CN102623677A - Process for producing high capacity molybdenum dioxide/carbon cathode materials - Google Patents
Process for producing high capacity molybdenum dioxide/carbon cathode materials Download PDFInfo
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- CN102623677A CN102623677A CN2012101005075A CN201210100507A CN102623677A CN 102623677 A CN102623677 A CN 102623677A CN 2012101005075 A CN2012101005075 A CN 2012101005075A CN 201210100507 A CN201210100507 A CN 201210100507A CN 102623677 A CN102623677 A CN 102623677A
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- molybdenum dioxide
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- 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
Abstract
The invention discloses a process for producing high capacity molybdenum dioxide/carbon cathode materials. The process includes the steps of 1) immersing cotton fiber fabric of a certain size in an ethanol solution of phosphomolybdic acid and stirring; 2) drying and ageing the immersed cotton fiber fabric; and 3) subjecting the dried and aged cotton fiber fabric to heat treatment in mixed gases, and obtaining the molybdenum dioxide/the carbon (MoO2/C) composite materials. The invention further discloses cathode materials which are produced by the process, an electrode slice which is made of the cathode materials and a button cell which comprises the electrode slice. According to the molybdenum dioxide/the carbon composite materials produced by the process, the specific capacity is high, the multiplying power property and the cycling stability are good, and the coulomb efficiency is high. The process is simple and suitable for large-scale production.
Description
Technical field
The present invention relates to the lithium ion battery field, be specifically related to a kind of preparation method of high power capacity long circulation life negative material.
Background technology
Lithium ion battery is because of advantages such as energy density is high, average open-circuit voltage is high and have extended cycle life have been widely used in moving, portable electronics.Advantage is widely used in consumer electronics sector but flexible packing lithium ion battery is because of its size flexible design, security performance be good etc.But it is also increasingly high that miniaturization of electronic products, lightening development require the energy density of lithium ion battery, also increasingly high to the capacity requirement of lithium ion battery electrode material, especially negative active core-shell material.
At present, commercial lithium ion battery negative material adopts graphite material more, but its theoretical capacity 372mAh g only
-1, and the low (1.5～1.7g/cm of compacted density
3), big limitations the further lifting of lithium ion battery energy density.The embedded reactive (graphite material) of comparing; Metal oxide based negative material based on conversion reaction has high lithium ion theory of storage specific capacity; But owing to its big bulk effect, low reasons such as conductivity; Often show as cycle performance and high rate performance is poor as lithium ion battery negative material, so limited its commercial applications.Molybdenum dioxide has high theoretical specific capacity (838mAhg because of it
-1), high compacted density (6.5g cm
-3), high conductivity and by broad research.People such as L.C.Yang adopt the molybdenum dioxide negative material of the method preparation of high temperature reduction molybdenum trioxide, and the preparation process that is adopted is mainly: MoO will be equipped with in (1)
3Porcelain boat put into tube furnace; (2) mist of feeding alcohol vapour and argon gas in tube furnace is with the air emptying in the tube furnace quartz ampoule; (3) 400 ℃ of following heat treatment 12 hours in the mist of alcohol vapour that flows and argon gas finally obtains MoO
2Product.Heat treatment period is longer in the preparation process, prepared MoO
2Specific capacity is 318mAh g only
-1, less than MoO
2Half of theoretical specific capacity, and the cycle-index of being reported is merely (Journal of Power Sources, 179 (2008): 357-360), can not satisfy the application of suitability for industrialized production 20 times.
Summary of the invention
The present invention is directed to the deficiency of prior art, a kind of preparation method of high power capacity long circulation life molybdenum dioxide/carbon negative pole material is provided, this method prepares heat treatment period weak point in the process, and the material of preparing is big as the negative material capacity, has extended cycle life.
Realize that the concrete technical scheme that the object of the invention adopted is following.
