CN104795545A - Composite electrode material of molybdenum dioxide quantum dot embedded mesoporous carbon nanosheets, as well as preparation method and application of composite electrode material - Google Patents
Composite electrode material of molybdenum dioxide quantum dot embedded mesoporous carbon nanosheets, as well as preparation method and application of composite electrode material Download PDFInfo
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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
- H01M4/00—Electrodes
- H01M4/02—Electrodes composed of, or comprising, active material
- H01M4/36—Selection of substances as active materials, active masses, active liquids
- H01M4/362—Composites
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B82—NANOTECHNOLOGY
- B82Y—SPECIFIC USES OR APPLICATIONS OF NANOSTRUCTURES; MEASUREMENT OR ANALYSIS OF NANOSTRUCTURES; MANUFACTURE OR TREATMENT OF NANOSTRUCTURES
- B82Y30/00—Nanotechnology for materials or surface science, e.g. nanocomposites
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- H01M10/00—Secondary cells; Manufacture thereof
- H01M10/05—Accumulators with non-aqueous electrolyte
- H01M10/052—Li-accumulators
- H01M10/0525—Rocking-chair batteries, i.e. batteries with lithium insertion or intercalation in both electrodes; Lithium-ion batteries
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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
- H01M4/00—Electrodes
- H01M4/02—Electrodes composed of, or comprising, active material
- H01M4/13—Electrodes for accumulators with non-aqueous electrolyte, e.g. for lithium-accumulators; Processes of manufacture thereof
- H01M4/139—Processes of manufacture
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- H01M4/00—Electrodes
- H01M4/02—Electrodes composed of, or comprising, active material
- 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
- H01M4/483—Selection of substances as active materials, active masses, active liquids of inorganic oxides or hydroxides for non-aqueous cells
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- H01M4/02—Electrodes composed of, or comprising, active material
- H01M4/36—Selection of substances as active materials, active masses, active liquids
- H01M4/58—Selection of substances as active materials, active masses, active liquids of inorganic compounds other than oxides or hydroxides, e.g. sulfides, selenides, tellurides, halogenides or LiCoFy; of polyanionic structures, e.g. phosphates, silicates or borates
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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
- H01M4/00—Electrodes
- H01M4/02—Electrodes composed of, or comprising, active material
- H01M4/62—Selection of inactive substances as ingredients for active masses, e.g. binders, fillers
- H01M4/624—Electric conductive fillers
- H01M4/625—Carbon or graphite
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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
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Abstract
The invention relates to composite electrode material of molybdenum dioxide quantum dot embedded mesoporous carbon nanosheets, as well as preparation method and application of composite electrode material. According to the invention, complex reaction of molybdenum source molecules and dopamine is carried out to obtain a low polymer, then under the action of dissolved oxygen, the product is subjected to auto polymerization and assembled into a three-dimensional flowerlike molybdenum-contained metallo-organic compound, then through high temperature carbonation, the composite material of molybdenum dioxide quantum dot embedded mesoporous carbon nanosheets is prepared, and finally is self-assembled into a three-dimensional flowerlike structure. The effective contact area of the composite material and electrolyte and electrochemical active sites are remarkably improved through the super-small sized molybdenum dioxide quantum dots, and the diffusion length of lithium ions is reduced; after the coupling with mesoporous carbon, the electron transmission rate is increased; based on the advantages, when the composite electrode material is applied to lithium ion battery cathode materials, and the advantages of high specific capacitance, rate capability and long cycle life are realized.
Description
Technical field
The present invention relates to new energy materials field, relate to a kind of lithium ion battery cathode material and its preparation method and application, be specifically related to a kind of molybdenum dioxide quantum dot and embed mesoporous carbon nanometer sheet, and be self-assembled into flower-like structure lithium ion battery negative material further.
Background technology
In recent years, the fast development of portable electric appts, hybrid electric vehicle, electric automobile and space technology, has higher requirement to the performance of the energy storage devices such as lithium ion battery.The preparation of high-efficient electrode material is the key of development lithium ion battery, and the lithium ion battery electrode material therefore developing high-energy-density, high-specific-power and long circulation life has become the focus of current research.Current business-like lithium ion battery negative material is mainly graphite-like material with carbon element, and the specific discharge capacity of such negative material in battery product is about 330mAh/g, and close to its theoretical value (372mAh/g), the space of improving its capacity is further very little.Therefore, development of new height ratio capacity negative material replaces graphite-like material with carbon element is the required key issue solved of development lithium ion battery.
