CN102420326A - Preparation method of bulky-grain spinel lithium manganate material - Google Patents
Preparation method of bulky-grain spinel lithium manganate material Download PDFInfo
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- CN102420326A CN102420326A CN2011103801332A CN201110380133A CN102420326A CN 102420326 A CN102420326 A CN 102420326A CN 2011103801332 A CN2011103801332 A CN 2011103801332A CN 201110380133 A CN201110380133 A CN 201110380133A CN 102420326 A CN102420326 A CN 102420326A
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Abstract
The invention discloses a preparation method of a bulky-grain spinel lithium manganate material, which belongs to the field of electrochemical materials. The bulky-grain spinel lithium manganate material is prepared through carrying out high-temperature sintering on a raw material such as manganese dioxide or manganese carbonate as with a doped element M to be converted into uniformly-doped bulky-grain mangano-manganic oxide, using the bulky-grain mangano-manganic oxide as the raw material of a Mn source, mixing the bulky-grain mangano-manganic oxide with an original material of Li, and sintering the obtained mixture. The mangano-manganic oxide prepared by the invention has a good crystalline grain shape; the grain size is in normal distribution; after the bulky-grain mangano-manganic oxide is used as the raw material of the Mn source and mixed with the original material of the Li, a bulky-grain lithium manganate product with a low surface area can be obtained without the obtained miture at a temperature which exceeds 900 DEG C; and the problem that oxygen loss is caused when the bulky-grain lithium manganate is prepared by high sintering exceeding 900 DEG C is solved. The lithium manganate prepared by the method has uniform granularity; the average grain size of the lithium manganate can be controlled in a range of 5-15 mum through the process; the specific surface area is between 0.2 m<2>/g and 0.6 m<2>/g; crystalline grains are complete; and the high-low temperature cycle service is excellent. The method provided by the invention has a simple process and low cost, and is applicable to industrial production.
Description
Technical field
The present invention relates to a kind of preparation method of bulky grain spinelle manganic acid lithium material, it belongs to electrochemistry, powder metallurgy and technical field of electronic products.
Background technology
Positive electrode is the important component part of secondary lithium battery, and its performance quality just plays key effect to the development and the application of lithium ion battery with cost.In the cost of lithium battery preparation, the proportion that positive electrode accounts for is maximum, more than 30%.The positive electrode of having developed at present mainly contains cobalt acid lithium, lithium nickelate, multielement cathode, the LiMn2O4 of spinel structure and the LiFePO4 of olivine structural of stratiform.Above-mentioned system positive electrode respectively has pluses and minuses, and different systems are fit to different battery products.In design with when choosing anode material for lithium-ion batteries, take all factors into consideration specific energy, cycle performance, fail safe, cost and to the influence of environment.
Aspect the security performance of power lithium-ion battery; Positive electrode is a limiting lithium ion electrokinetic cell development key always; Compare with negative material, positive electrode energy density and power density are lower, and also are the main causes that causes the lithium-ion-power cell potential safety hazard.Therefore, seek high-energy-density, high safety, environmental protection and low-cost electrode material and become electrokinetic cell development key factor.The positive electrode that generally uses at present is respectively cobalt acid lithium, LiMn2O4, nickle cobalt lithium manganate and LiFePO4.Cobalt acid lithium costs an arm and a leg, and it is bigger to be used for the potential safety hazard of electrokinetic cell, does not generally use as power battery anode material, and LiMn2O4 and LiFePO4 are owing to aboundresources, and fail safe is good, is the comparatively desirable positive electrode of lithium-ion-power cell.
The outstanding advantage of LiMn2O4 be that cost is low, security performance good and the layer structure positive electrode the high power charging-discharging ability that can not compare; Though specific capacity is relatively low; But for the bigger electrokinetic cell of volume, do not constitute tangible weakness, thereby become the first-selected positive electrode of lithium-ion-power cell.The problem that lithium manganate material faces is a cycle life, and especially the cycle performance of high temperature (>=55 ℃) is undesirable.The problem of circulation volume decay under the high temperature is a principal element that hinders LiMn2O4 electrokinetic cell large-scale application all the time.
