CN103680962A - A metal/ graphene composite current collector and a preparation method and application thereof - Google Patents
A metal/ graphene composite current collector and a preparation method and application thereof Download PDFInfo
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- CN103680962A CN103680962A CN201210361370.9A CN201210361370A CN103680962A CN 103680962 A CN103680962 A CN 103680962A CN 201210361370 A CN201210361370 A CN 201210361370A CN 103680962 A CN103680962 A CN 103680962A
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- Y02E—REDUCTION OF GREENHOUSE GAS [GHG] EMISSIONS, RELATED TO ENERGY GENERATION, TRANSMISSION OR DISTRIBUTION
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- Y02E60/13—Energy storage using capacitors
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Abstract
The invention belongs to composite material field and discloses a metal/ graphene composite current collector and a preparation method and application thereof. The preparation method comprises steps of: preparation of metal precursor/oxidized graphene suspension liquid, preparation of metal/graphene suspension liquid, and preparation of metal/graphene composite material. The metal/ graphene composite current collector is capable of greatly decreasing the weight of a current collector and further increasing the energy density of a super capacitor. Graphene and metal can be both dispersed by using ionic liquid as dispersant so as to obtain uniform dispersed solution. The metal has a strong effect on the graphene so as to enhance the mechanical strength and the conductivity of a graphene film.
Description
Technical field
The present invention relates to field of compound material, relate in particular to a kind of metal/graphite alkene composite current collector.The invention still further relates to the preparation method of metal/graphite alkene composite current collector.The invention still further relates to the application of metal/graphite alkene composite current collector in ultracapacitor.
Background technology
Ultracapacitor is a kind of novel energy storage device, there is the advantages such as high power density (for the more than 10 times of common batteries), high cycle life (cycle-index can reach more than 100,000 times), fast charging and discharging performance are good, be widely used in the AC-battery power source of military field, device for mobile communication, computer and electric automobile etc.Conventionally ultracapacitor mainly by electrode active material layer, electrolyte, assemble every film, collector, shell etc.The energy density of existing ultracapacitor is generally lower, the influencing factor of the energy density of ultracapacitor mainly contains the electric capacity of electrode material, the voltage of system, electrode material accounts for the proportion of the total weight of electrode active material layer, collector, sheathing material composition, therefore, increase the performance that the energy-storage property of electrode material and the weight of each composition material of reduction device can effectively improve device.Wherein, the quality of reduction collector is a method that effectively improves energy density.
Collector is a kind of structure or part that collects electric current, and major function is that the electric current that cell active materials is produced collects, and electron channel is provided, and accelerates electric charge and shifts, and improves and discharges and recharges a coulomb efficiency.As collector, need to meet the features such as conductivity is high, good mechanical property, quality is light, internal resistance is little.
At present, in most document or in industry, anodal aluminium foil, the negative pole of adopting of general collector adopts Copper Foil, because the density of metal collector is larger, quality is heavier, the weight of general collector accounts for the 20-25% of whole battery, and the proportion that electrode material accounts for whole battery greatly reduces, and finally causes the energy density of ultracapacitor lower.
Graphene has good character, the lighter weight of the graphene film of preparing by Graphene, its high mechanical performance and high conductivity also can meet the key property index of collector application simultaneously, therefore based on the prepared graphene film of Graphene, can serve as collector and use, and can reduce the quality of collector.
When the method for directly filtering by graphene suspension is prepared Graphene paper, because it is more difficult to get stable graphene suspension, the Graphene paper that causes it to prepare is even not, arranges irregularity, finally causes mechanical strength, conductivity lower.
Summary of the invention
Problem to be solved by this invention is to provide a kind of mechanical strength and the higher metal/graphite alkene composite current collector of conductivity.
The present invention also provides the preparation method of metal/graphite alkene composite current collector.
The present invention further provides the application of metal/graphite alkene composite current collector in ultracapacitor.