A kind of preparation method of molybdenum dioxide/carbon compound cathode materials, key step is following:
1) cotton fabric with certain size is immersed in the ethanolic solution of phosphomolybdic acid, and stirs;
2) cotton fabric after will soaking carries out drying with aging;
3) in mixed atmosphere, heat-treat with aging cotton fabric, promptly obtain molybdenum dioxide/carbon (MoO warp is dry
2/ C) composite material.
Wherein, the ethanolic solution concentration of said phosphomolybdic acid is 0.05～0.15mM/ml.
Wherein, the baking temperature in the said step (2) is 50～70 ℃.
Wherein, aging temperature is 80～100 ℃.
Wherein, said mixed atmosphere is Ar and H
2Gaseous mixture.
Wherein, said H
2Content be 5%-10%.
Wherein, said mixed atmosphere is the gaseous mixture of alcohol vapour and nitrogen.
The invention also discloses the prepared molybdenum dioxide/carbon compound cathode materials of above-mentioned preparation method.This negative material capacity is big, has extended cycle life good rate capability.
The invention also discloses a kind of electrode slice, it among NNPs is uniformly mixed into slurry by above-mentioned molybdenum dioxide/carbon compound cathode materials and conductive carbon and PVDF with mass ratio at 8: 1: 1, and is coated on the Copper Foil, again after vacuumize, and die-cut processing.
The invention also discloses a kind of button cell, comprise above-mentioned electrode slice.
Through method of the present invention obtain by ultra-fine MoO
2Nano particle (＜2nm) evenly being embedded into novel nano structural composite material in the carbon base body, the pattern of initial cotton fabric remains intact, the MoO that is obtained
2/ C is as lithium ion battery negative material, at 100mA g
-1Under the current density, discharge capacity is 1126mAh g first
-1, 600 cycle discharge specific capacities are 602mAh g
-1At 800mA g
-1Under the current density, 50 cycle discharge specific capacities are 409mAh g
-1, have the characteristic of height ratio capacity, long circulation life and high rate capability.
Description of drawings
Fig. 1 is the SEM figure of product of the present invention.
Fig. 2 is that product of the present invention is schemed at TEM.
Fig. 3 is the EDX figure of product of the present invention.
Fig. 4 is the voltage-capacity curve figure of product of the present invention when different period.
Fig. 5 is the cyclic curve figure of product of the present invention.
Fig. 6 is the cyclic curve comparison diagram of embodiment and Comparative Examples.
Embodiment
Below in conjunction with accompanying drawing and each embodiment, the present invention and beneficial effect thereof are elaborated.
Embodiment one
At first, will be of a size of 20mm * 20mm cotton fabric its be immersed in the ethanolic solution of phosphomolybdic acid that concentration is 0.1mM/ml, stirred 2 hours.
Then, 60 ℃ of dryings 5 minutes, 90 ℃ aging 3 hours.
At last at Ar/H
2(preferred H
2Account for cumulative volume 5%) 500 ℃ of heat treatment 5 hours in the mixed atmosphere, obtained a kind of ultra-fine MoO
2Nano particle (＜2nm) evenly embed the MoO of conductive carbon matrix
2/ C nanostructure composite material.
Fig. 1 is the SEM figure of product of the present invention, shows that end product has still kept the initial pattern of cotton fabric.Fig. 2 is the TEM figure of product of the present invention, and MoO is described
2Nano particle (＜2nm) evenly embed the conductive carbon matrix.Fig. 3 is the EDX figure of product of the present invention, and the main component that product of the present invention is described is MoO
2And carbon.