Generally believe, cause the reason of LiMn2O4 circulation time capacity attenuation to mainly contain following several kinds: the 1. dissolving of Mn influence; 2. Jahn-Teller distortion effect; 3. electrolyte decomposes under high potential; 4. instability of lattice etc.Lower the temperature, select the methods such as content of free acid in suitable electrolyte system, the reduction electrolyte to improve through element doping, surface modification, annealing.
Research shows the bulky grain of the low surface area that adopt mixing combines with morphology control prepares, and can obviously improve the high low temperature cycle performance of LiMn2O4.Mostly plain edition LiMn2O4 product is that primary particle forms less than 1 micron second particle, and crystal formation is incomplete, especially too big (1 m of specific area
2About/g), to material cycle life/especially high temperature service life is unfavorable.And the LiMn2O4 with good high low temperature cycle life is generally the bulky grain about 10 microns, because bulky grain has low specific area (less than 0.5 m
2/ g), reduced the contact area of material and electrolyte, can reduce the dissolving of manganese in the electrolyte, improve the stability of product in electrolyte, effectively improve the circulation (particularly high temperature circulation) and the storge quality of battery.
Usually improving sintering temperature is the effective method that improves the material granule granularity, reduces specific area with increasing sintering time; And must could effectively reduce its specific area in the high-temperature calcination that surpasses 10 hours more than 900 ℃ for lithium manganate material; But oxygen disappearance degree is more serious in the high-temperature calcination process, even can not full remuneration through annealing in process, partial oxygen lacks extremely harmful to high and low temperature cycle life; Inappropriate high-temperature calcination technology; Even if prepare the bulky grain of low specific surface area, but because the existence of oxygen disappearance problem makes its cycle life not only can not get improving, poor all the better.
Summary of the invention
The present invention seeks to through raw material manganese dioxide or manganese carbonate and doped chemical are carried out high temperature sintering; Make its bulky grain mangano-manganic oxide that converts even doping into, prepare oarse-grained lithium manganate material as the original material mixed sintering of Mn source raw material and Li.
A kind of preparation method of bulky grain spinelle manganic acid lithium material, concrete scheme is following:
A. with manganese dioxide (MnO
2) or manganese carbonate (MnCO
3) mix with certain proportion with doped chemical M, make that end product M/Mn=0.01-0.2, M are one or both elements among Al, Co, Ni, Cr, Zn, Y, Fe, Ag, Ca, V, Cu, Zr, Ti, Sn, Mo, La, Ce, Pr, the Nd;
B. with mixture between 900-1300 ℃, high-temperature calcination 1-48 hour, the cold or air cooling of stove;
C. 200 mesh sieves are crossed in broken powder process;
D. will more than contain the Mn source of doped chemical and the original material of Li mixes, wherein the mol ratio of Li and Mn is: Li/Mn=0.5-0.65, between 500-900 ℃ sintering 1-48 hour then, slow cooling to 200 ℃ was come out of the stove; The original material of the Li that selects for use comprises one or more in lithium carbonate, lithium nitrate or the lithium hydroxide.
E. broken powder process, powder classification.
The present invention is through carrying out high temperature sintering to raw material manganese dioxide or manganese carbonate and doped chemical; Make it convert the bulky grain mangano-manganic oxide of even doping into; The grain form of gained mangano-manganic oxide is good, and particle size distribution is normal distribution, as Mn source raw material with after the original material of Li mixes; Need not to surpass the LiMn2O4 product that 900 ℃ of sintering just can access the bulky grain low surface area, solved and surpass 900 ℃ of high temperature sinterings and prepare the problem that the bulky grain LiMn2O4 causes oxygen to lack.In the raw material modification stage, doped chemical is added simultaneously, the sintering of superhigh temperature makes element doping more even.Utilize the LiMn2O4 epigranular of prescription of the present invention and preparation method preparation, can control its average particle size particle size at 5-15 μ m through technology, specific area is at 0.2-0.6 m
2Between/the g, crystal grain is complete, and high low temperature cycle life is excellent.This preparation method technology is simple, cost is low, is useful for suitability for industrialized production.
