CN101630727A - Surface modified lithium ion battery anode material lithium cobaltate and modifying method thereof - Google Patents
Surface modified lithium ion battery anode material lithium cobaltate and modifying method thereof Download PDFInfo
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- CN101630727A CN101630727A CN200910044154A CN200910044154A CN101630727A CN 101630727 A CN101630727 A CN 101630727A CN 200910044154 A CN200910044154 A CN 200910044154A CN 200910044154 A CN200910044154 A CN 200910044154A CN 101630727 A CN101630727 A CN 101630727A
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- Prior art keywords
- lithium
- calcium carbonate
- cobalt acid
- modifying method
- anode material
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- WHXSMMKQMYFTQS-UHFFFAOYSA-N Lithium Chemical compound [Li] WHXSMMKQMYFTQS-UHFFFAOYSA-N 0.000 title claims abstract description 50
- 229910052744 lithium Inorganic materials 0.000 title claims abstract description 50
- 238000000034 method Methods 0.000 title claims abstract description 15
- 239000010405 anode material Substances 0.000 title claims abstract description 14
- HBBGRARXTFLTSG-UHFFFAOYSA-N Lithium ion Chemical class [Li+] HBBGRARXTFLTSG-UHFFFAOYSA-N 0.000 title claims abstract description 7
- VTYYLEPIZMXCLO-UHFFFAOYSA-L Calcium carbonate Chemical compound [Ca+2].[O-]C([O-])=O VTYYLEPIZMXCLO-UHFFFAOYSA-L 0.000 claims abstract description 52
- 239000000463 material Substances 0.000 claims abstract description 30
- 229910000019 calcium carbonate Inorganic materials 0.000 claims abstract description 23
- 238000000498 ball milling Methods 0.000 claims abstract description 18
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 17
- 150000001868 cobalt Chemical class 0.000 claims abstract description 13
- 238000005406 washing Methods 0.000 claims abstract description 12
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims abstract description 11
- 229910001416 lithium ion Inorganic materials 0.000 claims abstract description 11
- 229910003002 lithium salt Inorganic materials 0.000 claims abstract description 11
- 159000000002 lithium salts Chemical class 0.000 claims abstract description 11
- 238000012986 modification Methods 0.000 claims abstract description 6
- 230000004048 modification Effects 0.000 claims abstract description 6
- 239000011248 coating agent Substances 0.000 claims abstract description 5
- 238000000576 coating method Methods 0.000 claims abstract description 5
- 229910017052 cobalt Inorganic materials 0.000 claims description 38
- 239000010941 cobalt Substances 0.000 claims description 38
- GUTLYIVDDKVIGB-UHFFFAOYSA-N cobalt atom Chemical compound [Co] GUTLYIVDDKVIGB-UHFFFAOYSA-N 0.000 claims description 38
- 239000002253 acid Substances 0.000 claims description 34
- 238000010304 firing Methods 0.000 claims description 12
- 229940088417 precipitated calcium carbonate Drugs 0.000 claims description 6
- 238000010298 pulverizing process Methods 0.000 claims description 6
- 239000007787 solid Substances 0.000 claims description 6
- BRPQOXSCLDDYGP-UHFFFAOYSA-N calcium oxide Chemical compound [O-2].[Ca+2] BRPQOXSCLDDYGP-UHFFFAOYSA-N 0.000 claims description 4
- 239000000292 calcium oxide Substances 0.000 claims description 4
- ODINCKMPIJJUCX-UHFFFAOYSA-N calcium oxide Inorganic materials [Ca]=O ODINCKMPIJJUCX-UHFFFAOYSA-N 0.000 claims description 4
- 239000006185 dispersion Substances 0.000 claims description 3
- 238000013467 fragmentation Methods 0.000 claims description 3
- 238000006062 fragmentation reaction Methods 0.000 claims description 3
- 238000002360 preparation method Methods 0.000 claims description 3
- 239000012535 impurity Substances 0.000 claims description 2
- 238000005303 weighing Methods 0.000 claims description 2
- 239000011164 primary particle Substances 0.000 abstract description 3
- 238000004519 manufacturing process Methods 0.000 abstract description 2
- 238000000227 grinding Methods 0.000 abstract 1
- 238000001291 vacuum drying Methods 0.000 abstract 1