With the above-mentioned product that obtains as electrode material; Suitable slurry is coated on the Copper Foil in the N-methyl pyrrolidone, to be uniformly mixed into viscosity at 8: 1: 1 according to active material, conductive carbon, Kynoar mass ratio; After 80 ℃ of vacuumizes, die-cutly process the electrode slice that diameter is 8mm.With metal lithium sheet as to electrode, with 1mol/L LiPF
6/ (EC:DMC) be electrolyte, the charging/discharging voltage scope is 3.0～0.01V.Fig. 4 is the discharge curve of product of the present invention when different period, can see that first discharge specific capacity is up to 1126mAh g
-1, the specific capacity of the discharge 697mAh g that still has an appointment for the second time
-1, circulate after 600 times the specific capacity 602mAh g that still has an appointment
-1, shown good reversible capacity and cycle life.Fig. 5 is the cycle performance figure of product under the different electric current density of this method, can see that under the different electric current density, this product all shows excellent cycle performance.
Embodiment two
To be of a size of 20mm * 20mm cotton fabric its be immersed in the ethanolic solution of phosphomolybdic acid that concentration is 0.05mM/ml, stirred 2 hours.Then, 50 ℃ of dryings 30 minutes, then 100 ℃ of burin-in process 6 hours, at Ar/H
2(5%) 600 ℃ of heat treatments obtained MoO in 5 hours in the mixed atmosphere
2/ C composite material, its shape characteristic are ultra-fine MoO
2Nano particle is evenly distributed in the carbon base body.
With the above-mentioned MoO that obtains
2/ C composite material is assembled into button cell with embodiment one identical mode, the test chemical property.
Embodiment three
To be of a size of 20mm * 20mm cotton fabric its be immersed in the ethanolic solution of phosphomolybdic acid that concentration is 0.15mM/ml, stirred 2 hours.Then, 70 ℃ of dryings 5 minutes, then 80 ℃ of burin-in process 6 hours.At Ar/H
2(5%) 550 ℃ of heat treatment 6 hours in the mixed atmosphere obtains MoO
2/ C composite material.
With the above-mentioned MoO that obtains
2/ C composite material is by being assembled into button cell with embodiment one identical mode, the test chemical property.
Among above-mentioned each embodiment; The size of cotton fabric, the ethanolic solution of phosphomolybdic acid only are exemplary; Be not confined on the above-mentioned consumption, in general, the size of cotton fabric can be selected as the case may be; As long as the ethanolic solution of phosphomolybdic acid satisfies certain limit, all can like 0.05-0.2mM/ml.Simultaneously, the time of drying and burin-in process, temperature etc. can specifically be selected as the case may be, are not defined as the concrete numerical value in the foregoing description.In addition, in heat treatment process, the type of mist and content thereof and processing time and temperature etc. also are not limited to the value in the foregoing description, as long as can make cotton fabric carbonization and phosphomolybdic acid generation decomposition and reduction obtain MoO
2Get final product, can be the mist of alcohol vapour and nitrogen, also can be Ar/H like the type of mist
2The gaseous mixture of mist or other types is as adopting Ar/H
2(10%) mist, wherein the content of hydrogen can be adjusted as required, like H
2Content in gaseous mixture can be preferably 5%-10%.In addition, heat treatment time can change as adopting 3 hours-10 hours, and heat treatment temperature can be 400-600 ℃.
Utilize the contrast of prepared negative material of the foregoing description and concrete Comparative Examples below, specify the effect of the prepared negative material of method of the present invention.
Comparative Examples one
Phosphomolybdic acid by the Technology for Heating Processing sintering identical with embodiment 1, is obtained the MoO of pure phase
2Material.Then, with the MoO that obtains
2Material is by being assembled into button cell with embodiment one identical mode, the test chemical property.
Comparative Examples two
The cotton fabric that will be of a size of 20mm * 20mm obtains the pure carbon material by the Technology for Heating Processing sintering identical with embodiment 1.Then, the material with carbon element that obtains by being assembled into button cell with embodiment one identical mode, is tested chemical property.
Fig. 6 is the cyclic curve comparison diagram of embodiment and Comparative Examples, can find out independent MoO
2The cycle performance of material and independent material with carbon element is very poor, and the MoO for preparing by method provided by the invention
2Nano particle evenly embeds the MoO of conductive carbon matrix
2/ C nanostructure composite material has good cycle performance.