Description of drawings:
Fig. 1 is the raw-material surface sweeping Electronic Speculum of the manganese dioxide of embodiment 1 shape appearance figure (SEM)
Fig. 2 is the raw-material particle size distribution figure of the manganese dioxide of embodiment 1
Fig. 3 is the X-ray diffractogram (XRD) of first section sintered product mangano-manganic oxide of embodiment 1
Fig. 4 is the surface sweeping Electronic Speculum shape appearance figure (SEM) of first section sintered product mangano-manganic oxide of embodiment 1
Fig. 5 is the particle size distribution figure of the phase I sintered product mangano-manganic oxide of embodiment 1
Fig. 6 is the X-ray diffractogram (XRD) of second section sintered product spinel lithium manganate of embodiment 1
Fig. 7 is the surface sweeping Electronic Speculum shape appearance figure (SEM) of second section sintered product spinel lithium manganate of embodiment 1
Fig. 8 is the particle size distribution figure of the second stage sintered product spinel lithium manganate of embodiment 1
Fig. 9 is 25 ℃ and 55 ℃ of following loop attenuation figure of the second stage sintered product spinel lithium manganate of embodiment 1
Figure 10 is the charging and discharging curve of following 1-100 the circulation of 25 ℃ of second stage sintered product spinel lithium manganate of embodiment 1
Embodiment:
The raw material that adopts is manganese dioxide, lithium carbonate and the aluminium hydroxide of technical grade, and final proportioning is Li
1.05Mn
1.77Al
0.18Ox at first mixes manganese dioxide and aluminium hydroxide by proportioning, be as cold as 200 ℃ at 1100 ℃ of sintering 10h stoves and come out of the stove; Broken back mixes with lithium carbonate, ℃ comes out of the stove broken powder process in the slow cooling to 200 in 10 hours of 800 ℃ of sintering; Powder classification promptly obtains required spinel lithium manganate.
Used raw material manganese dioxide is sheet (like Fig. 1), and particle size distribution wide (like Fig. 2) obtains product with first section sintering and does the XRD test, and as shown in Figure 3, this product is a mangano-manganic oxide.The SEM figure of Fig. 4 can find out that the crystal grain crystalline form is complete, and granularity is about 8 microns.Fig. 5 is a particle size distribution, can see that particle size distribution is normal distribution.Fig. 6 is the XRD of end product, can see it being spinel lithium manganate, and the peak of high angle squints to low-angle, explains that doped chemical diminishes lattice and makes spinel structure become more stable, thereby has significantly improved the cycle performance of material.The crystal grain perfect crystalline (as shown in Figure 7) of gained LiMn2O4, crystal particle scale are about 10 microns, and particle size distribution is normal distribution (as shown in Figure 8).
The gained material is used for battery performance test, with LiMn2O4 sample, SP with gather difluoroethylene (PVDF) partially and form, after it is mixed according to 80:15:5 (mass ratio); The slurries that mix are applied on the aluminium foil, and as negative pole, electrolyte is 1mol/L LiPF6/EC+DEC+DMC (volume ratio 1:1:1) with the Li sheet; It is assembled into 2032 button cells, 25 ℃ and 55 ℃ of following 0.5C chargings, 1C discharge; The 5min that pauses at interval circulates 500 times, and charging/discharging voltage is 3.3-4.30V.Fig. 9 is the variation of discharge capacity with cycle-index, and 25 ℃ of following initial discharge capacities are 96mAh/g, and 500 times the circulation back is 91.9mAh/g; Residual capacity 95.7%; 55 ℃ of following initial discharge capacities are 98.6mAh/g, and 200 times the circulation back is 87.2mAh/g, residual capacity 88.8%.Figure 10 is the charging and discharging curve of following 1-100 the circulation of 25 ℃ of spinel lithium manganate, finds out from charging and discharging curve, modifies the 4.0V and the 4.15V abolition of plateau of back material, becomes smooth continuous curve.