Technical scheme of the present invention is as follows:
A preparation method for metal/graphite alkene composite current collector, comprises the steps:
Graphite oxide is joined in ionic liquid solution, and being configured to concentration is the graphite oxide ionic liquid solution of 0.5 ~ 3mg/ml, and ultrasonic agitation is 0.5 ~ 3 hour subsequently; Then in solution, add metallic precursor, ultrasonic agitation is 0.5 ~ 3 hour again, obtains metallic precursor graphene oxide suspension; Wherein, the mass ratio of graphite oxide and metal precursor is 1:1-5:1;
Described metallic precursor graphene oxide suspension is placed at 180 ~ 200 ℃ of temperature to heat treated 5 ~ 15 minutes, obtains metallic graphite carbon alkene suspension;
To under described metallic graphite carbon alkene suspension vacuum condition, filter, after having filtered, in the water that is 9:1 ~ 5:5 in volume ratio by screening and the mixed solvent of ethanol, soak 2 ~ 5 hours, continue subsequently to filter under vacuum condition, after complete, by the dry processing of screening, obtain described metal/graphite alkene composite current collector.
The preparation method of described metal/graphite alkene composite current collector, wherein, in described ionic liquid solution, the concentration of ionic liquid is 0.5-30mg/ml.
The preparation method of described metal/graphite alkene composite current collector, wherein, in described ionic liquid solution, solute is glyoxaline ion liquid, solvent is DMF, dimethyl sulfoxide (DMSO)), DMA or 1-METHYLPYRROLIDONE.
Described glyoxaline ion liquid comprises 1-ethyl-3-methylimidazole tetrafluoroborate, 1-butyl-3-methyl imidazolium tetrafluoroborate, 1-butyl-3-methylimidazole hexafluorophosphate; 1-cetyl-3-methylimidazole bromine salt, 1-cetyl-3-ethyl imidazol(e) bromine salt, 1-dodecyl-3-methylimidazole bromine salt or 1-decyl-3-methylimidazole bromine salt.
The preparation method of described metal/graphite alkene composite current collector, wherein, described metal is gold or platinum; Described metallic precursor comprises platinum nitrate, chloroplatinic acid or gold chloride.
The preparation method of described metal/graphite alkene composite current collector, wherein, carries out in microwave reactor processing adding of described metallic precursor graphene oxide suspension.
The preparation method of described metal/graphite alkene composite current collector, wherein, the filter paper adopting in filtering under described vacuum condition is miillpore filter.
The preparation method of described metal/graphite alkene composite current collector, wherein, the dry processing of described screening is to carry out in the baking oven of 40 ℃.
The present invention also provides a kind of metal/graphite alkene composite current collector that adopts above-mentioned preparation method to make.
The present invention further provides the application of above-mentioned metal/graphite alkene composite current collector in ultracapacitor.
Metal/graphite alkene composite current collector provided by the invention, compares with traditional Copper Foil, aluminium foil, can greatly reduce the weight of collector, and then improves the energy density of ultracapacitor; Using ionic liquid as dispersant, both can well dispersed graphite alkene, also can dispersed metal, obtain the dispersion soln of homogeneous; Add and the Graphene of metal have stronger effect, can strengthen mechanical strength and the conductivity of graphene film.
Metal/graphite alkene composite current collecting preparation provided by the invention adds metal precursor in graphene oxide, can make metal and graphite oxide disperse more uniformly, and by microwave reduction, method is comparatively simple.
Accompanying drawing explanation
Fig. 1 is preparation technology's flow chart of metal/graphite alkene composite current collector of the present invention.