Table 1 is the electrical performance data of embodiment and Comparative Examples, shows the MoO of the inventive method preparation
2/ C nanostructure composite material has height ratio capacity, high rate capability and long circulation life.
The electrical property of table 1 embodiment
In sum; Molybdenum dioxide/carbon composite that the preparation method of the molybdenum dioxide negative material that proposes according to the present invention prepares has the high rate performance that high specific capacity, outstanding cycle performance are become reconciled as lithium ion battery negative material; And the preparation method is simple, is fit to large-scale production.
Need to prove that according to the announcement and the elaboration of above-mentioned specification, those skilled in the art in the invention can also change and revise above-mentioned execution mode.Therefore, the embodiment that discloses and describe above the present invention is not limited to also should be in the protection range of claim of the present invention to equivalent modifications more of the present invention and change.In addition, although used some specific terms in this specification, these terms are explanation for ease just, the present invention is not constituted any restriction.
Claims (10)
1. the preparation method of a molybdenum dioxide/carbon compound cathode materials, key step is following:
1) cotton fabric with certain size is immersed in the ethanolic solution of phosphomolybdic acid;
2) cotton fabric after soaking is carried out drying with aging;
3) in mixed atmosphere, heat-treat with aging cotton fabric, promptly obtain molybdenum dioxide/carbon (MoO warp is dry
2/ C) composite material.
2. the preparation method of a kind of molybdenum dioxide/carbon compound cathode materials according to claim 1, wherein, the ethanolic solution concentration of said phosphomolybdic acid is 0.05～0.15mM/ml.
3. the preparation method of a kind of molybdenum dioxide/carbon compound cathode materials according to claim 1 and 2, wherein, the baking temperature in the said step (2) is 50～70 ℃.
4. according to the preparation method of one of claim 1-3 described a kind of molybdenum dioxide/carbon compound cathode materials, wherein, aging temperature is 80～100 ℃.
5. according to the preparation method of one of claim 1-4 described a kind of molybdenum dioxide/carbon compound cathode materials, wherein, said mixed atmosphere is Ar and H
2Gaseous mixture.
6. the preparation method of a kind of molybdenum dioxide/carbon compound cathode materials according to claim 5, wherein, said H
2Content in gaseous mixture is 5%-10%.
7. according to the preparation method of one of claim 1-6 described a kind of molybdenum dioxide/carbon compound cathode materials, said mixed atmosphere is the gaseous mixture of alcohol vapour and nitrogen.
8. the prepared molybdenum dioxide/carbon compound cathode materials of the described preparation method of one of claim 1-7.
9. electrode slice, it among NMPs is uniformly mixed into slurry by the described molybdenum dioxide/carbon compound cathode materials of claim 8 and conductive carbon and PVDF with mass ratio at 8: 1: 1, and is coated on the Copper Foil, again after vacuumize, die-cut processing.
10. a button cell comprises the described electrode slice of claim 9.