- UBEWDCMIDFGDOO-UHFFFAOYSA-N cobalt(2+);cobalt(3+);oxygen(2-) Chemical group [O-2].[O-2].[O-2].[O-2].[Co+2].[Co+3].[Co+3] UBEWDCMIDFGDOO-UHFFFAOYSA-N 0.000 description 14
- 239000008367 deionised water Substances 0.000 description 9
- 229910021641 deionized water Inorganic materials 0.000 description 9
- XGZVUEUWXADBQD-UHFFFAOYSA-L lithium carbonate Chemical compound [Li+].[Li+].[O-]C([O-])=O XGZVUEUWXADBQD-UHFFFAOYSA-L 0.000 description 7
- 229910052808 lithium carbonate Inorganic materials 0.000 description 7
- 238000007599 discharging Methods 0.000 description 4
- 238000009826 distribution Methods 0.000 description 4
- 238000001035 drying Methods 0.000 description 4
- 239000002245 particle Substances 0.000 description 4
- 229910013870 LiPF 6 Inorganic materials 0.000 description 3
- OKKJLVBELUTLKV-UHFFFAOYSA-N Methanol Chemical compound OC OKKJLVBELUTLKV-UHFFFAOYSA-N 0.000 description 3
- 239000003792 electrolyte Substances 0.000 description 3
- WMFOQBRAJBCJND-UHFFFAOYSA-M Lithium hydroxide Chemical compound [Li+].[OH-] WMFOQBRAJBCJND-UHFFFAOYSA-M 0.000 description 2
- 238000010521 absorption reaction Methods 0.000 description 2
- 238000004458 analytical method Methods 0.000 description 2
- 238000005516 engineering process Methods 0.000 description 2
- 238000003701 mechanical milling Methods 0.000 description 2
- 238000002156 mixing Methods 0.000 description 2
- 239000000126 substance Substances 0.000 description 2
- FUJCRWPEOMXPAD-UHFFFAOYSA-N Li2O Inorganic materials [Li+].[Li+].[O-2] FUJCRWPEOMXPAD-UHFFFAOYSA-N 0.000 description 1
- 239000011149 active material Substances 0.000 description 1
- 239000011247 coating layer Substances 0.000 description 1
- 230000000052 comparative effect Effects 0.000 description 1
- 238000010586 diagram Methods 0.000 description 1
- XUCJHNOBJLKZNU-UHFFFAOYSA-M dilithium;hydroxide Chemical compound [Li+].[Li+].[OH-] XUCJHNOBJLKZNU-UHFFFAOYSA-M 0.000 description 1
- 230000007613 environmental effect Effects 0.000 description 1
- 238000009776 industrial production Methods 0.000 description 1
- 239000003595 mist Substances 0.000 description 1
- 239000000203 mixture Substances 0.000 description 1
- 239000003960 organic solvent Substances 0.000 description 1
- 230000021962 pH elevation Effects 0.000 description 1
- 230000000704 physical effect Effects 0.000 description 1
- 239000000843 powder Substances 0.000 description 1
- 239000011435 rock Substances 0.000 description 1
- 239000010865 sewage Substances 0.000 description 1
Images
Classifications
-
- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
- Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
- Y02E—REDUCTION OF GREENHOUSE GAS [GHG] EMISSIONS, RELATED TO ENERGY GENERATION, TRANSMISSION OR DISTRIBUTION
- Y02E60/00—Enabling technologies; Technologies with a potential or indirect contribution to GHG emissions mitigation
- Y02E60/10—Energy storage using batteries
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- Battery Electrode And Active Subsutance (AREA)
Abstract
The invention relates a surface modified lithium ion battery anode material lithium cobaltate and a modifying method thereof; the material is lithium ion battery anode material lithium cobaltate coated with a layer of calcium carbonate. The method comprises the following steps: weighting lithium salt and cobalt salt; adding lithium salt in a ball mill, then adding coating material calcium carbonate, then adding cobalt salt, finally adding industrial alcohol to perform ball milling; after ball milling, performing vacuum drying to the obtained material, then performing first kilning; grinding the obtained material, washing with impurity-removing water, performing second kilning; and obtaining the product by dispersing treatment, wherein, when weighting lithium salt and cobalt salt, the molar ratio of Li to Co is 1.038. After the modification, the granularity of lithium cobaltate primary particles is improved, the specific area of lithium cobaltate can be reduced, the production cost is reduced, the water absorptivity of lithium cobaltate is improved and the processability of the obtained product is good.
