CN104538616A - Preparation method of cathode material-lithium manganate of lithium-ion power battery - Google Patents
Preparation method of cathode material-lithium manganate of lithium-ion power battery Download PDFInfo
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- CN104538616A CN104538616A CN201410796688.9A CN201410796688A CN104538616A CN 104538616 A CN104538616 A CN 104538616A CN 201410796688 A CN201410796688 A CN 201410796688A CN 104538616 A CN104538616 A CN 104538616A
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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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- H01M4/36—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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- H01M—PROCESSES OR MEANS, e.g. BATTERIES, FOR THE DIRECT CONVERSION OF CHEMICAL ENERGY INTO ELECTRICAL ENERGY
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- H01M10/0525—Rocking-chair batteries, i.e. batteries with lithium insertion or intercalation in both electrodes; Lithium-ion batteries
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Abstract
The invention discloses a preparation method of a cathode material-lithium manganate of a lithium-ion power battery. Carbon used as a reducing agent and silicon dioxide used as a coating agent are added in one or two of manganese source materials including electrolytic manganese dioxide, chemical manganese dioxide and manganese carbonate for high-temperature sintering to prepare a lithium manganate precursor with less than or equal to 0.15% (in mass percentage) of SO4<2->, then the lithium manganate precursor is mixed with lithium carbonate, the mixture is sintered to obtain lithium manganate with less than or equal to 0.13% (in mass percentage) of SO4<2->. According to the preparation method, the modified reaction of the manganese source material is enabled to be carried out in a direction for improving the SO4<2-> removing effect by use of the reducibility of C, and the coating agent-SiO2 is remained in the lithium manganate precursor, therefore, the integration effect of impurity removal and coating modification can be achieved; the prepared lithium manganate has excellent physical and chemical properties and electrochemical performance, has the capacity retention ratio more than or equal to 85% after being cycled for 1000 times under 1C multiplying power, the initial capacity of the lithium manganate battery is improved compared with that of the lithium manganate battery prepared by a common method, the cycle performance is improved obviously, the battery performance is stable and the preparation method can be used for the power battery.
Description
Technical field
The present invention relates to a kind of preparation method of lithium ion power battery cathode material LiMn2O4.
Background technology
At present, the raw material preparing lithium cell anode material lithium manganate adopts the manganese source material such as various Mn oxide or manganese salt usually.SO is found in research
4 2-be the important foreign ion affecting lithium cell anode material lithium manganate chemical property, reduce manganese source material SO
4 2-content be the most important factor improving LiMn2O4 chemical property.At present, SO in various Mn oxide or manganese salt on market
4 2-content is higher, is generally 0.6% ~ 2%, the LiMn2O4 product SO made with this manganese source material
4 2-content reaches 0.8%-2%, has a strong impact on the chemical property of manganate cathode material for lithium.Therefore, SO in manganese source material how is reduced
4 2-content, be one of key technology solving lithium ion power battery cathode material LiMn2O4 high temperature cyclic performance and storge quality.
According to the literature, high-temperature process reduces SO in manganese source material
4 2-the effective ways of content, SO
4 2-there is following reaction under the high temperature conditions: SO
4 2-→ SO
2+ O
2.This reaction is the endothermic reaction, and temperature is higher, reacts more thorough, SO
4 2-clearance larger, but temperature is higher, and larger to the structural deterioration of manganese source material, the LiMn2O4 architectural characteristic of preparation is poorer, causes the chemical property of LiMn2O4 to be deteriorated.Therefore, the SO in manganese source material how is effectively reduced at a lower temperature
4 2-content is the key improving LiMn2O4 impurity-eliminating effect.From SO
4 2-removal reaction equation it can also be seen that, this reaction is reduction reaction, under the condition that temperature is certain, add appropriate reducing agent be conducive to react carrying out, SO can be improved significantly
4 2-removal effect.
