CN103000874A - Preparation method of carbon-coated ternary positive electrode material - Google Patents
Preparation method of carbon-coated ternary positive electrode material Download PDFInfo
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- CN103000874A CN103000874A CN2012104400593A CN201210440059A CN103000874A CN 103000874 A CN103000874 A CN 103000874A CN 2012104400593 A CN2012104400593 A CN 2012104400593A CN 201210440059 A CN201210440059 A CN 201210440059A CN 103000874 A CN103000874 A CN 103000874A
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- Y02E—REDUCTION OF GREENHOUSE GAS [GHG] EMISSIONS, RELATED TO ENERGY GENERATION, TRANSMISSION OR DISTRIBUTION
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Abstract
The invention relates to the preparation of a ternary positive electrode material of a lithium ion battery, and particularly relates to a preparation method of a carbon-coated ternary positive electrode material. The method is characterized by comprising the following steps of: (1) adding a ternary positive electrode material LiNixCoyMnzO2 into deionized water or an organic solvent to obtain a mixed solution; (2) adding an organic carbon source with the weight accounting for 10% to 30% of the weight of the ternary positive electrode material into the mixed solution, and adding a carbonization catalyst with the weight accounting for 0.5% to 5% of the weight of the organic carbon source to obtain another mixed solution; (3) spray-granulating the mixed solution by using a spray dryer to obtain lithium manganate coated with organic carbon; and (4) heating lithium manganate powder to be at the temperature being 300 to 450 DEG C, sintering for 0.5 to 4 hours, and cooling to obtain a final product. The preparation method provided by the invention can prevent the damage to a crystal form of the ternary positive electrode material by high-temperature carbonization, and can effectively improve the electrode conductivity, improve the surface of an active material and protect the electrode from direct contact with electrolyte, so that the cycle life is prolonged.
Description
Technical field
The present invention relates to the preparation of ternary cathode material of lithium ion battery, especially a kind of carbon coats the preparation method of tertiary cathode material.
Background technology
In lithium ion battery, positive electrode is its most important part, also is the key that determines performance of lithium ion battery.At present the industrialization anode material for lithium-ion batteries be LiCoO2, research and comparison is ripe, high comprehensive performance, but expensive, toxicity is larger, and there is defective in security performance, is especially overcharging under the condition, material is unstable, and easy and electrolyte reacts, and application is a greater impact; In addition LiCoO
2Only have half lithium reversible embedding to take off, actual reversible capacity is about 145mAh/g, and the limiting lithium ion cell capacity improves, and can not satisfy the needs of the electrical source of power battery such as electric vehicle power sources, therefore needs to seek the new material of high-performance and low-cost.
In cobalt acid lithium substitution material, tertiary cathode material nickel, cobalt and manganese oxide system has the advantages such as cost is low, specific capacity is high, voltage platform is high, anti-excessively punching performance is good, good heat stability, and receives much concern.Studies show that this positive electrode concentrated the separately advantage of the materials such as LiCoO2, LiMn2O4 and LiNiO2.Therefore no matter tertiary cathode material is the communication product lithium ion battery, or electrokinetic cell, and great development space and potentiality are arranged
Along with the understanding of people to lithium ion battery electrode material, it is found that its surface texture has very large impact to its chemical property.Because the physical attribute of the conductivity of material with carbon element brilliance, the chemistry of superelevation and electrochemical stability, uniqueness and cheap cost, carbon coats becomes one of most widely used method in the lithium ion battery.Coat surface chemistry, the guard electrode effectively to improve electrode conductivuty, improve active material with carbon and avoid its directly contact electrolyte, thereby can obtain better cycle life.Carbon coats and to combine with nanometer technology, better conductivity, lithium ion diffusion velocity faster can be provided, thereby obtain better high rate performance.Especially carbon-coated LiFePO 4 for lithium ion batteries has promoted LiFePO4 to move towards the industrialization from the laboratory, and therefore, the research tool that the carbon of positive electrode is coated is of great significance.
