CN107845775A - Graphene/v2o5 composite material and preparation method thereofs and anode - Google Patents
Graphene/v2o5 composite material and preparation method thereofs and anode Download PDFInfo
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- CN107845775A CN107845775A CN201710924275.8A CN201710924275A CN107845775A CN 107845775 A CN107845775 A CN 107845775A CN 201710924275 A CN201710924275 A CN 201710924275A CN 107845775 A CN107845775 A CN 107845775A
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- kermesinus
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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
- H01M4/1391—Processes of manufacture of electrodes based on mixed oxides or hydroxides, or on mixtures of oxides or hydroxides, e.g. LiCoOx
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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
- H01M4/131—Electrodes based on mixed oxides or hydroxides, or on mixtures of oxides or hydroxides, e.g. LiCoOx
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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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- 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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Abstract
The invention discloses graphene/v2o5 composite material and preparation method thereofs, it comprises the following steps：Step 1: it is 70 ~ 90 DEG C of distilled water to take constant temperature, weighs some g solids ammonium metavanadates and add in distilled water and stir to being completely dissolved；Step 2: taking some ml graphene dispersing solutions, and it is added dropwise into ammonium metavanadate aqueous solution, and is completely dissolved under stirring；Step 3: taking some ml 40% sulfuric acid solution, and heating stirring simultaneously is instilled with 1 ~ 5 drop/s speed and, to kermesinus precipitation is generated, when kermesinus precipitation is not further added by, stops that sulfuric acid solution, heating is added dropwise；Step 4: continuing to stir and separate out upper strata clear water, after being cleaned 1 ~ 5 time using distilled water, suction filtration obtains kermesinus precipitation；12h is dried Step 5: kermesinus precipitation is positioned in vacuum drying chamber at 120 DEG C, obtains graphene/V2O5 compounds；Step 6: the graphene after drying/V2O5 compounds are calcined into 4 ~ 8h at 300 ~ 450 DEG C, grinding is then taken out, obtains graphene/V2O5 composite powders.
Description
Technical field
The present invention relates to battery electrode material and its preparing technical field, is applied to do battery electrode more particularly to one kind
The graphene of material/v2o5 composite material and preparation method thereofs.
Background technology
At present, energy shortage turns into governments at all levels' increasingly concern, and cleaning, regeneration, the safe and reliable energy make
With extremely urgent.The advantages that lithium ion battery is because of its higher energy density, good cyclical stability and low self-discharge rate,
It is one of renewable chemical energy source of excellent performance.In many anode material for lithium-ion batteries, there is layer structure just
Hand over phase V2O5 with its raw material sources extensively, relative low price, easily prepare, security is good the advantages that receive extensive concern,
It is considered as the anode material for lithium-ion batteries of new generation for having very much application prospect.It is but poor cyclical stability, relatively low
Lithium ion diffusion coefficient and bad electron conduction are always to restrict V2O5 as anode material for lithium-ion batteries practical application
Key issue.
V2O5 is because the advantages that its intercalation configuration and high-energy-density, can be applicable on electrode material, but V2O5 is by electricity
It is poor with cycle performance that the larger limitation of sub- transport resistance causes its specific capacity in high magnification relatively low.Graphene is by as compound
Material and introduce, not only strengthening electric conductivity and can prevent vanadium from dissolving.Wherein, V2O5 internet startup disks are within graphene sheet layer,
V2O5 is that lithium ion receives main body, and graphene nano layer provides passage for electric transmission, had when the composite is as electrode
Performance, good cycle performance and height ratio capacity are deviate from good ion insertion.Therefore, vanadic anhydride and graphene is compound
Material shows unprecedented advantage as the electrode material of lithium ion battery and ultracapacitor.
Therefore, now provide a kind of graphene/v2o5 composite material and preparation method thereofs and anode.
The content of the invention
Therefore, the present invention provides a kind of graphene/v2o5 composite material and preparation method thereofs and anode.