Embodiment 2
The raw material that adopts is manganese dioxide, lithium carbonate and the cobaltosic oxide of technical grade, and final proportioning is Li
1.1Mn
1.72Co
0.18Ox at first mixes manganese dioxide and cobaltosic oxide by proportioning, come out of the stove at 1100 ℃ of sintering 10h and in air, cool off; Broken back mixes with lithium hydroxide, ℃ comes out of the stove broken powder process in the slow cooling to 200 in 10 hours of 800 ℃ of sintering; Powder classification promptly obtains required spinel lithium manganate.
The raw material that adopts is manganese carbonate, lithium carbonate, aluminium hydroxide and the yittrium oxide of technical grade, and final proportioning is Li
1.1Mn
1.72Al
0.13Y
0.05Ox; At first mangano-manganic oxide, aluminium hydroxide and yittrium oxide are mixed by proportioning, come out of the stove to be chilled in 1000 ℃ of air of coming out of the stove at stove at 1200 ℃ of sintering 10h and cool off, broken back mixes with lithium hydroxide; ℃ come out of the stove in the slow cooling to 200 in 10 hours of 800 ℃ of sintering; Broken powder process, powder classification promptly obtains required spinel lithium manganate.
Claims (2)
1. the preparation method of a bulky grain spinelle manganic acid lithium material is characterized in that, specifically preparation process may further comprise the steps:
A. manganese dioxide or manganese carbonate and doped chemical M are mixed with certain proportion; Make that the mol ratio of doped chemical M and Mn is in the end product: M/Mn=0.01-0.2, M are one or both elements among Al, Co, Ni, Cr, Zn, Y, Fe, Ag, Ca, V, Cu, Zr, Ti, Sn, Mo, La, Ce, Pr, the Nd;
B. with mixture between 900-1300 ℃, high-temperature calcination 1-48 hour, the cold or air cooling of stove;
C. 200 mesh sieves are crossed in broken powder process;
D. will cross the Mn source that contains doped chemical of 200 mesh sieves and the original material of Li and mix, wherein the mol ratio of Li and Mn is: Li/Mn=0.5-0.65, and between 500-900 ℃ sintering 1-48 hour then, slow cooling to 200 ℃ was come out of the stove;
E. broken powder process, powder classification.
2. the preparation method of bulky grain spinelle manganic acid lithium material as claimed in claim 1 is characterized in that: the original material of the Li that selects for use comprises one or more in lithium carbonate, lithium nitrate or the lithium hydroxide.
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Cited By (12)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103050680A (en) * | 2012-12-19 | 2013-04-17 | 中钢集团安徽天源科技股份有限公司 | High-density doped trimanganese tetroxide and preparation method thereof |
| CN104518213A (en) * | 2013-09-26 | 2015-04-15 | 天津通一新能源科技有限公司 | Synthesis method of poly lithium manganate material |
| CN106299255A (en) * | 2016-08-25 | 2017-01-04 | 合肥国轩高科动力能源有限公司 | Preparation method of large-particle-size spinel lithium nickel manganese oxide |
| CN106410180A (en) * | 2016-11-11 | 2017-02-15 | 河南师范大学 | Lithium ion battery positive pole material, and preparation method and application thereof |
| CN107364901A (en) * | 2017-07-27 | 2017-11-21 | 湖南长远锂科有限公司 | A kind of high-voltage spinel nickel lithium manganate cathode material and preparation method thereof |
| CN109437340A (en) * | 2018-12-07 | 2019-03-08 | 长安大学 | A kind of rare earth modified NiMn2O4Spinel powder and its preparation method and application |
| CN109585793A (en) * | 2017-09-28 | 2019-04-05 | 江苏津谊新能源科技有限公司 | A kind of anode material for lithium-ion batteries |
