constant temperature 1～10h(is preferred 2～6h), after be cooled to 600 ± 5 ℃, constant temperature 1～20h(preferred 5～16h), be cooled to again room temperature, then pulverize, mistake 〉=325 mesh sieves.
Further, in the manganese compound of described two kinds of different-grain diameters, granule manganese compound quality: bulky grain manganese compound quality=(0.1～1): 1.
If granule manganese compound quality: bulky grain manganese compound quality is less than 0.1, and short grained quantity not sufficient to be filling the space between bulky grain, thereby to the lifting DeGrain of compacted density.If granule manganese compound quality: bulky grain manganese compound quality is greater than 1, too much short grained existence, and in material, whole particle diameter distributes on the low sidely, and compacting also can reduce.Therefore preferred granule manganese compound quality: bulky grain manganese compound quality=(0.1～1): 1.
Further, the doped compound of the described M of containing element is Al (OH)
3, CrO
3, NiO, TiO
2, MgO or Co
3O
4In one or more mixture, the addition of every kind of material is 0.05～5wt% of total material.
Described granule manganese compound, bulky grain manganese compound can be MnO2 or Mn3O4 etc.; Described lithium compound can be Li
2CO
3
Described LiMn2O4 powder is primary particle more than 0.25 μ m by particle diameter, or primary particle assembles, or the second particle that sintering forms forms.(primary particle is particle minimum in SEM figure, and the bulky grain that primary particle is gathered into is called second particle, or the sintering particle of growing up and fusing together)
The application of the present invention's manganate cathode material for lithium in non-aqueous electrolyte lithium secondary battery: as positive electrode active materials or wherein a part of.
Described non-aqueous electrolyte lithium secondary battery is made of manganate cathode material for lithium, nonaqueous electrolytic solution and negative pole.Wherein, nonaqueous electrolytic solution can be the conventional electrolysis liquid (solvent of electrolyte, except the combination of using ethylene carbonate and diethyl carbonate, can also use one or more the organic solvent in the ethers such as carbonates such as comprising propene carbonate, dimethyl carbonate and dimethoxy-ethane, electrolyte can be one or more the mixture in the lithium salts such as lithium hexafluoro phosphate, LiBF4, lithium perchlorate, be dissolved in described organic solvent and use), or contain the additive PS or/and vinylene carbonate.The active material of negative pole can be lithium metal, graphite, contain the alloy material of Si or Sn, perhaps lithium titanate etc.
That described non-aqueous electrolyte lithium secondary battery can be made is square, coin shape or column type etc.
The present invention's manganate cathode material for lithium, compacted density can suitably improve, and can promote energy content of battery density thus, can improve battery multiplying power and high temperature cyclic performance simultaneously.
Description of drawings
Fig. 1 is the XRD collection of illustrative plates of embodiment 1,2,3, the 4 LiMn2O4 powder that synthesize;
Fig. 2 is the particle diameter distribution map of the synthetic LiMn2O4 powder of embodiment 1 and Comparative Examples 1;
Fig. 3 is the SEM figure of the synthetic LiMn2O4 powder of embodiment 1;
Fig. 4 is the SEM figure of the synthetic LiMn2O4 powder of embodiment 4;
Fig. 5 is the SEM figure of the synthetic LiMn2O4 powder of embodiment 8;
Fig. 6 is the SEM figure of the synthetic LiMn2O4 powder of Comparative Examples 1;
Fig. 7 is the 1st time (1 of embodiment 4
st) and the 2nd time (2
nd) charging and discharging curve figure.
Embodiment
The invention will be further described below in conjunction with drawings and Examples.
The manganate cathode material for lithium of the present embodiment, chemical formula are Li
1+xMn
2-xO
4, for Powdered.(Li
1+xMn
2-x-yM
yO
4, the M element that do not adulterate, y=0,0.03≤x≤0.15)
The preparation method comprises the following steps: with 77.93g average grain diameter D
50Be the granule MnO of 3 μ m
2, 701.37g average grain diameter D
50Be the bulky grain MnO of 17 μ m
2(granule MnO
2Quality: bulky grain MnO
2Quality=1:9), with 184.70g average grain diameter D
50Be the Li of 5 μ m
2CO
3The 5L ball grinder batch mixing of packing into, the batch mixing ball is alumina balls, ball material mass ratio 1:1 mixes 3h; The material pine burning alms bowl of packing into after mixing, the Muffle furnace sintering first is warming up to 600 ℃, constant temperature 2h, then be warming up to 900 ℃, constant temperature 4 h, after be cooled to 600 ℃, then constant temperature 8 h, then be cooled to room temperature pulverize, and cross 325 mesh sieves.
Use button cell to estimate initial stage charge-discharge characteristic and the high temperature cyclic performance of the manganate cathode material for lithium of the present embodiment.