Summary of the invention
The object of the invention is, in order to not reduce under lithium manganate material electrical property head puts the prerequisite of capacity, significantly improve the cycle performance of electric energy, provide a kind of and reduce SO
4 2-the preparation method of the lithium ion power battery cathode material LiMn2O4 of content, it is characterized in that with carbon (C) be reducing agent, with silicon dioxide (SiO
2) be covering, first reducing agent and covering are added in manganese source material and carry out high temperature sintering, make SO
4 2-the LiMn2O4 precursor of mass percentage≤0.15%, then sinter after mixing with lithium carbonate with this manganate precursor for lithium, finally make SO
4 2-the LiMn2O4 product of mass percentage≤0.13%.SO
4 2-there is reduction reaction under the high temperature conditions: SO
4 2-→ SO
2+ O
2.The present invention selects carbon (C) as the reducing agent of this reaction, is conducive to the carrying out of reduction reaction, can improves SO significantly
4 2-removal effect, reach the modified effect obviously improving LiMn2O4.
Described manganese source material comprise in electrolytic manganese dioxide, chemical manganese bioxide, manganese carbonate one or both.
The mass ratio of the source material of manganese described in the present invention and reducing agent C is 1 ︰ 0.01 ~ 0.1, manganese source material and covering SiO
2mass ratio be 1 ︰ 0.01 ~ 0.1, mixed mixture puts into sintering furnace in proportion, manganate precursor for lithium sintering schedule is be warming up to 600 ~ 900 DEG C with the speed of 1 ~ 5 DEG C/min, sintering 3 ~ 20h, be cooled to 300 DEG C with the speed of 1 ~ 5 DEG C/min, cool to room temperature with the furnace, through pulverizing grinding, cross 200 mesh sieves, obtain SO
4 2-the LiMn2O4 precursor of mass percentage≤0.15%.Again by this manganate precursor for lithium and lithium carbonate by Mn ︰ Li=2 ︰ 1.05 molar ratio ingredient mix, LiMn2O4 sintering schedule is be warming up to 800 DEG C with the speed of 5 DEG C/min, sintering 16h, room temperature is cooled to again with the speed of 5 DEG C/min, grinding, sieves, finally obtains SO
4 2-the lithium ion power battery cathode material LiMn2O4 product of mass percentage≤0.13%.
Manganese source material of the present invention comprise in electrolytic manganese dioxide, chemical manganese bioxide, manganese carbonate one or both.That two kinds of manganese source materials mass ratio that feeds intake is 1:1 when manganese source material is two kinds.
The present invention utilizes the reproducibility of C, after adding appropriate C, carry out high-temperature process, makes the modified-reaction of manganese source material towards being conducive to improving SO
4 2-the direction of removal effect carry out, improve SO
4 2-clearance, improve the modified effect of manganese source material.CO is become after reducing agent C is at high temperature oxidized
2gaseous volatilization falls, and can not affect the performance of manganese source material, covering SiO
2then stay in manganate precursor for lithium, sintering with lithium carbonate the integrated result reaching removal of impurities and coating modification in the process preparing LiMn2O4 further.With SiO
2as LiMn2O4 clad material, by being first added in manganese source material, then carrying out LiMn2O4 coating modification in LiMn2O4 preparation, under the prerequisite of capacity can being put not reducing lithium manganate material electrical property head, significantly improving the cycle performance of electric energy.SO in the LiMn2O4 prepared by the method
4 2-mass percentage is less than 0.13%, physical and chemical performance and excellent electrochemical performance.The LiMn2O4 of preparation is that the lithium ion battery of positive electrode assembling circulates 1000 capability retention >=85% under 1C multiplying power, the lithium manganate battery head prepared compared with commonsense method puts capacity raising, cycle performance obviously improves, and battery performance is stablized, and can be used for electrokinetic cell.This process is simple to operate, is easy to realize industrialization.