Embodiment
Metal/graphite alkene composite current collector provided by the invention, as shown in Figure 1, its preparation technology's flow process is as follows:
(1) preparation of metal precursor/graphene oxide suspension:
Take graphite oxide and join in ionic liquid solution, being configured to concentration is the graphene oxide ionic liquid solution of 0.5-3mg/ml, and ultrasonic agitation 0.5-3h, adds metal precursor, ultrasonic agitation 0.5-3h; Wherein:
In described ionic liquid solution, the mass concentration of ionic liquid is 1 ~ 5%;
In described ionic liquid solution, ionic liquid is glyoxaline ion liquid, and this glyoxaline ion liquid comprises: 1-ethyl-3-methylimidazole tetrafluoroborate, 1-butyl-3-methyl imidazolium tetrafluoroborate, 1-butyl-3-methylimidazole hexafluorophosphate; 1-cetyl-3-methylimidazole bromine salt, 1-cetyl-3-ethyl imidazol(e) bromine salt, 1-dodecyl-3-methylimidazole bromine salt or 1-decyl-3-methylimidazole bromine salt; Preferred 1-ethyl-3-methylimidazole tetrafluoroborate, 1-cetyl-3-methylimidazole bromine salt, 1-decyl-3-methylimidazole bromine salt;
Metal is selected gold or platinum, and metal precursor is: platinum nitrate, chloroplatinic acid or gold chloride;
Ionic liquid solution, ionic liquid is solute, DMF (DMF), dimethyl sulfoxide (DMSO) (DMSO), DMA (DMAc) or 1-METHYLPYRROLIDONE (NMP) they are solvent; Ionic liquid is directly added, and its viscosity is larger, easily forms spawn with Graphene, adds the solvent can dissolved ions liquid, and reduction viscosity is also more conducive to mixing of metal precursor and graphene oxide.
The mass ratio of graphite oxide and metal precursor is 1: 1-5:1;
(2) preparation of metal/graphite alkene suspension:
Metal precursor/graphene oxide suspension that (1) is prepared is put into microwave reactor (preferably microwave oven), adjusting makes the power of microwave reach 600-800W, at the temperature of 180 ℃-200 ℃, heat 5-15 minute, obtain homodisperse metal/graphite alkene suspension.
(3) preparation of metal/graphite alkene composite current collector:
Adopt the metal/graphite alkene suspension obtaining in miillpore filter vacuum filtration (2), after filtrate has been filtered, stop vacuum filtration, in funnel, add in the mixed solvent (volume ratio of water and ethanol is 9:1-5:5) of water and ethanol, soak filter cake (comprising miillpore filter and screening) 2-5h, to remove unnecessary ionic liquid solution, in this process, keep solution interface to exceed filter cake; Then continue vacuum filtration 1-5h, after filtration, filter cake is placed in to baking oven in 40 ℃ of oven dry, then screening is taken off from miillpore filter, obtain metal/graphite alkene composite current collector.
Below in conjunction with accompanying drawing, preferred embodiment of the present invention is described in further detail.
Embodiment 1
(1) preparation of platinum presoma/graphene oxide suspension:
Graphite oxide 1g is joined in the DMF solution of 1-ethyl-3-methylimidazole tetrafluoroborate, (wherein the concentration of ionic liquid is 0.5mg/ml, the mass ratio of ionic liquid and graphite oxide is 1:1), being configured to concentration is the graphene oxide ionic liquid mixed solution of 0.5mg/ml, ultrasonic 0.5h, add platinum nitrate 1g, ultrasonic 0.5h, obtains platinum presoma/graphene oxide suspension.
(2) preparation of platinum/graphen suspension:
Platinum presoma/graphene oxide suspension that (1) is prepared is put into microwave oven, regulates and makes the power of microwave reach 600W, heats 15 minutes at the temperature of 180 ℃, obtains homodisperse platinum/graphen suspension.
(3) preparation of platinum/graphen composite current collector:
Adopt the platinum/graphen suspension in miillpore filter vacuum filtration (2), after filtrate has been filtered, stop vacuum filtration, in funnel, add the mixture (ratio of water and ethanol is 9:1) of a certain amount of water and ethanol, soak filter cake 2h, to remove unnecessary ionic liquid, in this process, keep solution interface to exceed filter cake, then continue vacuum filtration 1h, after filtration, filter cake is placed in to baking oven in 40 ℃ of oven dry, then film is taken off from filter membrane, obtained platinum/graphen composite current collector.
Embodiment 2
(1) preparation of platinum presoma/graphene oxide suspension:
Take a certain amount of graphite oxide 2g, join that in the DMSO solution of 1-cetyl-3-methylimidazole bromine salt, (wherein the concentration of ionic liquid is 10mg/ml, the mass ratio of ionic liquid and Graphene is 5:1), being configured to concentration is the graphene oxide ionic liquid mixed solution of 2mg/ml, ultrasonic 1h, add chloroplatinic acid 1g, ultrasonic 1h, platinum presoma/graphene oxide suspension.