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Cited By (11)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103066288A (en) * | 2012-12-07 | 2013-04-24 | 上海锦众信息科技有限公司 | Preparation method of molybdenum-carbon composite cathode material of lithium ion battery |
| CN105355899A (en) * | 2015-11-10 | 2016-02-24 | 上海应用技术学院 | Preparation method for molybdenum dioxide-active carbon composite material |
| RU2656466C1 (en) * | 2017-05-31 | 2018-06-05 | Федеральное государственное бюджетное учреждение науки Институт химии твердого тела Уральского отделения Российской академии наук | Molybdenum dioxide / carbon composite production method |
| CN108321375A (en) * | 2018-02-06 | 2018-07-24 | 哈尔滨师范大学 | A kind of in-situ doping type nanometer molybdenum base material, Preparation method and use |
| CN108878158A (en) * | 2017-05-16 | 2018-11-23 | 中国科学院福建物质结构研究所 | A kind of preparation method and purposes of C-base composte material |
| CN109244423A (en) * | 2018-10-23 | 2019-01-18 | 大连交通大学 | A kind of preparation method with porous spongy carbon-based nano electrode material |
| CN110047659A (en) * | 2019-03-28 | 2019-07-23 | 南京理工大学 | A kind of preparation method of biomass-based flexible electrode material |
| CN113582231A (en) * | 2021-06-08 | 2021-11-02 | 湖南师范大学 | MoO (MoO)2Preparation method of/carbon composite interlayer |
| CN114743807A (en) * | 2022-05-19 | 2022-07-12 | 江苏大学 | Inside and outside raw MoO2Preparation method of/three-dimensional carbon composite material |
| CN115000370A (en) * | 2022-06-02 | 2022-09-02 | 烟台大学 | Molybdenum dioxide confinement growth and modification three-dimensional porous carbon composite electrode material and preparation method thereof |
| CN115092962A (en) * | 2022-05-20 | 2022-09-23 | 江苏师范大学 | Molybdenum dioxide/carbon composite electrode material and preparation method and application thereof |
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Non-Patent Citations (1)
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Cited By (15)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103066288A (en) * | 2012-12-07 | 2013-04-24 | 上海锦众信息科技有限公司 | Preparation method of molybdenum-carbon composite cathode material of lithium ion battery |
| CN105355899A (en) * | 2015-11-10 | 2016-02-24 | 上海应用技术学院 | Preparation method for molybdenum dioxide-active carbon composite material |
| CN108878158B (en) * | 2017-05-16 | 2020-02-21 | 中国科学院福建物质结构研究所 | Preparation method and application of carbon-based composite material |
| CN108878158A (en) * | 2017-05-16 | 2018-11-23 | 中国科学院福建物质结构研究所 | A kind of preparation method and purposes of C-base composte material |
| RU2656466C1 (en) * | 2017-05-31 | 2018-06-05 | Федеральное государственное бюджетное учреждение науки Институт химии твердого тела Уральского отделения Российской академии наук | Molybdenum dioxide / carbon composite production method |
| CN108321375A (en) * | 2018-02-06 | 2018-07-24 | 哈尔滨师范大学 | A kind of in-situ doping type nanometer molybdenum base material, Preparation method and use |
| CN108321375B (en) * | 2018-02-06 | 2020-06-09 | 哈尔滨师范大学 | In-situ doped nano molybdenum-based material, preparation method and application |
| CN109244423B (en) * | 2018-10-23 | 2021-03-09 | 大连交通大学 | Preparation method of porous spongy carbon-based nano electrode material |
| CN109244423A (en) * | 2018-10-23 | 2019-01-18 | 大连交通大学 | A kind of preparation method with porous spongy carbon-based nano electrode material |
| CN110047659A (en) * | 2019-03-28 | 2019-07-23 | 南京理工大学 | A kind of preparation method of biomass-based flexible electrode material |
| CN113582231A (en) * | 2021-06-08 | 2021-11-02 | 湖南师范大学 | MoO (MoO)2Preparation method of/carbon composite interlayer |
| CN114743807A (en) * | 2022-05-19 | 2022-07-12 | 江苏大学 | Inside and outside raw MoO2Preparation method of/three-dimensional carbon composite material |
| CN114743807B (en) * | 2022-05-19 | 2024-03-19 | 江苏大学 | Internally and externally generated MoO 2 Preparation method of three-dimensional carbon composite material |
| CN115092962A (en) * | 2022-05-20 | 2022-09-23 | 江苏师范大学 | Molybdenum dioxide/carbon composite electrode material and preparation method and application thereof |
| CN115000370A (en) * | 2022-06-02 | 2022-09-02 | 烟台大学 | Molybdenum dioxide confinement growth and modification three-dimensional porous carbon composite electrode material and preparation method thereof |
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Application publication date: 20120801 |