Research discovery molybdenum dioxide causes great interest (the Huang Y. of scientific research personnel as having the advantage such as lower resistivity, good electrochemical stability during lithium ion battery negative material, Song.Y., et al.Self-Assembled Hierarchical MoO2/Graphene Nanoarchitectures and TheirApplication as a High-Performance Anode Material for Lithium-Ion Batteries.ACSNano, 2011,5,7100 – 7107).Under normal temperature, the storage lithium mechanism of block molybdenum dioxide is MoO
2+ xLi
++ xe
-→ Li
xmoO
2(0 < x < 1), its theoretical capacity is about 209mAh/g (LiMoO
2).But, work as MoO
2be reduced in nanoscale, its embedding lithium mechanism is changed to MoO
2+ 4Li
++ 4e
-→ 2Li
2o+Mo.Under this embedding lithium mechanism, can embed four lithium ions, its theoretical capacity is up to 838mAh/g.Therefore, the molybdenum dioxide of nanoscale has high specific discharge capacity.Such as, (Zhou L., Wu H.B., Wang Z.Y., the et al.Interconnected MoO such as Zhou
2nanocrystals with Carbon Nanocoating as High-CapacityAnode Materials for Lithium-ion Batteries.ACS Applied Materials & Interfaces, 2011,3 (12): 4853 ~ 4857) MoO that the carbon nanometer that utilized hydro thermal method to prepare is coated
2nano particle composite material.This material is under the current density of 200mA/g, and after 50 circulations, capacity still remains on 629mAh/g.(Chen L., Guo B., Fang C., the et al.Synthesis and Lithium Storage Mechanism ofUltrafine MoO such as Chen
2nanorods.Chem.Mater.2012,24,457 ~ 463) then utilize SBA-15 as template, adopt the method for nanometer casting to prepare to be of a size of ~ ultra-fine the MoO of 5nm
2nano wire.This material is under the current density of C/20, and after 29 circulations, specific capacity reaches 830mAh/g, close to its theoretical capacity 838mAh/g.
Summary of the invention
The object of this invention is to provide a kind of molybdenum dioxide quantum dot and embed mesoporous carbon nanometer sheet, and be self-assembled into the preparation method of three-dimensional flower-shaped structure nanometer composite material and the application in field of lithium ion battery thereof.Mentality of designing is as follows:
Utilize molybdenum source molecule and dopamine molecule generation complex reaction, under the effect of dissolved oxygen, autohemagglutination merges the metallo-organic compound be assembled into containing molybdenum, again by high temperature cabonization process, prepare a kind of molybdenum dioxide quantum dot and embedded mesoporous carbon nanosheet composite material, and be self-assembled into three-dimensional flower-shaped structure further.Wherein, the size of molybdenum dioxide quantum dot is less than 1nm.The molybdenum dioxide quantum dot of super-small significantly improves effective contact area and the electrochemical site of itself and electrolyte, reduces the diffusion length of lithium ion simultaneously; After being coupled with mesoporous carbon, also accelerate the transmission rate of electronics.Based on these advantages, during as lithium ion battery negative material, show the cycle life of high specific capacitance, high high rate performance and excellence.
The present invention is achieved by the following technical solutions:
Molybdenum dioxide quantum dot embeds a combination electrode material for mesoporous carbon nanometer sheet, and described molybdenum dioxide quantum dot embeds in described mesoporous carbon nanometer sheet, and is self-assembled into flower-like structure; Wherein, the diameter of described flower-like structure is 1 ~ 2 μm, and the diameter of described mesoporous carbon nanometer sheet is 300 ~ 600nm, thickness is 20 ~ 60nm; The size of described molybdenum dioxide quantum dot is less than 1nm.
Above-mentioned molybdenum dioxide quantum dot embeds the preparation method of mesoporous carbon nanometer sheet combination electrode material, comprises the steps:
(1) 0.2 ~ 0.6g triblock copolymer polyoxyethylene-poly-oxypropylene polyoxyethylene is dissolved in 200 ~ 600mL deionized water, then add 0.25 ~ 0.75g tromethamine to stir and obtain cushioning liquid, again 0.3 ~ 0.9g molybdenum source presoma is scattered in described cushioning liquid, after ultrasonic 30 ~ 90min, is cooled to room temperature;
(2) 150 ~ 450mg dopamine is added while stirring in the mixed solution obtained in step (1), first dopamine and molybdenum source molecular complex are molybdenum/dopamine oligomer, stirring reaction 3 ~ 24h is continued at 10 ~ 40 DEG C in air atmosphere, described molybdenum/dopamine oligomer autohemagglutination merges and is assembled into the three-dimensional flower-shaped metallorganic containing molybdenum, filters, collects after centrifugal, carrying out washing treatment the metallorganic of the molybdenum obtained;
(3) the metallorganic carburizing reagent 2 ~ 4h at 500 ~ 600 DEG C in an inert atmosphere of molybdenum will obtained in step (2), namely obtains described molybdenum dioxide quantum dot and embeds mesoporous carbon nanometer sheet combination electrode material.