Description
Background technology
The present invention relates to a kind of lithium ion cell anode material lithium cobaltate and method of modifying thereof of surface modification.
Technical field
Cobalt acid lithium has the specific capacity height as anode material for lithium-ion batteries, and stable performance and preparation technology simply have been widely used in the active material of anode material for lithium-ion batteries.Because the aerial water absorption of cobalt acid lithium is more intense, alkalization has especially easily suppressed the flowability of cobalt acid lithium when the organic solvent mixing is sized mixing.How improving cobalt acid lithium processing characteristics effectively, reduce the problems such as specific area of material, is the technical problem of the required solution of those skilled in the art.
Summary of the invention
Purpose of the present invention aims to provide a kind of surface modification lithium ion cell anode material lithium cobaltate and method of modifying, has improved the granularity of cobalt acid lithium primary particle, can reduce the specific area of cobalt acid lithium, has reduced production cost.Improved the water absorbing properties of cobalt acid lithium, the products obtained therefrom good processability.
Material of the present invention is to coat one deck calcium carbonate on the lithium ion cell anode material lithium cobaltate surface.
A kind of surface modifying method of lithium ion cell anode material lithium cobaltate may further comprise the steps, and is 1.038 to take by weighing lithium salts and cobalt salt respectively by the molal weight ratio of LI: Co; In ball mill, add lithium salts earlier, add coating material calcium carbonate again, add cobalt salt then, add industrial alcohol at last, carry out ball milling; Material behind the ball milling then burns till after vacuumize first; Material after burning till spends the water impurity washing, twice firing after fragmentation, pulverizing; Dispersion treatment promptly.
The present invention mixes calcium carbonate in mechanical milling process, make cobalt acid lithium surface coat one deck calcium carbonate, can improve the chemical property of cobalt acid lithium effectively.
The calcium carbonate that the present invention adopts is precipitated calcium carbonate.
Described precipitated calcium carbonate average grain diameter 40～200nm, whiteness 〉=90%, specific area 27～31m
2/ g, CaCO
3, 〉=97%.
In the calcium carbonate in contained calcium oxide and the cobalt salt contained cobalt mass ratio be 0.0062～0.0065.
The ball milling time is preferably 90 ± 5 minutes.
The preferred liquid-solid volume ratio of alcohol and cobalt salt, lithium salts and calcium carbonate is 5～10: 1.
Described burning till is to carry out in full-automatic ejection plate kiln, and heat-treating atmosphere is an air.
The preferred firing mode of the present invention is:
Burning till first is to carry out in the full-automatic pushed bat kiln of 20M, burns till first to be divided into 11 warm areas, and preparation cobalt acid lithium master warm area is the 6-10 warm area, main warm area temperature 1030 degree, push pedal speed 10mm/min.
Twice firing is to carry out in the full-automatic pushed bat kiln of 20M, and the twice firing temperature is 300 degree, push pedal speed 40mm/min.