Embodiment
Embodiment 1: by 2kg manganese carbonate (SO
4 2-mass percentage is 1.02%), 0.02kgC and 0.2kgSiO
2mixing, mixture puts into sintering furnace, is warming up to 600 DEG C with the speed of 1 DEG C/min, and sintering 20h, is cooled to 300 DEG C with the speed of 1 DEG C/min, then cools to room temperature with the furnace.Through pulverizing grinding, crossing 200 mesh sieves, obtaining SO
4 2-the LiMn2O4 precursor of mass percentage 0.15%.Again with this manganate precursor for lithium and lithium carbonate by Mn ︰ Li=2 ︰ 1.05 molar ratio ingredient mix, in sintering furnace, be warming up to 800 DEG C with the speed of 5 DEG C/min, sintering 16h, room temperature is cooled to again with the speed of 5 DEG C/min, grinding, sieves, the LiMn2O4 product SO obtained
4 2-content is 0.13%, and under the lithium ion battery 1C multiplying power of assembling for positive electrode with this LiMn2O4, circulation 1000 capability retentions are for 85.58%.
Embodiment 2: by 2kg chemical manganese bioxide (SO
4 2-mass percentage is 1.24%), 0.06kgC and 0.16kgSiO
2mixing, mixture puts into sintering furnace, is warming up to 800 DEG C with the speed of 3 DEG C/min, and sintering 12h, is cooled to 300 DEG C with the speed of 3 DEG C/min, then cools to room temperature with the furnace.Through pulverizing grinding, crossing 200 mesh sieves, obtaining SO
4 2-the LiMn2O4 precursor of mass percentage 0.12%.Again with this manganate precursor for lithium and lithium carbonate by Mn ︰ Li=2 ︰ 1.05 molar ratio ingredient mix, in sintering furnace, be warming up to 800 DEG C with the speed of 5 DEG C/min, sintering 16h, room temperature is cooled to again with the speed of 5 DEG C/min, grinding, sieves, the LiMn2O4 product SO obtained
4 2-content is 0.10%, and under the lithium ion battery 1C multiplying power of assembling for positive electrode with this LiMn2O4, circulation 1000 capability retentions are for 86.73%.
Embodiment 3: by 2kg electrolytic manganese dioxide (SO
4 2-mass percentage is 1.84%), 0.10kgC and 0.12kgSiO
2mixing, mixture puts into sintering furnace, is warming up to 900 DEG C with the speed of 5 DEG C/min, and sintering 3h, is cooled to 300 DEG C with the speed of 5 DEG C/min, then cools to room temperature with the furnace.Through pulverizing grinding, crossing 200 mesh sieves, obtaining SO
4 2-the LiMn2O4 precursor of mass percentage 0.13%.Again with this manganate precursor for lithium and lithium carbonate by Mn ︰ Li=2 ︰ 1.05 molar ratio ingredient mix, in sintering furnace, be warming up to 800 DEG C with the speed of 5 DEG C/min, sintering 16h, room temperature is cooled to again with the speed of 5 DEG C/min, grinding, sieves, the LiMn2O4 product SO obtained
4 2-content is 0.11%, and under the lithium ion battery 1C multiplying power of assembling for positive electrode with this LiMn2O4, circulation 1000 capability retentions are for 86.21%.
Embodiment 4: by 2kg manganese carbonate (SO
4 2-mass percentage is 1.02%), 0.12kgC and 0.10kgSiO
2mixing, mixture puts into sintering furnace, is warming up to 700 DEG C with the speed of 4 DEG C/min, and sintering 10h, is cooled to 300 DEG C with the speed of 4 DEG C/min, then cools to room temperature with the furnace.Through pulverizing grinding, crossing 200 mesh sieves, obtaining SO
4 2-the LiMn2O4 precursor of mass percentage 0.09%.Again with this manganate precursor for lithium and lithium carbonate by Mn ︰ Li=2 ︰ 1.05 molar ratio ingredient mix, in sintering furnace, be warming up to 800 DEG C with the speed of 5 DEG C/min, sintering 16h, room temperature is cooled to again with the speed of 5 DEG C/min, grinding, sieves, the LiMn2O4 product SO obtained
4 2-content is 0.08%, and under the lithium ion battery 1C multiplying power of assembling for positive electrode with this LiMn2O4, circulation 1000 capability retentions are for 87.03%.