The making of button cell: at first mix 92.0wt% as the LiMn2O4 powder of positive active material, 2.5wt% is as the acetylene black of electric conducting material and the graphite KS-15 of 2.5wt%, 3wt% is as the Kynoar in 1-Methyl-2-Pyrrolidone of being dissolved in of adhesive, be coated on afterwards on the Al metal forming, with 120
oC is dry, after this stamped from sheetstock is diameter 16mm, with 1.5t/cm
3Crimping, using thickness of electrode is that the electrode of 50 μ m is as positive pole; Negative pole uses the lithium metal that is stamped into diameter 16mm, and electrolyte uses the LiPF that is dissolved with 1mol/L
6With volume ratio 3:7 mixing EC(ethylene carbonate) and the DEC(diethyl carbonate) solution, make CR2032 type button cell.
Carry out volume test first, high rate performance and high temperature cyclic performance test.
The initial stage charge-discharge characteristic at room temperature is charged to 4.3V, carries out with the current density of 0.1C, after carrying out 90 minutes constant-potential charges, is discharged to 3.0V with the current density of 0.1C, measures initial stage charging capacity, initial stage discharge capacity and the initial stage efficient of this moment.
In addition, as hot properties, implement the high temperature circulation test.In test, utilize 60
oC insulating box, voltage range are 3.0～4.3V, carry out the 1st circulation, the 2nd circulation and the 3rd cycle charge-discharge with the multiplying power of 0.5C, carry out cycle charge-discharge the 4th～54 time with the multiplying power of 1C.High temperature circulation capacity dimension holdup is that the 1C discharge capacity of the 54th circulation is with respect to the ratio of the 2nd 0.5C discharge capacity.
The manganate cathode material for lithium of the present embodiment, chemical formula are Li
1+xMn
2-xO
4, for Powdered.(Li
1+xMn
2-x-yM
yO
4, the M element that do not adulterate, y=0,0.03≤x≤0.15)
The difference of preparation method and embodiment 1 is: the MnO of two kinds of different-grain diameters
2In, granule MnO
2Quality: bulky grain MnO
2Quality=3:7.
Initial stage charge-discharge characteristic and high temperature cyclic performance to the manganate cathode material for lithium of the present embodiment are tested, and method of testing is with embodiment 1, and test result sees Table 1.
The manganate cathode material for lithium of the present embodiment, chemical formula are Li
1+xMn
2-xO
4, for Powdered.(Li
1+xMn
2-x-yM
yO
4, the M element that do not adulterate, y=0,0.03≤x≤0.15)
The difference of preparation method and embodiment 1 is: in the manganese compound of two kinds of different-grain diameters, and granule MnO
2Quality: bulky grain MnO
2Quality=4:6.
Initial stage charge-discharge characteristic and high temperature cyclic performance to the manganate cathode material for lithium of the present embodiment are tested, and method of testing is with embodiment 1, and test result sees Table 1.
Embodiment 4
The manganate cathode material for lithium of the present embodiment, chemical formula are Li
1+xMn
2-x-yM
yO
4, for Powdered.(in formula, M is Al, 0.03≤x≤0.15,0≤y≤0.20)
The difference of preparation method and embodiment 2 is: the Al (OH) that is added with 1.2wt% in mixed material
3
Initial stage charge-discharge characteristic and high temperature cyclic performance to the manganate cathode material for lithium of the present embodiment are tested, and method of testing is with embodiment 1, and test result sees Table 1.
Embodiment 5
The manganate cathode material for lithium of the present embodiment, chemical formula are Li
1+xMn
2-x-yM
yO
4, for Powdered.
(in formula, M is Mg, 0.03≤x≤0.15,0≤y≤0.20)
The difference of preparation method and embodiment 4 is: the MgO that is added with 1.8wt% in the batch mixing process.
Initial stage charge-discharge characteristic and high temperature cyclic performance to the manganate cathode material for lithium of the present embodiment are tested, and method of testing is with embodiment 1, and test result sees Table 1.
The manganate cathode material for lithium of the present embodiment, chemical formula are Li
1+xMn
2-x-yM
yO
4, for Powdered.
(in formula, M is Co, 0.03≤x≤0.15,0≤y≤0.20)
The difference of preparation method and embodiment 4 is: the Co that is added with 1.8wt% in the batch mixing process
3O
4
Initial stage charge-discharge characteristic and high temperature cyclic performance to the manganate cathode material for lithium of the present embodiment are tested, and method of testing is with embodiment 1, and test result sees Table 1.
The manganate cathode material for lithium of the present embodiment, chemical formula are Li
1+xMn
2-x-yM
yO
4, for Powdered.