The vacuumize time is 45～70 minutes, vacuum degree " 0.065Mpa.
The dispersion treatment time is high speed 5min, low speed 10min.
Used lithium salts is a lithium carbonate, and cobalt salt is a cobaltosic oxide; The water-washing process water is a deionized water.Wherein cobaltosic oxide and lithium carbonate are LITHIUM BATTERY.
Cobalt acid lithium of the present invention surface coats one deck calcium carbonate material, and its advantage is:
(1) can regulate the size of cobalt acid lithium primary particle, reduce the specific area of cobalt acid powder for lithium material.Increased the specific capacity of cobalt acid lithium.
(2) Biao Mian lithium carbonate coating layer has effectively improved the water absorption of cobalt acid lithium, has reduced the content of LiOH in the cobalt acid lithium.Improved the processing characteristics of cobalt acid lithium.
(3), reduced in the water-washing process alkalinization of contained Li2O in the cobalt acid lithium greatly because cobalt acid lithium has coated one deck calcium carbonate particle.
The concrete execution mode of the present invention is:
1. prepare burden.The Co that the present invention uses Jinchuan to provide
3O
4, the Li that the Shehong, Sichuan is provided
2CO
3LI: Co=1.038 (molal weight ratio).
2. ball milling drying.In vertical ball mill, add Li earlier
2CO
3, add coating CaCO again
3, add Co then
3O
4Add alcohol (52% methyl alcohol+48% ethanol) at last, carry out ball milling.Material behind the ball milling directly utilizes vacuum pump to be extracted into vacuum drier to carry out drying.Wherein said ball mill is the QMJ200 vertical ball mill of Shanghai China rock instrument and equipment Co., Ltd.CaCO
3In contained calcium oxide and Co
3O
4In contained cobalt mass ratio be that 0.0064. mixture ball milling material is 150 minutes.Liquid-solid volume ratio is 5～10: 1 (alcohol and cobalt salt, lithium salts, calcium carbonate volume ratio)
The vacuumize time is 45～70 minutes, vacuum degree " 0.065Mpa
3. dried material is placed to drop in the full-automatic ejection plate kiln in 24 hours and is burnt till.Heat-treating atmosphere is an air.Push pedal speed 10mm/min.Use burning kiln to be the full-automatic pushed bat kiln of 20M.Be divided into 11 temperature.The made cobalt acid of the present invention lithium master warm area is the 6-10 warm area.Main warm area temperature 1030 degree.
4. the material after burning till carries out fragmentation, pulverizes classification.With the deionized water washing, twice firing is handled.Can obtain cobalt acid lithium of the present invention.Pulverization conditions: charging frequency 3HZ, grading wheel frequency 14HZ, pulverizer pressure 0.18Mpa.Pulverizer intensity: 5 grades (totally 9 grades).
Cobalt acid lithium mass ratio after deionized water and the pulverizing is 5: 1.
The twice firing temperature is 300 degree, 6 hours processing times.Material behind the twice firing disperses in mixer.Mixer frequency 1400HZ, jitter time high speed 5min, low speed 10min.
In sum, modification cobalt acid lithium material of the present invention has particle size distribution all to be had, and specific area is little, and processing characteristics is good, the specific capacity height of cobalt acid lithium; The jolt ramming height, the characteristic that chemical property is good.
Method of the present invention also can have been saved the consumption of washing process deionized water, in industrial production, the cobalt acid lithium that does not carry out the calcium carbonate coating is in water-washing process, the consumption of deionized water very big (volume ratio of cobalt acid lithium and deionized water is 1: 20～50). method of the present invention is because cobalt acid lithium surface has coated one deck calcium carbonate, the deionized water consumption significantly reduces (volume ratio of cobalt acid lithium and deionized water is 1: 5～10) in the water-washing process, reduce sewage emissions, showed the environmental requirement that new material utilizes.Method of the present invention is simple to operate, is suitable for the extensive use of anode material of lithium battery industry.