Therefore, the invention provides graphene/v2o5 composite material and preparation method thereofs, it comprises the following steps：
Step 1: the distilled water for taking constant temperature to be 70 ~ 90 DEG C, weighs some g solids ammonium metavanadates and adds in distilled water and stir extremely
It is completely dissolved；
Step 2: taking some ml graphene dispersing solutions, it meets following ratio：Solid ammonium metavanadate（g）：Graphene dispersing solution
（mg/ml）=5:1~2:1, and be added dropwise under stirring into ammonium metavanadate aqueous solution, and be completely dissolved；
Step 3: taking some ml 40% sulfuric acid solution, it meets following ratio：Solid ammonium metavanadate（g）：Sulfuric acid solution
（ml）=1:1~1:3, and instilled with 1 ~ 5 drop/s speed in the solution after the completion of step 2 reaction, while heating stirring is to life
Precipitated into kermesinus, when kermesinus precipitation is not further added by, stops that sulfuric acid solution is added dropwise and stop heating；
Step 4: continuing the product of whipping step three, and upper strata clear water is separated out, after being cleaned 1 ~ 5 time using distilled water, filtered
Precipitated to kermesinus；
Step 5: by obtained kermesinus precipitation be positioned in vacuum drying chamber at 120 DEG C dry 12h, obtain graphene/
V2O5 compounds；
Step 6: the graphene after drying/V2O5 compounds are calcined into 4 ~ 8 h at 300 ~ 450 DEG C, grinding is then taken out,
Obtain graphene/V2O5 composite powders.
In step 1, take distilled water and be contained up in beaker, then beaker is placed in thermostat water bath, be heated to 70
~ 90 DEG C, and keep constant temperature, 5 ~ 10 g solid ammonium metavanadate is then weighed, adds in distilled water and magnetic agitation is to completely molten
Solution.
In step 2,1 ~ 5 mg/ mL graphene dispersing solutions are taken, and under the conditions of magnetic agitation, metavanadic acid is added dropwise
To being completely dissolved in aqueous ammonium.
In step 3,5 ~ 30 mL 40% (byvolume) sulfuric acid solutions are taken, are stirred with 1 ~ 5 drop/s speed in heating
Mix and added under state in the solution after the completion of step 2 is reacted, continue 20min to kermesinus precipitation is generated, when kermesinus precipitates not
When being further added by, stop that sulfuric acid solution is added dropwise and stop heating.
In step 6, it is calcined using Muffle furnace.
Anode, it includes aluminium foil, and the positive electrode being covered on aluminium foil, and the positive electrode includes graphite
Alkene/V2O5 combination electrode materials and Kynoar and Super-P, and the two meets mass ratio：Graphene/V2O5 is compound
Electrode material：Kynoar and Super-P=80:10, wherein, the graphene/V2O5 combination electrode materials are using as above
The made graphene of described method/V2O5 composite powders.
The present invention has the following advantages that part relative to prior art：
The preparation technology of graphene of the present invention/V2O5 composites is simple, and sintering process does not need atmosphere protection, and
Sintering temperature is 300 ~ 450 DEG C, and sintering time is short, and production process energy consumption is low, and production cost is low；On the other hand, the preparation process
Middle use medicament is all inorganic medicament, it is not necessary to using with volatility, organic medicament of harmfulness, the preparation process green ring
Protect；Meanwhile graphene/V2O5 the composites prepared by this method can be as lithium ion battery and the positive pole of ultracapacitor
Active material uses, and when doing electrode material, discharge capacity is higher, and under 50 mA/g current densities, specific discharge capacity reaches
300 ~ 350 mAh/g, and the forthright again of the composite is also improved significantly.
Brief description of the drawings
, below will be to specific in order to illustrate more clearly of the specific embodiment of the invention or technical scheme of the prior art
The required accompanying drawing used is briefly described in embodiment or description of the prior art, it should be apparent that, in describing below
Accompanying drawing is some embodiments of the present invention, for those of ordinary skill in the art, before creative work is not paid
Put, other accompanying drawings can also be obtained according to these accompanying drawings.