The structure of described combination electrode material is: described molybdenum dioxide quantum dot embeds in described mesoporous carbon nanometer sheet, and is self-assembled into flower-like structure; Wherein, the diameter of described flower-like structure is 1 ~ 2 μm, and the diameter of described mesoporous carbon nanometer sheet is 300 ~ 600nm, thickness is 20 ~ 60nm; The size of described molybdenum dioxide quantum dot is less than 1nm.
Described molybdenum source presoma is the molybdenum such as sodium molybdate or ammonium molybdate source.
The mass ratio of described molybdenum source presoma and dopamine is 2:1 ~ 6:1.
Described inert atmosphere is argon gas.
Above-mentioned molybdenum dioxide quantum dot embeds the application of the combination electrode material of mesoporous carbon nanometer sheet, and described combination electrode material is applied to lithium ion battery as negative material.
Molybdenum dioxide/mesoporous carbon composite electrode material prepared by the present invention can show excellent chemical property as lithium ion battery negative material.The molybdenum dioxide quantum dot of super-small significantly improves effective contact area and the electrochemical site of itself and electrolyte, reduces the diffusion length of lithium ion simultaneously; After being coupled with mesoporous carbon, also accelerate the transmission rate of electronics.Based on these advantages, during as lithium ion battery negative material, show the cycle life of high specific capacitance, high high rate performance and excellence.
Accompanying drawing explanation
Fig. 1 is the XRD curve of embodiment 1 product;
In Fig. 2, (a) is embodiment 1 Product scan Electronic Speculum figure, b (), (c) are the transmission electron microscope pictures of embodiment 1 product, (d), (e), (f) are respectively the distribution diagram of element of the molybdenum of embodiment 1 product, oxygen, carbon;
Fig. 3 is the Electrochemical results that product prepared by embodiment 1 is used as lithium ion battery negative material.
Embodiment
Below by embodiment, the present invention is specifically described.What be necessary to herein means out is that following examples are only for the invention will be further described; limiting the scope of the invention can not be interpreted as; some nonessential improvement and adjustment that professional and technical personnel's content according to the present invention in this field is made, still belong to protection scope of the present invention.
Embodiment 1
0.2g triblock copolymer polyoxyethylene-poly-oxypropylene polyoxyethylene is dissolved in 200ml water, then add 0.25g tromethamine to stir and obtain cushioning liquid, again 0.3g sodium molybdate is scattered in described cushioning liquid, cool to room temperature after ultrasonic 30min;
150mg dopamine is added while stirring, stirring reaction 8h at 10 DEG C, filter centrifugation washing collecting reaction product in above-mentioned mixed solution;
By products therefrom carburizing reagent 2h at 500 DEG C in an inert atmosphere, described molybdenum dioxide/mesoporous carbon composite electrode material can be obtained.The XRD curve of product as shown in Figure 1, the transmission electron microscope photo of product as shown in Figure 2, in Fig. 2, (a) is embodiment 1 Product scan Electronic Speculum figure, b (), (c) are the transmission electron microscope pictures of embodiment 1 product, (d), (e), (f) are respectively the distribution diagram of element of the molybdenum of embodiment 1 product, oxygen, carbon.Used as lithium ion battery negative material, CR2016 type button cell is adopted to test its chemical property.Fig. 3 is the rate charge-discharge test result figure of material, and as can be seen from the figure along with the increase of current density, its capacity suppression ratio is comparatively slow, illustrates that this material has good rate charge-discharge performance.And the circulation volume several times under each multiplying power keeps stable, when current density returns low range, capacity can well recover, and proves that this material has good cyclical stability.