Embodiment 5: by 2kg chemical manganese bioxide (SO
4 2-mass percentage is 1.24%), 0.16kgC and 0.06kgSiO
2mixing, mixture puts into sintering furnace, is warming up to 850 DEG C with the speed of 2 DEG C/min, and sintering 8h, is cooled to 300 DEG C with the speed of 2 DEG C/min, then cools to room temperature with the furnace.Through pulverizing grinding, crossing 200 mesh sieves, obtaining SO
4 2-the LiMn2O4 precursor of mass percentage 0.10%.Again with this manganate precursor for lithium and lithium carbonate by Mn ︰ Li=2 ︰ 1.05 molar ratio ingredient mix, in sintering furnace, be warming up to 800 DEG C with the speed of 5 DEG C/min, sintering 16h, room temperature is cooled to again with the speed of 5 DEG C/min, grinding, sieves, the LiMn2O4 product SO obtained
4 2-content is 0.08%, and under the lithium ion battery 1C multiplying power of assembling for positive electrode with this LiMn2O4, circulation 1000 capability retentions are for 86.64%.
Embodiment 6: by 2kg electrolytic manganese dioxide (SO
4 2-mass percentage is 1.84%), 0.20kgC and 0.02kgSiO
2mixing, mixture puts into sintering furnace, is warming up to 800 DEG C with the speed of 2 DEG C/min, and sintering 16h, is cooled to 300 DEG C with the speed of 2 DEG C/min, then cools to room temperature with the furnace.Through pulverizing grinding, crossing 200 mesh sieves, obtaining SO
4 2-the LiMn2O4 precursor of mass percentage 0.11%.Again with this manganate precursor for lithium and lithium carbonate by Mn ︰ Li=2 ︰ 1.05 molar ratio ingredient mix, in sintering furnace, be warming up to 800 DEG C with the speed of 5 DEG C/min, sintering 16h, room temperature is cooled to again with the speed of 5 DEG C/min, grinding, sieves, the LiMn2O4 product SO obtained
4 2-content is 0.09%, and under the lithium ion battery 1C multiplying power of assembling for positive electrode with this LiMn2O4, circulation 1000 capability retentions are for 86.01%.
Embodiment 7: by 2kg manganese carbonate (SO
4 2-mass percentage is 1.02%), 0.06kgC and 0.06kgSiO
2mixing, mixture puts into sintering furnace, is warming up to 750 DEG C with the speed of 3 DEG C/min, and sintering 10h, is cooled to 300 DEG C with the speed of 3 DEG C/min, then cools to room temperature with the furnace.Through pulverizing grinding, crossing 200 mesh sieves, obtaining SO
4 2-the LiMn2O4 precursor of mass percentage 0.13%.Again with this manganate precursor for lithium and lithium carbonate by Mn ︰ Li=2 ︰ 1.05 molar ratio ingredient mix, in sintering furnace, be warming up to 800 DEG C with the speed of 5 DEG C/min, sintering 16h, room temperature is cooled to again with the speed of 5 DEG C/min, grinding, sieves, the LiMn2O4 product SO obtained
4 2-content is 0.11%, and under the lithium ion battery 1C multiplying power of assembling for positive electrode with this LiMn2O4, circulation 1000 capability retentions are for 86.12%.
Embodiment 8: by 2kg electrolytic manganese dioxide (SO
4 2-mass percentage is 1.84%), 0.10kgC and 0.08kg SiO
2mixing, mixture puts into sintering furnace, is warming up to 850 DEG C with the speed of 4 DEG C/min, and sintering 12h, is cooled to 300 DEG C with the speed of 4 DEG C/min, then cools to room temperature with the furnace.Through pulverizing grinding, crossing 200 mesh sieves, obtaining SO
4 2-the LiMn2O4 precursor of mass percentage 0.13%.Again with this manganate precursor for lithium and lithium carbonate by Mn ︰ Li=2 ︰ 1.05 molar ratio ingredient mix, in sintering furnace, be warming up to 800 DEG C with the speed of 5 DEG C/min, sintering 16h, room temperature is cooled to again with the speed of 5 DEG C/min, grinding, sieves, the LiMn2O4 product SO obtained
4 2-content is 0.11%, and under the lithium ion battery 1C multiplying power of assembling for positive electrode with this LiMn2O4, circulation 1000 capability retentions are for 85.99%.