Because the LiNixCoyMnzO2 synthesis condition is under air or oxygen atmosphere, synthesis temperature is up to 900 ℃.So the method that traditional realization carbon that passes through the organic carbon decomposition coats is difficult to realize at tertiary cathode material: at first the carbon coating must be at inert atmosphere, with the synthetic oxygen atmosphere contradiction that needs of tertiary cathode material, secondly, realize that carbon decomposes and graphitization temperature up to 700 ℃~900 ℃, be easy to the metal ions such as nickel, cobalt, manganese are reduced into simple substance.Therefore, present carbon coats the technique of only taking dry blend or the mixed oar of carbonaceous conductive agent.
For the problems referred to above, coat experience according to carbon abundant in the LiFePO4 preparation process, the invention pass through to select reasonable carbon source, the carbonization catalyst is realized the carbon coating of low temperature ternary positive electrode under protective atmosphere.After coating, improved in tertiary cathode material carbon the electronic conductivity of electrode material, strengthened the transmission speed of ion at electrode surface, two kinds of synergies are so that contain the electrode material of a small amount of carbon and can discharge and recharge fully, and coulombic efficiency is higher, reduces the polarization of electrode surface in the cyclic process.
Summary of the invention
The purpose of this invention is to provide the preparation method that a kind of carbon coats tertiary cathode material, can the Effective Raise electrode conductivuty and obtain better cycle life.
A kind of carbon coats the preparation method of tertiary cathode material, and its special feature is, comprises the steps:
(1) with tertiary cathode material LiNi
xCo
yMn
zO
2, wherein 0.3≤x≤1,0≤y≤0.5,0≤z≤0.5 and X+Y+Z=1 join in deionized water or the organic solvent, wherein LiNi
xCo
yMn
zO
2With the weight ratio of deionized water or organic solvent be 1:1~3, evenly mix;
(2) add the organic carbon source that accounts for tertiary cathode material weight 10%~30% in the gained mixed liquor, stir, evenly mix, and then add and occupy machine carbon source weight 0.5%~5% carbided catalyst, be stirred to emulsified state with mulser, evenly mix;
(3) the gained mixed liquor is obtained the LiMn2O4 that organic carbon coats after by the spray dryer mist projection granulating, 180~250 ℃ of spray drying inlet temperatures, outlet temperature are 60~90 ℃;
(4) gained LiMn2O4 powder is packed in the crucible, vacuumize, pass into inert atmosphere, keep being heated to 300 ℃~450 ℃ sintering 0.5h~4h under the inert atmosphere conditions, then cooling gets final product.
At least a during to be that sucrose, glucose, polyethylene glycol, resorcinol and ring are smart stick with paste of organic carbon source in the step (2).
Carbided catalyst is one or more in ferrocene, dicyclopentadienyl nickel, cobaltocene, two luxuriant manganese, two luxuriant lithiums, nickel acetate, cobalt acetate and the manganese acetate in the step (2).
Organic solvent is one or more in ethanol, methyl alcohol, acetone or the n-formyl sarcolysine base pyrrolidones in the step (2).
Sintering carries out in electric furnace or microwave agglomerating furnace in the step (4).
Inert atmosphere is one or more in nitrogen and the argon gas in the step (4).
Preparation method of the present invention is, select the organic carbon of low temperature pyrolysis, add suitable carbided catalyst, tertiary cathode material is by the mist projection granulating mode, at tertiary cathode material coated with uniform one deck organic carbon, then under inert atmosphere, 350 ℃~500 ℃ of low temperature are under the effect of catalyst, organic carbon is cracked into DIC, is coated on the tertiary cathode material surface.Avoid the destruction of high temperature cabonization with the tertiary cathode material crystal formation, caused simultaneously the separating out of reduction of metal.Surface chemistry, the guard electrode of effectively improve electrode conductivuty, improving active material avoided its directly contact electrolyte, thereby can obtain better cycle life.