(in formula, M is Al, 0.03≤x≤0.15,0≤y≤0.20)
The difference of preparation method and embodiment 1 is: raw material is used average grain diameter D instead
50Be the bulky grain Mn of 24 μ m
3O
4With average grain diameter D
50Be the granule Mn of 6 μ m
3O
4, granule Mn
3O
4Quality: bulky grain Mn
3O
4Quality=2:8 is added with the Al (OH) of 1.8wt% in the batch mixing process
3
Initial stage charge-discharge characteristic and High temperature storage characteristic to the manganate cathode material for lithium of the present embodiment are tested, and method of testing is with embodiment 1, and test result sees Table 1.
The manganate cathode material for lithium of the present embodiment, chemical formula are Li
1+xMn
2-x-yM
yO
4, for Powdered.
(in formula, M is Al, 0.03≤x≤0.15,0≤y≤0.20)
The difference of preparation method and embodiment 7 is: granule Mn
3O
4Quality: bulky grain Mn
3O
4Quality=4:6 is added with the Al (OH) of 1.8wt% in the batch mixing process
3
Initial stage charge-discharge characteristic and High temperature storage characteristic to the manganate cathode material for lithium of the present embodiment are tested, and method of testing is with embodiment 1, and test result sees Table 1.
The manganate cathode material for lithium of the present embodiment, chemical formula are Li
1+xMn
2-x-yM
yO
4, for Powdered.
(in formula, M is Ni, 0.03≤x≤0.15,0≤y≤0.20)
The difference of preparation method and embodiment 7 is: granule Mn
3O
4Quality: bulky grain Mn
3O
4Quality=4:6 is added with the NiO of 1.8wt% in the batch mixing process.
Initial stage charge-discharge characteristic and High temperature storage characteristic to the manganate cathode material for lithium of the present embodiment are tested, and method of testing is with embodiment 1, and test result sees Table 1.
The manganate cathode material for lithium of the present embodiment, chemical formula are Li
1+xMn
2-x-yM
yO
4, for Powdered.(in formula, M is Cr, 0.03≤x≤0.15,0≤y≤0.20)
The difference of preparation method and embodiment 7 is: granule Mn
3O
4Quality: bulky grain Mn
3O
4Quality=4:6 is added with the CrO of 1.0wt% in the batch mixing process
3
Initial stage charge-discharge characteristic and High temperature storage characteristic to the manganate cathode material for lithium of the present embodiment are tested, and method of testing is with embodiment 1, and test result sees Table 1.
Embodiment 11
The manganate cathode material for lithium of the present embodiment, chemical formula are Li
1+xMn
2-x-yM
yO
4, for Powdered.
(in formula, M is Ti, 0.03≤x≤0.15,0≤y≤0.20)
The difference of preparation method and embodiment 7 is: granule Mn
3O
4Quality: bulky grain Mn
3O
4Quality=4:6 is added with the TiO of 0.5wt% in the batch mixing process
2
Initial stage charge-discharge characteristic and High temperature storage characteristic to the manganate cathode material for lithium of the present embodiment are tested, and method of testing is with embodiment 1, and test result sees Table 1.
Comparative example 1
This comparative example is with the difference of embodiment 1: be single raw material, namely only use 779.3g average grain diameter D
50The manganese compound of 17 μ m.
Initial stage charge-discharge characteristic and high temperature cyclic performance to this comparative example are tested, and method of testing is with embodiment 1, and test result sees Table 1.
Comparative example 2
This comparative example is with the difference of embodiment 1: raw material 545.5g average grain diameter D
50Be the granule MnO of 3 μ m
2With 233.8 g average grain diameter D
50Be the granule MnO of 17 μ m
2, granule MnO
2Quality: bulky grain MnO
2Quality=7:3.
Initial stage charge-discharge characteristic and high temperature cyclic performance to this comparative example are tested, and method of testing is with embodiment 1, and test result sees Table 1.
Comparative example 3
This comparative example is with the difference of embodiment 1: raw material 545.5g average grain diameter D
50Be the granule MnO of 3 μ m
2With 233.8 g average grain diameter D
50Be the granule MnO of 17 μ m
2, granule MnO
2Quality: bulky grain MnO
2Quality=7:3; Be added with the Al (OH) of 1.2wt% in the batch mixing process
3
Initial stage charge-discharge characteristic and high temperature cyclic performance to this comparative example are tested, and method of testing is with embodiment 1, and test result sees Table 1.
Beneficial effect is analyzed
As known from Table 1, the powder-compacting of each embodiment is 3.0g/cm
3, higher than prepared Comparative Examples 1 sample (2.66g/cm by single raw material
3).Yi Zhi adopts the mode of size particles collocation higher than the product compacting of adopting single raw material to obtain.Adopting the collocation of raw material size particles is the effective ways that promote powder-compacting.