Embodiment 2
0.4g triblock copolymer polyoxyethylene-poly-oxypropylene polyoxyethylene is dissolved in 400ml water, then add 0.5g tromethamine to stir and obtain cushioning liquid, again 0.6g sodium molybdate is scattered in described cushioning liquid, cool to room temperature after ultrasonic 60min;
450mg dopamine is added while stirring, stirring reaction 12h at 20 DEG C, filter centrifugation washing collecting reaction product in above-mentioned mixed solution;
By products therefrom carburizing reagent 3h at 500 DEG C in an inert atmosphere, described molybdenum dioxide/mesoporous carbon composite electrode material can be obtained.Electro-chemical test part with embodiment 1, the prepared materials show experimental result almost identical with embodiment 1.
Embodiment 3
0.6g triblock copolymer polyoxyethylene-poly-oxypropylene polyoxyethylene is dissolved in 600ml water, then add 0.75g tromethamine to stir and obtain cushioning liquid, again 0.9g ammonium molybdate is scattered in described cushioning liquid, cool to room temperature after ultrasonic 60min;
150mg dopamine is added while stirring, stirring reaction 24h at 40 DEG C, filter centrifugation washing collecting reaction product in above-mentioned mixed solution;
By products therefrom carburizing reagent 4h at 600 DEG C in an inert atmosphere, described molybdenum dioxide/mesoporous carbon composite electrode material can be obtained.Electro-chemical test part with embodiment 1, the prepared materials show experimental result almost identical with embodiment 1.
The foregoing is only preferred embodiment of the present invention, be not used for limiting practical range of the present invention.Have in any art and usually know the knowledgeable, without departing from the spirit and scope of the present invention, when doing various variation and retouching, therefore protection scope of the present invention is when being as the criterion with claims institute confining spectrum.
Claims (7)
1. molybdenum dioxide quantum dot embeds a combination electrode material for mesoporous carbon nanometer sheet, and it is characterized in that, described molybdenum dioxide quantum dot embeds in described mesoporous carbon nanometer sheet, and is self-assembled into flower-like structure; Wherein, the diameter of described flower-like structure is 1 ~ 2 μm, and the diameter of described mesoporous carbon nanometer sheet is 300 ~ 600nm, thickness is 20 ~ 60nm; The size of described molybdenum dioxide quantum dot is less than 1nm.
2. molybdenum dioxide quantum dot embeds a preparation method for mesoporous carbon nanometer sheet combination electrode material, it is characterized in that, comprises the steps:
(1) 0.2 ~ 0.6g triblock copolymer polyoxyethylene-poly-oxypropylene polyoxyethylene is dissolved in 200 ~ 600mL deionized water, then add 0.25 ~ 0.75g tromethamine to stir and obtain cushioning liquid, again 0.3 ~ 0.9g molybdenum source presoma is scattered in described cushioning liquid, after ultrasonic 30 ~ 90min, is cooled to room temperature;
(2) 150 ~ 450mg dopamine is added while stirring in the mixed solution obtained in step (1), first dopamine and molybdenum source molecular complex are molybdenum/dopamine oligomer, stirring reaction 3 ~ 24h is continued at 10 ~ 40 DEG C in air atmosphere, described molybdenum/dopamine oligomer autohemagglutination merges and is assembled into the three-dimensional flower-shaped metallorganic containing molybdenum, filters, collects after centrifugal, carrying out washing treatment the metallorganic of the molybdenum obtained;
(3) the metallorganic carburizing reagent 2 ~ 4h at 500 ~ 600 DEG C in an inert atmosphere of molybdenum will obtained in step (2), namely obtains described molybdenum dioxide quantum dot and embeds mesoporous carbon nanometer sheet combination electrode material.
3. preparation method according to claim 2, is characterized in that, the structure of described combination electrode material is: described molybdenum dioxide quantum dot embeds in described mesoporous carbon nanometer sheet, and is self-assembled into flower-like structure; Wherein, the diameter of described flower-like structure is 1 ~ 2 μm, and the diameter of described mesoporous carbon nanometer sheet is 300 ~ 600nm, thickness is 20 ~ 60nm; The size of described molybdenum dioxide quantum dot is less than 1nm.
4. preparation method according to claim 2, is characterized in that, described molybdenum source presoma is sodium molybdate or ammonium molybdate.
5. preparation method according to claim 2, is characterized in that, the mass ratio of described molybdenum source presoma and dopamine is 2:1 ~ 6:1.
6. preparation method according to claim 2, is characterized in that, described inert atmosphere is argon gas.
7. molybdenum dioxide quantum dot according to claim 1 embeds the application of the combination electrode material of mesoporous carbon nanometer sheet, and it is characterized in that, described combination electrode material is applied to lithium ion battery as negative material.