Description of drawings
Fig. 1 is the XRD figure of sample after tertiary cathode material carbon coats among the embodiment 1, and carbon content is respectively 1%, 3%, 5%, can find out that the degree of crystallinity of sample is high, and crystalline phase is purer, does not destroy crystal formation;
Fig. 2 is the perspective SEM comparison diagram of synthetic sample among the embodiment 1, for not coating the tertiary cathode material of carbon-coating;
Fig. 3 is the perspective SEM comparison diagram of synthetic sample among the embodiment 1, for carbon-coating and the positive electrode after coating, can see obvious carbon film.
Embodiment
Preparation method of the present invention is by suitable organic carbon; add carbided catalyst; coat the even organic substance of one deck by mist projection granulating on the tertiary cathode material surface; 350 ℃~500 ℃ sintering 0.5h~4h obtain the tertiary cathode material that even carbon coats under protective atmosphere; pass through XRD; XPS detects, and material keeps good layer structure, and carbon content is between 2%~10%.After coating, improved in tertiary cathode material carbon the electronic conductivity of electrode material, strengthened the transmission speed of ion at electrode surface, two kinds of synergies are so that tertiary cathode material can discharge and recharge fully, and coulombic efficiency is higher, reduces the polarization of electrode surface in the cyclic process.Novelty has solved 700 ℃~900 ℃ pyrocarbon coatings and has caused easily metallic reducing, and the low temperature carbon source is difficult to the contradiction of carbonization.
The pyrocarbon coating causes metallic reducing easily in the background technology in order to solve, and the low temperature carbon source is difficult to the problem of carbonization, the invention provides a kind of new method of coated modified carbon tertiary cathode material.By evenly being mixed in solution, organic carbon source, catalyst and tertiary cathode material disperse, then carrying out carbon with the method for mist projection granulating coats, at 350 ℃~500 ℃ sintering 0.5h~4h of inert atmosphere, organic carbon is cracked into DIC, be coated on the tertiary cathode material surface, weight ratio is 1%~10%.
Below in conjunction with embodiment the present invention is done to describe in further detail, following embodiment only is used for explanation the present invention, but the practical range that is not intended to limit the present invention.
Embodiment 1:
1) with LiNi
1/3Co
1/3Mn
1/3O
2Take by weighing 100g and join in the 200ml deionized water, magnetic agitation is evenly mixed.
2) add in the gained mixed liquor and account for LiNi
1/3Co
1/3Mn
1/3O
2The polyvinyl alcohol 15g of tertiary cathode material weight 15%, magnetic agitation is evenly mixed.
3) in the gained mixed liquor, add the ferrocene 0.15g that accounts for polyvinyl alcohol weight 1%, be stirred to emulsified state with mulser, mix.
4) the gained mixed liquor is obtained organic carbon after by the spray dryer mist projection granulating and evenly coat the tertiary cathode material powder.The spray drying parameter is set to, and 250 ℃ of inlet temperatures, outlet temperature are 90 ℃.
5) the gained powder is packed in the crucible, place electric tube furnace, vacuumize, logical nitrogen will vacuumize, logical nitrogen process repeats 3 times, and 400 ℃ of heating 2h namely obtain the tertiary cathode material that carbon coats.
The sample of the present invention by above-described embodiment 1 to such as shown in Fig. 2,3, Fig. 2 is tertiary cathode material, Fig. 3 is the tertiary cathode material that carbon coats.
Embodiment 2:
1) with LiNi
0.5Co
0.2Mn
0.3O
2Take by weighing 150g and join in the 450g absolute ethyl alcohol, magnetic agitation is evenly mixed.
2) add in the gained mixed liquor and account for LiNi
0.5Co
0.2Mn
0.3O
2The sucrose 15g of tertiary cathode material weight 10% stirs, and evenly mixes.
3) add that to account for sucrose weight ratio be 3% cobaltocene 0.45g in the gained mixed liquor, magnetic agitation is stirred to emulsified state with mulser, mixes.
4) the gained mixed liquor is obtained organic carbon after by the spray dryer mist projection granulating and evenly coat the tertiary cathode material powder.The spray drying parameter is set to, and 180 ℃ of inlet temperatures, outlet temperature are 60 ℃, and induced draft fan speed is set to 70%.