(2) preparation of platinum/graphen suspension:
Platinum presoma/graphene oxide suspension that (1) is prepared is put into microwave oven, regulates and makes the power of microwave reach 700W, heats 10 minutes at the temperature of 190 ℃, obtains homodisperse platinum/graphen suspension.
(3) platinum/graphen film preparation:
Adopt the platinum/graphen suspension in miillpore filter vacuum filtration (2), after filtrate has been filtered, stop vacuum filtration, in funnel, add the mixture (ratio of water and ethanol is 4:1) of a certain amount of water and ethanol, soak filter cake 3h, to remove unnecessary ionic liquid, in this process, keep solution interface to exceed filter cake, then continue vacuum filtration 3h, after filtration, filter cake is placed in to baking oven in 40 ℃ of oven dry, then film is taken off from filter membrane, obtained platinum/graphen composite current collector.
Embodiment 3
(1) preparation of golden presoma/graphene oxide suspension:
Take a certain amount of graphite oxide 5g, join that in the nmp solution of 1-decyl-3-methylimidazole bromine salt, (wherein the concentration of ionic liquid is 30mg/ml, the mass ratio of ionic liquid and Graphene is 10:1), being configured to concentration is the graphene oxide ionic liquid mixed solution of 3mg/ml, ultrasonic 3h, add gold chloride 1g, ultrasonic 3h, obtains golden presoma/graphene oxide suspension;
(2) preparation of gold/graphene suspension:
Golden presoma/graphene oxide suspension that (1) is prepared is put into microwave oven, regulates and makes the power of microwave reach 800W, heats 5 minutes at the temperature of 200 ℃, obtains homodisperse gold/graphene suspension.
(3) gold/graphene film preparation:
Adopt the gold/graphene suspension in miillpore filter vacuum filtration (2), after filtrate has been filtered, stop vacuum filtration, in funnel, add the mixture (ratio of water and ethanol is 5:5) of a certain amount of water and ethanol, soak filter cake 5h, to remove unnecessary ionic liquid, in this process, keep solution interface to exceed filter cake, then continue vacuum filtration 5h, after filtration, filter cake is placed in to baking oven in 40 ℃ of oven dry, then film is taken off from filter membrane, obtained gold/Graphene composite current collector.
Followingly be the conductivity of platinum/graphen composite current collector that embodiment 1 is made and pull on strength detection, refer to table 1.
1, the mensuration of conductivity:
Sample is at room temperature used to the two electrical measurement four point probe tester testing conductivities of D41-11D/ZM type.When measuring current is shown as probe coefficient, press electricalresistivityρ's button, screen directly shows that electricalresistivityρ is worth, and according to γ=l/ ρ, directly calculates conductivity.The conductivity of measuring platinum/graphen composite current collector by four probe method is 7.8 * 10
5s/m.
2, hot strength test:
Extension test carries out on dynamic mechanical analyzer (DMA Q800/TA), and sample is cut into 3 * 15mm
2rectangular sheet carry out tension test test.
Hot strength test, the hot strength of platinum/graphen composite current collector is 345.7Mpa, intensity is higher.
Should be understood that, the above-mentioned statement for preferred embodiment of the present invention is comparatively detailed, can not therefore think the restriction to scope of patent protection of the present invention, and scope of patent protection of the present invention should be as the criterion with claims.