Embodiment 9: by 2kg chemical manganese bioxide (SO
4 2-mass percentage is 1.24%), 0.16kgC and 0.16kg SiO
2mixing, mixture puts into sintering furnace, is warming up to 850 DEG C with the speed of 2 DEG C/min, and sintering 16h, is cooled to 300 DEG C with the speed of 2 DEG C/min, then cools to room temperature with the furnace.Through pulverizing grinding, crossing 200 mesh sieves, obtaining SO
4 2-the LiMn2O4 precursor of mass percentage 0.09%.Again with this manganate precursor for lithium and lithium carbonate by Mn ︰ Li=2 ︰ 1.05 molar ratio ingredient mix, in sintering furnace, be warming up to 800 DEG C with the speed of 5 DEG C/min, sintering 16h, room temperature is cooled to again with the speed of 5 DEG C/min, grinding, sieves, the LiMn2O4 product SO obtained
4 2-content is 0.08%, and under the lithium ion battery 1C multiplying power of assembling for positive electrode with this LiMn2O4, circulation 1000 capability retentions are for 87.32%.
Embodiment 10: by 1kg manganese carbonate (SO
4 2-mass percentage is 1.02%), 1kg chemical manganese bioxide (SO
4 2-mass percentage is 1.24%), 0.06kgC and 0.16kg SiO
2mixing, mixture puts into sintering furnace, is warming up to 800 DEG C with the speed of 3 DEG C/min, and sintering 8h, is cooled to 300 DEG C with the speed of 3 DEG C/min, then cools to room temperature with the furnace.Through pulverizing grinding, crossing 200 mesh sieves, obtaining SO
4 2-the LiMn2O4 precursor of mass percentage 0.11%.Again with this manganate precursor for lithium and lithium carbonate by Mn ︰ Li=2 ︰ 1.05 molar ratio ingredient mix, in sintering furnace, be warming up to 800 DEG C with the speed of 5 DEG C/min, sintering 16h, room temperature is cooled to again with the speed of 5 DEG C/min, grinding, sieves, the LiMn2O4 product SO obtained
4 2-content is 0.09%, and under the lithium ion battery 1C multiplying power of assembling for positive electrode with this LiMn2O4, circulation 1000 capability retentions are for 86.98%.
Embodiment 11: by 1kg manganese carbonate (SO
4 2-mass percentage is 1.02%), 1kg electrolytic manganese dioxide (SO
4 2-mass percentage is 1.84%), 0.10kgC and 0.12kg SiO
2mixing, mixture puts into sintering furnace, is warming up to 750 DEG C with the speed of 2 DEG C/min, and sintering 16h, is cooled to 300 DEG C with the speed of 2 DEG C/min, then cools to room temperature with the furnace.Through pulverizing grinding, crossing 200 mesh sieves, obtaining SO
4 2-the LiMn2O4 precursor of mass percentage 0.11%.Again with this manganate precursor for lithium and lithium carbonate by Mn ︰ Li=2 ︰ 1.05 molar ratio ingredient mix, in sintering furnace, be warming up to 800 DEG C with the speed of 5 DEG C/min, sintering 16h, room temperature is cooled to again with the speed of 5 DEG C/min, grinding, sieves, the LiMn2O4 product SO obtained
4 2-content is 0.09%, and under the lithium ion battery 1C multiplying power of assembling for positive electrode with this LiMn2O4, circulation 1000 capability retentions are for 86.74%.
Embodiment 12: by 1kg chemical manganese bioxide (SO
4 2-mass percentage is 1.24%), 1kg electrolytic manganese dioxide (SO
4 2-mass percentage is 1.84%), 0.16kgC and 0.06kg SiO
2mixing, mixture puts into sintering furnace, is warming up to 850 DEG C with the speed of 2 DEG C/min, and sintering 16h, is cooled to 300 DEG C with the speed of 2 DEG C/min, then cools to room temperature with the furnace.Through pulverizing grinding, crossing 200 mesh sieves, obtaining SO
4 2-the LiMn2O4 precursor of mass percentage 0.11%.Again with this manganate precursor for lithium and lithium carbonate by Mn ︰ Li=2 ︰ 1.05 molar ratio ingredient mix, in sintering furnace, be warming up to 800 DEG C with the speed of 5 DEG C/min, sintering 16h, room temperature is cooled to again with the speed of 5 DEG C/min, grinding, sieves, the LiMn2O4 product SO obtained
4 2-content is 0.09%, and under the lithium ion battery 1C multiplying power of assembling for positive electrode with this LiMn2O4, circulation 1000 capability retentions are for 86.13%.