5) during the gained powder is packed crucible into, place electric tube furnace, vacuumize, logical nitrogen will vacuumize, lead to the nitrogen process and repeat 3 times, and 500 ℃ of heating 4h namely obtain the tertiary cathode material that carbon coats.
Embodiment 3:
1) with LiNi
0.4Co
0.4Mn
0.2O
2Take by weighing 200g and join in the 300g n-formyl sarcolysine base pyrrolidones, stir, evenly mix.
2) add in the gained mixed liquor and account for LiNi
0.4Co
0.4Mn
0.2O
2The glucose 60g of tertiary cathode material weight 30%, magnetic agitation is evenly mixed.
3) add that to account for the glucose weight ratio be 3% nickel acetate 1.8g in the gained mixed liquor, magnetic agitation is stirred to emulsified state with mulser, mixes.
4) the gained mixed liquor is obtained organic carbon after by the spray dryer mist projection granulating and evenly coat the tertiary cathode material powder.The spray drying parameter is set to, and 220 ℃ of inlet temperatures, outlet temperature are 80 ℃, and induced draft fan speed is set to 60%.
5) during the gained powder is packed crucible into, place microwave oven, vacuumize, logical nitrogen will vacuumize, lead to the nitrogen process and repeat 3 times, and 350 ℃ of heating 0.5h namely obtain the tertiary cathode material that carbon coats.
Embodiment 4:
1) with LiNi
0.6Co
0.3Mn
0.1O
2Take by weighing 100g and join in the 200ml acetone, stir, evenly mix.
2) add in the gained mixed liquor and account for LiNi
0.6Co
0.3Mn
0.1O
2The resorcinol 10g of tertiary cathode material weight 10% stirs, and evenly mixes.
3) add that to account for the resorcinol weight ratio be 0.5% manganese acetate 0.05g in the gained mixed liquor, be stirred to emulsified state with mulser, mix.
4) the gained mixed liquor is obtained organic carbon after by the spray dryer mist projection granulating and evenly coat the tertiary cathode material powder.The spray drying parameter is set to, and 200 ℃ of inlet temperatures, outlet temperature are 70 ℃.
5) during the gained powder is packed crucible into, in the electric tube furnace, vacuumize, logical nitrogen will vacuumize, lead to the nitrogen process and repeat 3 times, and 450 ℃ of heating 4h namely obtain the tertiary cathode material that carbon coats.
Claims (6)
1. the preparation method of a carbon coating tertiary cathode material is characterized in that, comprises the steps:
(1) with tertiary cathode material LiNi
xCo
yMn
zO
2, wherein 0.3≤x≤1,0≤y≤0.5,0≤z≤0.5 and X+Y+Z=1 join in deionized water or the organic solvent, wherein LiNi
xCo
yMn
zO
2With the weight ratio of deionized water or organic solvent be 1:1~3, evenly mix;
(2) add the organic carbon source that accounts for tertiary cathode material weight 10%~30% in the gained mixed liquor, stir, evenly mix, and then add and occupy machine carbon source weight 0.5%~5% carbided catalyst, be stirred to emulsified state with mulser, evenly mix;
(3) the gained mixed liquor is obtained the LiMn2O4 that organic carbon coats after by the spray dryer mist projection granulating, 180~250 ℃ of spray drying inlet temperatures, outlet temperature are 60~90 ℃;
(4) gained LiMn2O4 powder is packed in the crucible, vacuumize, pass into inert atmosphere, keep being heated to 300 ℃~450 ℃ sintering 0.5h~4h under the inert atmosphere conditions, then cooling gets final product.
2. a kind of carbon as claimed in claim 1 coats the preparation method of tertiary cathode material, it is characterized in that: at least a during to be that sucrose, glucose, polyethylene glycol, resorcinol and ring are smart stick with paste of organic carbon source in the step (2).
3. a kind of carbon as claimed in claim 1 coats the preparation method of tertiary cathode material, it is characterized in that: carbided catalyst is one or more in ferrocene, dicyclopentadienyl nickel, cobaltocene, two luxuriant manganese, two luxuriant lithiums, nickel acetate, cobalt acetate and the manganese acetate in the step (2).