Fig. 1 is the SEM spectrum of graphene of the present invention/V2O5 composites；
Fig. 2 is the Raman collection of illustrative plates of graphene of the present invention/V2O5 composites；
Fig. 3 is graphene of the present invention/specific discharge capacity of the V2O5 combination electrode materials under different current density conditions；
Fig. 4 is specific discharge capacity of the graphene of the present invention/V2O5 composites under 200 mA/g current density conditions.
Embodiment
Technical scheme is clearly and completely described below in conjunction with accompanying drawing, it is clear that described implementation
Example is part of the embodiment of the present invention, rather than whole embodiments.Based on the embodiment in the present invention, ordinary skill
The every other embodiment that personnel are obtained under the premise of creative work is not made, belongs to the scope of protection of the invention.
As long as in addition, technical characteristic involved in invention described below different embodiments non-structure each other
It is be combined with each other into conflict can.
Embodiment 1
Graphene/v2o5 composite material and preparation method thereofs are present embodiments provided, it comprises the following steps：
Step 1: the distilled water for taking constant temperature to be 70 ~ 90 DEG C, weighs some g solids ammonium metavanadates and adds in distilled water and stir extremely
It is completely dissolved；
Step 2: taking some ml graphene dispersing solutions, it meets following ratio：Solid ammonium metavanadate（g）：Graphene dispersing solution
（mg/ml）=5:1~2:1, and be added dropwise under stirring into ammonium metavanadate aqueous solution, and be completely dissolved；
Step 3: taking some ml 40% sulfuric acid solution, it meets following ratio：Solid ammonium metavanadate（g）：Sulfuric acid solution
（ml）=1:1~1:3, and instilled with 1 ~ 5 drop/s speed in the solution after the completion of step 2 reaction, while heating stirring is to life
Precipitated into kermesinus, when kermesinus precipitation is not further added by, stops that sulfuric acid solution is added dropwise and stop heating；
Step 4: continuing the product of whipping step three, and upper strata clear water is separated out, after being cleaned 1 ~ 5 time using distilled water, filtered
Precipitated to kermesinus；
Step 5: by obtained kermesinus precipitation be positioned in vacuum drying chamber at 120 DEG C dry 12h, obtain graphene/
V2O5 compounds；
Step 6: the graphene after drying/V2O5 compounds are calcined into 4 ~ 8 h at 300 ~ 450 DEG C, grinding is then taken out,
Obtain graphene/V2O5 composite powders.
In the present embodiment, the preparation technology of graphene/V2O5 composites is simple, and sintering process does not need atmosphere to protect
Shield, and sintering temperature is 300 ~ 450 DEG C, sintering time is short, and production process energy consumption is low, and production cost is low；On the other hand, the system
The use of medicament is all inorganic medicament during standby, it is not necessary to using with volatility, organic medicament of harmfulness, the preparation process
It is green；Meanwhile graphene/V2O5 the composites prepared by this method can be used as lithium ion battery and ultracapacitor
Positive electrode active materials use, and when doing electrode material, discharge capacity is higher, under 50 mA/g current densities, specific discharge capacity
300 ~ 350 mAh/g are reached, and the forthright again of the composite is also improved significantly.
Specifically, in step 1, take distilled water and be contained up in beaker, then beaker is placed in thermostat water bath,
70 ~ 90 DEG C are heated to, and keeps constant temperature, then weighs 5 ~ 10 g solid ammonium metavanadate, is added in distilled water and magnetic agitation
To being completely dissolved.
In step 2,1 ~ 5 mg/ mL graphene dispersing solutions are taken, and under the conditions of magnetic agitation, metavanadic acid is added dropwise
To being completely dissolved in aqueous ammonium.