Claims (3)
1. the preparation method of a lithium ion power battery cathode material LiMn2O4, it is characterized in that with carbon being reducing agent, take silicon dioxide as covering, add in manganese source material electrolytic manganese dioxide, chemical manganese bioxide, manganese carbonate to carry out high temperature sintering in one or both make SO
4 2-the LiMn2O4 precursor of mass percentage≤0.15%, then sinter after mixing with lithium carbonate with this manganate precursor for lithium, finally obtain SO
4 2-the product LiMn2O4 of mass percentage≤0.13%.
2. the preparation method of a kind of lithium ion power battery cathode material LiMn2O4 according to claim 1, it is characterized in that the mass ratio of manganese source material and reducing agent carbon is 1 ︰ 0.01 ~ 0.1, the mass ratio of manganese source material and covering silicon dioxide is 1 ︰ 0.01 ~ 0.1, manganate precursor for lithium sintering schedule is be warming up to 600 ~ 900 DEG C with the speed of 1 ~ 5 DEG C/min, sintering 3 ~ 20h, 300 DEG C are cooled to again with the speed of 1 ~ 5 DEG C/min, cool to room temperature with the furnace, through pulverizing grinding, cross 200 mesh sieves, obtain SO
4 2-the LiMn2O4 precursor of mass percentage≤0.15%, again manganate precursor for lithium and lithium carbonate are pressed the molar ratio ingredient mixed sintering of Mn ︰ Li=2 ︰ 1.05, LiMn2O4 sintering schedule is be warming up to 800 DEG C with the speed of 5 DEG C/min, sintering 16h, room temperature is cooled to again with the speed of 5 DEG C/min, grinding, sieves, finally obtains SO
4 2-the product LiMn2O4 of mass percentage≤0.13%.
3. the method according to claim 1 and 2, is characterized in that: when manganese source material is two kinds in electrolytic manganese dioxide, chemical manganese bioxide, manganese carbonate, and the mass ratio that feeds intake of two kinds of manganese source materials is 1 ︰ 1.
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Cited By (3)
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| CN105958034A (en) * | 2016-07-06 | 2016-09-21 | 福建师范大学 | Method for preparing silicon oxide coated spinel lithium-rich lithium manganate material |
| CN108083342A (en) * | 2017-10-31 | 2018-05-29 | 湖南海利锂电科技股份有限公司 | Lithium-ion-power cell manganate cathode material for lithium and preparation method thereof |
| CN111362307A (en) * | 2020-03-09 | 2020-07-03 | 晋江云智新材料科技有限公司 | Preparation method of single-crystal lithium manganate positive electrode material for lithium ion battery |
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| CN103311531A (en) * | 2013-05-20 | 2013-09-18 | 无锡晶石新型能源有限公司 | Method for preparing lithium manganate through adding sintering aid by means of low temperature sintering |
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| Publication number | Priority date | Publication date | Assignee | Title |
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| CN105958034A (en) * | 2016-07-06 | 2016-09-21 | 福建师范大学 | Method for preparing silicon oxide coated spinel lithium-rich lithium manganate material |
| CN108083342A (en) * | 2017-10-31 | 2018-05-29 | 湖南海利锂电科技股份有限公司 | Lithium-ion-power cell manganate cathode material for lithium and preparation method thereof |
| CN108083342B (en) * | 2017-10-31 | 2019-08-13 | 湖南海利锂电科技股份有限公司 | Lithium-ion-power cell manganate cathode material for lithium and preparation method thereof |
| CN111362307A (en) * | 2020-03-09 | 2020-07-03 | 晋江云智新材料科技有限公司 | Preparation method of single-crystal lithium manganate positive electrode material for lithium ion battery |
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