4. a kind of carbon as claimed in claim 1 coats the preparation method of tertiary cathode material, it is characterized in that: organic solvent is one or more in ethanol, methyl alcohol, acetone or the n-formyl sarcolysine base pyrrolidones in the step (2).
5. a kind of carbon as claimed in claim 1 coats the preparation method of tertiary cathode material, it is characterized in that: sintering carries out in electric furnace or microwave agglomerating furnace in the step (4).
6. a kind of carbon as claimed in claim 1 coats the preparation method of tertiary cathode material, it is characterized in that: inert atmosphere is one or more in nitrogen and the argon gas in the step (4).
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Cited By (8)
Publication number | Priority date | Publication date | Assignee | Title |
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CN104900869A (en) * | 2015-04-30 | 2015-09-09 | 浙江天能能源科技有限公司 | Preparation method of carbon-coated nickel-cobalt-aluminum ternary positive electrode material |
WO2016058491A1 (en) * | 2014-10-14 | 2016-04-21 | 江苏华东锂电技术研究院有限公司 | Method for carbon-coating lithium-ion battery electrode active material |
CN106025208A (en) * | 2016-06-04 | 2016-10-12 | 苏州思创源博电子科技有限公司 | Preparation method for carbon-coated ternary positive electrode material |
CN106025207A (en) * | 2016-06-04 | 2016-10-12 | 苏州思创源博电子科技有限公司 | Preparation method for carbon-coated manganese-based positive electrode material |
CN106684346A (en) * | 2016-12-13 | 2017-05-17 | 苏州宇量电池有限公司 | Carbon coating method suitable for preparing electrode material by spray drying method |
CN109860534A (en) * | 2018-12-18 | 2019-06-07 | 中科廊坊过程工程研究院 | A kind of tertiary cathode material and preparation method thereof of carbon quantum dot modification |
CN110429275A (en) * | 2019-08-26 | 2019-11-08 | 银隆新能源股份有限公司 | The preparation method and carbon coating tertiary cathode material of carbon coating tertiary cathode material |
CN111653735A (en) * | 2020-02-24 | 2020-09-11 | 深圳市翔丰华科技股份有限公司 | Low-temperature carbon-coated porous silicon composite negative electrode material and preparation method thereof |
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Cited By (9)
Publication number | Priority date | Publication date | Assignee | Title |
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WO2016058491A1 (en) * | 2014-10-14 | 2016-04-21 | 江苏华东锂电技术研究院有限公司 | Method for carbon-coating lithium-ion battery electrode active material |
CN104900869A (en) * | 2015-04-30 | 2015-09-09 | 浙江天能能源科技有限公司 | Preparation method of carbon-coated nickel-cobalt-aluminum ternary positive electrode material |
CN106025208A (en) * | 2016-06-04 | 2016-10-12 | 苏州思创源博电子科技有限公司 | Preparation method for carbon-coated ternary positive electrode material |
CN106025207A (en) * | 2016-06-04 | 2016-10-12 | 苏州思创源博电子科技有限公司 | Preparation method for carbon-coated manganese-based positive electrode material |
CN106684346A (en) * | 2016-12-13 | 2017-05-17 | 苏州宇量电池有限公司 | Carbon coating method suitable for preparing electrode material by spray drying method |
CN109860534A (en) * | 2018-12-18 | 2019-06-07 | 中科廊坊过程工程研究院 | A kind of tertiary cathode material and preparation method thereof of carbon quantum dot modification |
CN109860534B (en) * | 2018-12-18 | 2022-04-15 | 廊坊绿色工业技术服务中心 | Carbon quantum dot modified ternary cathode material and preparation method thereof |
CN110429275A (en) * | 2019-08-26 | 2019-11-08 | 银隆新能源股份有限公司 | The preparation method and carbon coating tertiary cathode material of carbon coating tertiary cathode material |
CN111653735A (en) * | 2020-02-24 | 2020-09-11 | 深圳市翔丰华科技股份有限公司 | Low-temperature carbon-coated porous silicon composite negative electrode material and preparation method thereof |
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Application publication date: 20130327 |