The particle size distribution figure of comparative example 1 and Comparative Examples 1, in embodiment 1 sample, the particle segment of 0.5～2.5 μ m is less than Comparative Examples 1, and in embodiment 1 sample in the particle segment of 4.0～8.0 μ m more than Comparative Examples 1, illustrate that in embodiment 1, powder content lacks than Comparative Examples 1, and in embodiment 1, the small-particle of 4.0～8.0 μ m is more, and this part particle has larger contribution to improving powder-compacting.
Comparing embodiment 1, embodiment 4, the SEM figure of embodiment 8 and Comparative Examples 1, primary particle is formed by the granule growth, and smooth surface is reunited closely, and this structure is conducive to improve compacting.
With embodiment 1,2,3,4 synthetic LiMn2O4 powder have carried out the XRD detection, and its result as shown in Figure 1.Show that synthetic product is pure spinel-type LiMn
2O
4Material.Wherein the XRD diffraction maximum of embodiment 4 moves to right with respect to embodiment 1, embodiment 2 and embodiment 3 integral body.Because with the little Al of radius
3+Replaced the large Mn of radius
3+, lattice constant diminishes, and causes to the high angle skew, and Al is described
3+Doping has entered intracell, plays the effect of stable crystal structure.
Lattice constant diminishes, and corresponding crystallite dimension diminishes, the SEM figure of comparing embodiment 1 and embodiment 4, and the primary particle size in embodiment 4 is less than embodiment 1, with consistent from the XRD spectra analysis result.
The high rate performance comparative illustration.The discharge capacity of most of embodiment 2C with respect to 0.1C discharge capacity major part more than 96.0%, far above 81.8% of Comparative Examples 1.Because there have been two kinds of particles of size, short grained existence is improved the high rate performance of battery.
The high temperature cyclic performance comparative illustration.Each embodiment is at 60 ℃, and 1C circulation the 54th all capability retentions are all more than 90.0%, higher than Comparative Examples 1 and Comparative Examples 2.
Fig. 7 be embodiment 4 LiMn2O4 powder with the charging and discharging curve of 0.1C electric current, without 3.0～3.3V platform, the oxygen defect state is little, is indicating good high temperature cyclic performance.
Table 1 is the part physics and chemistry result that each embodiment and Comparative Examples detect
Claims (5)
1. manganate cathode material for lithium, it is characterized in that: chemical formula is Li
1+xMn
2-x-yM
yO
4, for Powdered;
In described chemical formula, M is one or more the element that is selected from Ni, Co, Mg, Al, Cr, Ti, 0.03≤x≤0.15,0≤y≤0.20.
2. a method for preparing manganate cathode material for lithium claimed in claim 1, is characterized in that, comprises the following steps: with average grain diameter D
50Be the granule manganese compound of 0.1～10 μ m, average grain diameter D
50Be the bulky grain manganese compound of 12～30 μ m, average grain diameter D
50Be the lithium compound of 2～12 μ m and the doped compound that contains the M element, press chemical formula Li
1+xMn
2-x-yM
yO
4Metering is than weighing, and the ball grinder batch mixing of packing into, batch mixing ball are alumina balls, ball material mass ratio (0.5～1): 1, mix 1～5h; The material pine burning alms bowl of packing into after mixing, the Muffle furnace sintering first is warming up to 600 ± 5 ℃, constant temperature 1～10h, be warming up to 750～1000 ℃, then constant temperature 1～10h is cooled to 600 ± 5 ℃, constant temperature 1～20h again, be cooled to again room temperature, then pulverize, mistake 〉=325 mesh sieves.
3. the preparation method of manganate cathode material for lithium according to claim 2 is characterized in that: in the manganese compound of described two kinds of different-grain diameters, and granule manganese compound quality: bulky grain manganese compound quality=(0.1～1): 1.
4. the preparation method of according to claim 2 or 3 described manganate cathode material for lithium, it is characterized in that: the doped compound of the described M of containing element is Al (OH)
3, CrO
3, NiO, TiO
2, MgO, Co
3O
4In one or more mixture, the addition of every kind of material is 0.05～5wt% of total material.
5. the application of manganate cathode material for lithium as claimed in claim 1 in non-aqueous electrolyte lithium secondary battery.
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| CN106532033A (en) * | 2015-09-09 | 2017-03-22 | 无锡晶石新型能源有限公司 | Preparation method for mixed lithium manganate material |
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| CN110904495A (en) * | 2019-12-02 | 2020-03-24 | 中南大学 | Preparation method of monocrystal polyhedral lithium manganate positive electrode material |
| CN114105220A (en) * | 2021-11-09 | 2022-03-01 | 远景动力技术(江苏)有限公司 | Modified spinel type positive electrode material, preparation method thereof and lithium ion battery positive electrode plate |
| CN114105220B (en) * | 2021-11-09 | 2024-01-16 | 远景动力技术(江苏)有限公司 | Modified spinel type positive electrode material, preparation method thereof and lithium ion battery positive electrode sheet |
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