Description of drawings
Fig. 1 is a sample A particle size distribution figure;
Fig. 2 is a sample B particle size distribution figure;
Fig. 3 is sample B charging and discharging curve figure (first);
Positive electrode No:test-C
Negative material title: Li Metal
Electrolyte is formed: EC: DMC: LiPF
6=1: 1: 1
Discharge and recharge scope: 3.0～4.3V
Charging current: 0.1C
Discharging current: 0.1C
Fig. 4 is a sample B discharge curve;
(0.1,0.2,0.5,0.8,1.0C (the 2nd, 4,6,8,10cyc))
Positive electrode No:test-C
Negative material title: LiMetal
Electrolyte is formed: EC: DMC: LiPF
6=1: 1: 1
Discharge and recharge scope: 3.0～4.3V
Charging current: 0.1C, 0.2C, 0.5C, 0.8C, 1.0C
Discharging current: 0.1C, 0.2C, 0.5C, 0.8C, 1.0C
Fig. 5 is a sample B cycle graph;
Positive electrode No:test-C
Negative material title: LiMetal
Electrolyte is formed: EC: DMC: LiPF
6=1: 1: 1
Discharge and recharge scope: 3.0～4.3V
Charging current: 1.0C
Discharging current: 1.0C
Embodiment
Following execution mode is intended to illustrate the present invention rather than limitation of the invention further.
Comparative Examples 1.
With lithium carbonate, cobaltosic oxide is that 1.038 calculating are weighed according to molal weight.In ball mill, add lithium carbonate earlier, add cobaltosic oxide again.According to liquid-solid ratio is 5: 1 adding alcohol.Carry out ball milling.90 minutes ball milling time.Drying material in vacuum behind the ball milling 60 minutes.Burn till according to claim, the broken pulverizing, washing, twice firing disperses.The gained sample send the physics complete analysis.(sample A)
With lithium carbonate, cobaltosic oxide is that 1.038 calculating are weighed according to molal weight.In ball mill, add lithium carbonate earlier, add calcium carbonate (mass ratio that wherein contains cobalt in the calcium carbonate in contained calcium oxide and the cobaltosic oxide is 0.0064) then.Add cobaltosic oxide again.According to liquid-solid ratio is 5: 1 adding alcohol.Carry out ball milling.90 minutes ball milling time.Drying material in vacuum behind the ball milling 60 minutes.Burn till according to claim, the broken pulverizing, washing, twice firing disperses.The gained sample send the physics complete analysis.(sample B)
According to the result of embodiment 1,2, having carried out finished product cobalt acid lithium that calcium carbonate coats operation in the mechanical milling process, to compare the Granularity Distribution that does not coat more concentrated, do not have micro mist.The jolt ramming height, specific area is little, and processing characteristics is good.
Sample AB physical property comparison diagram
| Sample | ??D10 | ?D50 | ?D90 | ??tep??density | ??SBET | Water-washing process deionized water consumption (liquid-solid ratio) |
| Sample A | ??6.02 | ?12.13 | ?23.51 | ??2.88 | ??0.323 | ??0.049 |
| Sample B | ??7.16 | ?14.06 | ?24.82 | ??2.95 | ??0.289 | ??0.047 |
Claims (10)
1, a kind of lithium ion battery anode material lithium cobaltate of surface modification is characterized in that, the lithium ion cell anode material lithium cobaltate surface coats one deck calcium carbonate.
2, according to the described cobalt acid lithium material of claim 1, it is characterized in that the calcium carbonate of employing is precipitated calcium carbonate.
3, according to the described cobalt acid lithium material of claim 2, it is characterized in that precipitated calcium carbonate average grain diameter 40～200nm, whiteness 〉=90%, specific area 27～31m
2/ g, CaCO
3, 〉=97%.