| CN111342045A (en) * | 2020-03-21 | 2020-06-26 | 青岛红星新能源技术有限公司 | Preparation method of high-performance power type lithium manganate positive electrode material |
| CN111348686A (en) * | 2020-03-21 | 2020-06-30 | 青岛红星新能源技术有限公司 | Method for modifying high-capacity high-rate-performance high-voltage lithium manganate cathode material |
| CN112744866A (en) * | 2020-12-29 | 2021-05-04 | 无锡晶石新型能源股份有限公司 | Preparation method of lithium manganate with low specific surface area and large particle size |
| CN115724468A (en) * | 2022-11-21 | 2023-03-03 | 中钢天源股份有限公司 | Preparation method of pre-doped lithium manganate precursor material and product thereof |
| CN115849453A (en) * | 2022-12-16 | 2023-03-28 | 惠州亿纬锂能股份有限公司 | Ternary codoped manganese dioxide material and preparation method and application thereof |
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Cited By (17)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103050680A (en) * | 2012-12-19 | 2013-04-17 | 中钢集团安徽天源科技股份有限公司 | High-density doped trimanganese tetroxide and preparation method thereof |
| CN103050680B (en) * | 2012-12-19 | 2016-02-10 | 中钢集团安徽天源科技股份有限公司 | A kind of high density doping mangano-manganic oxide and preparation method thereof |
| CN104518213A (en) * | 2013-09-26 | 2015-04-15 | 天津通一新能源科技有限公司 | Synthesis method of poly lithium manganate material |
| CN106299255A (en) * | 2016-08-25 | 2017-01-04 | 合肥国轩高科动力能源有限公司 | Preparation method of large-particle-size spinel lithium nickel manganese oxide |
| CN106299255B (en) * | 2016-08-25 | 2019-09-10 | 合肥国轩高科动力能源有限公司 | Preparation method of spinel-type lithium nickel manganese oxide with large particle size |
| CN106410180A (en) * | 2016-11-11 | 2017-02-15 | 河南师范大学 | Lithium ion battery positive pole material, and preparation method and application thereof |
| CN107364901A (en) * | 2017-07-27 | 2017-11-21 | 湖南长远锂科有限公司 | A kind of high-voltage spinel nickel lithium manganate cathode material and preparation method thereof |
| CN107364901B (en) * | 2017-07-27 | 2019-03-05 | 湖南长远锂科有限公司 | A kind of high-voltage spinel nickel lithium manganate cathode material and preparation method thereof |
| CN109585793A (en) * | 2017-09-28 | 2019-04-05 | 江苏津谊新能源科技有限公司 | A kind of anode material for lithium-ion batteries |
| CN109437340A (en) * | 2018-12-07 | 2019-03-08 | 长安大学 | A kind of rare earth modified NiMn2O4Spinel powder and its preparation method and application |
| CN111342045A (en) * | 2020-03-21 | 2020-06-26 | 青岛红星新能源技术有限公司 | Preparation method of high-performance power type lithium manganate positive electrode material |
| CN111348686A (en) * | 2020-03-21 | 2020-06-30 | 青岛红星新能源技术有限公司 | Method for modifying high-capacity high-rate-performance high-voltage lithium manganate cathode material |
| CN112744866A (en) * | 2020-12-29 | 2021-05-04 | 无锡晶石新型能源股份有限公司 | Preparation method of lithium manganate with low specific surface area and large particle size |
| CN115724468A (en) * | 2022-11-21 | 2023-03-03 | 中钢天源股份有限公司 | Preparation method of pre-doped lithium manganate precursor material and product thereof |
| CN115724468B (en) * | 2022-11-21 | 2024-03-19 | 中钢天源股份有限公司 | Preparation method of pre-doped lithium manganate precursor material and product thereof |
| CN115849453A (en) * | 2022-12-16 | 2023-03-28 | 惠州亿纬锂能股份有限公司 | Ternary codoped manganese dioxide material and preparation method and application thereof |
| CN115849453B (en) * | 2022-12-16 | 2024-05-03 | 惠州亿纬锂能股份有限公司 | Ternary co-doped manganese dioxide material and preparation method and application thereof |
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Application publication date: 20120418 |