In step 3,5 ~ 30 mL 40% (byvolume) sulfuric acid solutions are taken, are stirred with 1 ~ 5 drop/s speed in heating
Mix and added under state in the solution after the completion of step 2 is reacted, continue 20min to kermesinus precipitation is generated, when kermesinus precipitates not
When being further added by, stop that sulfuric acid solution is added dropwise and stop heating.
In step 6, it is calcined using Muffle furnace.
The stereoscan photograph of graphene made from the present embodiment 1/V2O5 composites, can by Fig. 1 as shown in Fig. 1
To find out that the particle size distribution of graphene/V2O5 composites is uniform, particle size is in 100 nm or so.
Further, Fig. 2 is graphene made from the present embodiment 1/V2O5 composite Raman collection of illustrative plates, as seen from Figure 2
By coprecipitation graphene and V2O5 there occurs compound, and graphene/V2O5 composites are prepared.
Further, chemical property such as Fig. 3 and Fig. 4 institutes of graphene made from the present embodiment 1/V2O5 composite positive poles
Show.It can be seen from Fig. 3 and Fig. 4 the specific discharge capacity of the graphene/V2O5 composite positive poles and discharge-rate performance compared with
Blank V2O5 positive electrodes are obviously improved, and under 50 mA/g current density conditions, graphene/V2O5 combination electrode materials are put
Electric specific capacity can reach 315 mAh/g；Under 200 mA/g current density conditions, graphene/V2O5 combination electrode materials electric discharge
Specific capacity can reach 275 mAh/g.
Embodiment 2
On the basis of above-described embodiment, the present embodiment further provides for a kind of anode, and it includes aluminium foil, and is covered in
Positive electrode on aluminium foil, the positive electrode include graphene/V2O5 combination electrode materials and Kynoar and Super-
P, and the two meets mass ratio：Graphene/V2O5 combination electrode materials：Kynoar and Super-P=80:10, its
In, the graphene/V2O5 combination electrode materials are compound using the made graphene/V2O5 of the method described in embodiment 1
Material powder.
Obviously, above-described embodiment is only intended to clearly illustrate example, and is not the restriction to embodiment.It is right
For those of ordinary skill in the art, can also make on the basis of the above description it is other it is various forms of change or
Change.There is no necessity and possibility to exhaust all the enbodiments.And the obvious change thus extended out or
Among changing still in the protection domain of the invention.
Claims (6)
1. graphene/v2o5 composite material and preparation method thereofs, it is characterised in that：It comprises the following steps：
Step 1: the distilled water for taking constant temperature to be 70 ~ 90 DEG C, weighs some g solids ammonium metavanadates and adds in distilled water and stir extremely
It is completely dissolved；
Step 2: taking some ml graphene dispersing solutions, it meets following ratio：Solid ammonium metavanadate（g）：Graphene dispersing solution
（mg/ml）=5:1~2:1, and be added dropwise under stirring into ammonium metavanadate aqueous solution, and be completely dissolved；
Step 3: taking some ml 40% sulfuric acid solution, it meets following ratio：Solid ammonium metavanadate（g）：Sulfuric acid solution
（ml）=1:1~1:3, and instilled with 1 ~ 5 drop/s speed in the solution after the completion of step 2 reaction, while heating stirring is to life
Precipitated into kermesinus, when kermesinus precipitation is not further added by, stops that sulfuric acid solution is added dropwise and stop heating；
Step 4: continuing the product of whipping step three, and upper strata clear water is separated out, after being cleaned 1 ~ 5 time using distilled water, filtered
Precipitated to kermesinus；
Step 5: by obtained kermesinus precipitation be positioned in vacuum drying chamber at 120 DEG C dry 12h, obtain graphene/
V2O5 compounds；
Step 6: the graphene after drying/V2O5 compounds are calcined into 4 ~ 8 h at 300 ~ 450 DEG C, grinding is then taken out,
Obtain graphene/V2O5 composite powders.