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Cited By (9)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN106099126A (en) * | 2016-06-11 | 2016-11-09 | 北京化工大学 | A kind of flower-like structure cobalt sulfide/carbon composite and preparation method thereof |
| CN107266098A (en) * | 2017-06-07 | 2017-10-20 | 常州瑞坦商贸有限公司 | A kind of preparation method of ceramic toughening special-purpose nanometer zirconium dioxide |
| CN109473650A (en) * | 2018-11-09 | 2019-03-15 | 东北大学秦皇岛分校 | A kind of MoO2/ rGO composite material and preparation method and application |
| CN109678210A (en) * | 2019-01-11 | 2019-04-26 | 中国检验检疫科学研究院 | MoO for the detection of highly sensitive Surface enhanced Raman spectroscopy2Quantum dot synthetic method |
| CN110957486A (en) * | 2019-11-14 | 2020-04-03 | 江苏大学 | Preparation method of superstructure tin-carbon-molybdenum oxide composite material and application of superstructure tin-carbon-molybdenum oxide composite material to electrode |
| CN110993911A (en) * | 2019-11-30 | 2020-04-10 | 湘潭大学 | Embedded lithium ion battery negative electrode material with high specific discharge capacity and preparation method thereof |
| CN111584834A (en) * | 2020-04-20 | 2020-08-25 | 中国计量大学 | Preparation of metal oxide quantum dot embedded three-dimensional carbon nano material |
| CN112310385A (en) * | 2020-10-12 | 2021-02-02 | 浙江理工大学 | Silver-ear-shaped nanosphere material assembled by molybdenum dioxide nanoparticles inlaid with carbon nanosheets and preparation and application thereof |
| CN112421007A (en) * | 2020-11-20 | 2021-02-26 | 贵州梅岭电源有限公司 | Preparation method of tungsten oxide/carbon flower-ball-shaped lithium battery composite negative electrode material |
-
2015
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| AKKISETTY BHASKAR, ET AL.: "Enhanced nanoscale conduction capability of MoO2/Graphene composite for high performance anodes in lithium ion batteries", 《JOURNAL OF POWER SOURCES》 * |
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Cited By (11)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN106099126A (en) * | 2016-06-11 | 2016-11-09 | 北京化工大学 | A kind of flower-like structure cobalt sulfide/carbon composite and preparation method thereof |
| CN107266098A (en) * | 2017-06-07 | 2017-10-20 | 常州瑞坦商贸有限公司 | A kind of preparation method of ceramic toughening special-purpose nanometer zirconium dioxide |
| CN109473650A (en) * | 2018-11-09 | 2019-03-15 | 东北大学秦皇岛分校 | A kind of MoO2/ rGO composite material and preparation method and application |
| CN109678210A (en) * | 2019-01-11 | 2019-04-26 | 中国检验检疫科学研究院 | MoO for the detection of highly sensitive Surface enhanced Raman spectroscopy2Quantum dot synthetic method |
| CN110957486A (en) * | 2019-11-14 | 2020-04-03 | 江苏大学 | Preparation method of superstructure tin-carbon-molybdenum oxide composite material and application of superstructure tin-carbon-molybdenum oxide composite material to electrode |
| CN110993911A (en) * | 2019-11-30 | 2020-04-10 | 湘潭大学 | Embedded lithium ion battery negative electrode material with high specific discharge capacity and preparation method thereof |
| CN110993911B (en) * | 2019-11-30 | 2022-04-19 | 湘潭大学 | Embedded lithium ion battery negative electrode material with high specific discharge capacity and preparation method thereof |
| CN111584834A (en) * | 2020-04-20 | 2020-08-25 | 中国计量大学 | Preparation of metal oxide quantum dot embedded three-dimensional carbon nano material |
| CN112310385A (en) * | 2020-10-12 | 2021-02-02 | 浙江理工大学 | Silver-ear-shaped nanosphere material assembled by molybdenum dioxide nanoparticles inlaid with carbon nanosheets and preparation and application thereof |
| CN112421007A (en) * | 2020-11-20 | 2021-02-26 | 贵州梅岭电源有限公司 | Preparation method of tungsten oxide/carbon flower-ball-shaped lithium battery composite negative electrode material |
| CN112421007B (en) * | 2020-11-20 | 2022-06-14 | 贵州梅岭电源有限公司 | Preparation method of tungsten oxide/carbon flower-ball-shaped lithium battery composite negative electrode material |
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