4, a kind of surface modifying method of lithium ion cell anode material lithium cobaltate is characterized in that, may further comprise the steps, and be 1.038 to take by weighing lithium salts and cobalt salt respectively by the molal weight ratio of LI:Co; In ball mill, add lithium salts earlier, add coating material calcium carbonate again, add cobalt salt then, add industrial alcohol at last, carry out ball milling; Material behind the ball milling then burns till after vacuumize first; Material after burning till spends the water impurity washing, twice firing after fragmentation, pulverizing; Dispersion treatment promptly.
5, surface modifying method according to claim 2 is characterized in that: in the calcium carbonate in contained calcium oxide and the cobalt salt contained cobalt mass ratio be 0.0062～0.0065.
6, according to the described cobalt acid lithium material of claim 4 or 5, it is characterized in that the calcium carbonate of employing is precipitated calcium carbonate.
7, according to the described cobalt acid lithium material of claim 6, it is characterized in that precipitated calcium carbonate average grain diameter 40～200nm, whiteness 〉=90%, specific area 27～31m
2/ g, CaCO
3, 〉=97%.
8, surface modifying method according to claim 4 is characterized in that: the ball milling time is 90 ± 5 minutes.
9, surface modifying method according to claim 4 is characterized in that: the liquid-solid volume ratio of alcohol and cobalt salt, lithium salts and calcium carbonate is 5～10: 1.
10, surface modifying method according to claim 4, it is characterized in that: burning till first is to carry out in the full-automatic pushed bat kiln of 20M, burn till first and be divided into 11 temperature, preparation cobalt acid lithium master warm area is the 6-10 warm area, main warm area temperature 1030 degree, push pedal speed 10mm/min, heat-treating atmosphere are air; Twice firing is to carry out in the full-automatic pushed bat kiln of 20M, and the twice firing temperature is 300 degree, and push pedal speed 40mm/min, heat-treating atmosphere are air.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN200910044154A CN101630727A (en) | 2009-08-18 | 2009-08-18 | Surface modified lithium ion battery anode material lithium cobaltate and modifying method thereof |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN200910044154A CN101630727A (en) | 2009-08-18 | 2009-08-18 | Surface modified lithium ion battery anode material lithium cobaltate and modifying method thereof |
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| Publication Number | Publication Date |
|---|---|
| CN101630727A true CN101630727A (en) | 2010-01-20 |
Family
ID=41575746
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| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN200910044154A Pending CN101630727A (en) | 2009-08-18 | 2009-08-18 | Surface modified lithium ion battery anode material lithium cobaltate and modifying method thereof |
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|---|---|
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Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102214818A (en) * | 2010-04-09 | 2011-10-12 | 索尼公司 | Battery |
| CN105406040A (en) * | 2015-11-03 | 2016-03-16 | 湖南长远锂科有限公司 | Coated and modified high-nickel ternary cathode material and preparation method thereof |
| CN106169578A (en) * | 2016-08-23 | 2016-11-30 | 金川集团股份有限公司 | A kind of preparation method of big granularity lithium cobaltate cathode material |
-
2009
- 2009-08-18 CN CN200910044154A patent/CN101630727A/en active Pending
Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102214818A (en) * | 2010-04-09 | 2011-10-12 | 索尼公司 | Battery |
| CN105406040A (en) * | 2015-11-03 | 2016-03-16 | 湖南长远锂科有限公司 | Coated and modified high-nickel ternary cathode material and preparation method thereof |
| CN105406040B (en) * | 2015-11-03 | 2019-01-11 | 湖南长远锂科有限公司 | Nickelic tertiary cathode material of coating modification and preparation method thereof |
| CN106169578A (en) * | 2016-08-23 | 2016-11-30 | 金川集团股份有限公司 | A kind of preparation method of big granularity lithium cobaltate cathode material |
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Open date: 20100120 |