Table 1
| Embodiment | Conductivity S/m | Hot strength Mpa |
| 1 | 7.8×10 5 | 345.7 |
| 2 | 7.7×10 5 | 343.2 |
| 3 | 7.5×10 5 | 340.9 |
Claims (10)
1. a preparation method for metal/graphite alkene composite current collector, is characterized in that, comprises the steps:
Graphite oxide is joined in ionic liquid solution, and being configured to concentration is the graphite oxide ionic liquid solution of 0.5 ~ 3mg/ml, and ultrasonic agitation is 0.5 ~ 3 hour subsequently; Then in solution, add metallic precursor, ultrasonic agitation is 0.5 ~ 3 hour again, obtains metallic precursor graphene oxide suspension; Wherein, the mass ratio of graphite oxide and metal precursor is 1:1-5:1;
Described metallic precursor graphene oxide suspension is placed at 180 ~ 200 temperature to heat treated 5 ~ 15 minutes, obtains metallic graphite carbon alkene suspension;
To under described metallic graphite carbon alkene suspension vacuum condition, filter, after having filtered, in the water that is 9:1 ~ 5:5 in volume ratio by screening and the mixed solvent of ethanol, soak 2 ~ 5 hours, continue subsequently to filter under vacuum condition, after complete, by the dry processing of screening, obtain described metal/graphite alkene composite current collector.
2. the preparation method of metal/graphite alkene composite current collector according to claim 1, is characterized in that, in described ionic liquid solution, the concentration of ionic liquid is 0.5 ~ 30mg/ml.
3. the preparation method of metal/graphite alkene composite current collector according to claim 1 and 2, is characterized in that, in described ionic liquid solution, solute is glyoxaline ion liquid, solvent is DMF, dimethyl sulfoxide (DMSO), DMA or 1-METHYLPYRROLIDONE.
4. the preparation method of metal/graphite alkene composite current collector according to claim 3, it is characterized in that, described glyoxaline ion liquid comprises 1-ethyl-3-methylimidazole tetrafluoroborate, 1-butyl-3-methyl imidazolium tetrafluoroborate, 1-butyl-3-methylimidazole hexafluorophosphate; 1-cetyl-3-methylimidazole bromine salt, 1-cetyl-3-ethyl imidazol(e) bromine salt, 1-dodecyl-3-methylimidazole bromine salt or 1-decyl-3-methylimidazole bromine salt.
5. the preparation method of metal/graphite alkene composite current collector according to claim 1, is characterized in that, described metal is gold or platinum; Described metallic precursor comprises platinum nitrate, chloroplatinic acid or gold chloride.
6. the preparation method of metal/graphite alkene composite current collector according to claim 1, is characterized in that, to processing adding of described metallic precursor graphene oxide suspension, in microwave reactor, carries out.
7. the preparation method of metal/graphite alkene composite current collector according to claim 1, is characterized in that, the filter paper adopting in filtering under described vacuum condition is miillpore filter.
8. the preparation method of metal/graphite alkene composite current collector according to claim 1, is characterized in that, the dry processing of described screening is to carry out in the baking oven of 40 ℃.
9. a metal/graphite alkene composite current collector, is characterized in that, this composite current collector adopts the arbitrary described preparation method of claim 1 to 8 to make.
10. the application of metal/graphite alkene composite current collector in ultracapacitor described in claim 9.
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Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
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| KR101617955B1 (en) | 2014-08-22 | 2016-05-03 | 영남대학교 산학협력단 | - Synthetic method for graphene SnO nanocomposites |
| CN108682876A (en) * | 2018-06-04 | 2018-10-19 | 黑龙江省科学院石油化学研究院 | A kind of high activity has the cube nano Pd catalyst and preparation method thereof of meso-hole structure |
| CN109187678A (en) * | 2018-07-11 | 2019-01-11 | 杭州电子科技大学 | Utilize the nitrite detection device of nanogold graphene modified electrochemical method |
| CN111116410A (en) * | 2020-01-12 | 2020-05-08 | 浙江锦华新材料股份有限公司 | Preparation method of butanone oxime |
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Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
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| KR101617955B1 (en) | 2014-08-22 | 2016-05-03 | 영남대학교 산학협력단 | - Synthetic method for graphene SnO nanocomposites |
| CN108682876A (en) * | 2018-06-04 | 2018-10-19 | 黑龙江省科学院石油化学研究院 | A kind of high activity has the cube nano Pd catalyst and preparation method thereof of meso-hole structure |
| CN109187678A (en) * | 2018-07-11 | 2019-01-11 | 杭州电子科技大学 | Utilize the nitrite detection device of nanogold graphene modified electrochemical method |
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Application publication date: 20140326 |