2. graphene according to claim 1/v2o5 composite material and preparation method thereofs, it is characterised in that：In step 1, steaming is taken
Distilled water is contained up in beaker, and then beaker is placed in thermostat water bath, is heated to 70 ~ 90 DEG C, and keeps constant temperature, is then claimed
Take 5 ~ 10 g solid ammonium metavanadate, add in distilled water and magnetic agitation is to being completely dissolved.
3. graphene according to claim 2/v2o5 composite material and preparation method thereofs, it is characterised in that：In step 2, take 1 ~
5 mg/ mL graphene dispersing solutions, and under the conditions of magnetic agitation, it is added dropwise in ammonium metavanadate aqueous solution to being completely dissolved.
4. graphene according to claim 3/v2o5 composite material and preparation method thereofs, it is characterised in that：In step 3, take 5 ~
30 mL 40% (byvolume) sulfuric acid solutions, step 2 is added under heating stirring state with 1 ~ 5 drop/s speed and reacted
In solution after, continue 20min and extremely generate kermesinus precipitation, when kermesinus precipitation is not further added by, it is molten to stop dropwise addition sulfuric acid
Liquid and stopping are heated.
5. graphene according to claim 4/v2o5 composite material and preparation method thereofs, it is characterised in that：In step 6, using horse
Not stove is calcined.
6. anode, it includes aluminium foil, and the positive electrode being covered on aluminium foil, it is characterised in that：The positive electrode
Including graphene/V2O5 combination electrode materials and Kynoar and Super-P, and the two meets mass ratio：Graphene/
V2O5 combination electrode materials：Kynoar and Super-P=80:10, wherein, the graphene/V2O5 combination electrode materials are
Using the made graphene of the method any one of claim 1-5/V2O5 composite powders.
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| Application Number | Priority Date | Filing Date | Title |
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| CN201710924275.8A CN107845775A (en) | 2017-09-30 | 2017-09-30 | Graphene/v2o5 composite material and preparation method thereofs and anode |
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| Application Number | Priority Date | Filing Date | Title |
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| CN201710924275.8A CN107845775A (en) | 2017-09-30 | 2017-09-30 | Graphene/v2o5 composite material and preparation method thereofs and anode |
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| CN107845775A true CN107845775A (en) | 2018-03-27 |
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN109860565A (en) * | 2019-02-25 | 2019-06-07 | 徐霞 | A kind of preparation method of Magnesium ion battery specific complex nanometer vanadium pentoxide |
| CN113036311A (en) * | 2021-03-01 | 2021-06-25 | 同济大学 | Porous carbon ball packaged vanadium oxide heterogeneous core-shell ball structure material, preparation method thereof, lithium-sulfur battery diaphragm and lithium-sulfur battery |
Citations (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN104637701A (en) * | 2015-01-28 | 2015-05-20 | 鲁东大学 | Method for preparing graphene-based vanadium pentoxide nanowire super capacitor electrode material |
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2017
- 2017-09-30 CN CN201710924275.8A patent/CN107845775A/en active Pending
Patent Citations (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN104637701A (en) * | 2015-01-28 | 2015-05-20 | 鲁东大学 | Method for preparing graphene-based vanadium pentoxide nanowire super capacitor electrode material |
Non-Patent Citations (2)
| Title |
|---|
| 李爽: ""石墨烯基锂离子电池复合电极材料的设计合成和电化学性能研究"", 《中国优秀硕士学位论文全文数据库(电子期刊) 工程科技I辑》 * |
| 陈仲等: ""石墨烯/V2O5复合材料的制备及其电化学性能"", 《中国化学会第28届学术年会第10分会场摘要集》 * |
Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN109860565A (en) * | 2019-02-25 | 2019-06-07 | 徐霞 | A kind of preparation method of Magnesium ion battery specific complex nanometer vanadium pentoxide |
| CN113036311A (en) * | 2021-03-01 | 2021-06-25 | 同济大学 | Porous carbon ball packaged vanadium oxide heterogeneous core-shell ball structure material, preparation method thereof, lithium-sulfur battery diaphragm and lithium-sulfur battery |
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