CN104064367A - Nitrogen doped carbon nanotube/ionic liquid composite film and preparation method thereof, and capacitor - Google Patents
Nitrogen doped carbon nanotube/ionic liquid composite film and preparation method thereof, and capacitor Download PDFInfo
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Abstract
The invention relates to a nitrogen doped carbon nanotube/ionic liquid composite film and a preparation method thereof. The preparation method comprises the following steps: (a), preparing a nitrogen doped carbon nanotube; and (b), preparing the nitrogen doped carbon nanotube/ionic liquid composite film. The invention further comprises an application of the nitrogen doped carbon nanotube/ionic liquid composite film in a capacitor. The content of nitrogen in the prepared nitrogen doped carbon nanotube/ionic liquid composite film is quite high, such that when the nitrogen doped carbon nanotube/ionic liquid composite film is used as the electrode material of the capacitor, the energy storage performance is excellent, the employed preparation method, equipment and process are simple, and large scale production is easily realized.
Description
Technical field
The present invention relates to chemical material preparation field, relate in particular to a kind of nitrogen-doped carbon nanometer pipe/ionic liquid laminated film and preparation method thereof.The invention still further relates to this application of nitrogen-doped carbon nanometer pipe/ionic liquid laminated film in capacitor.
Background technology
Nineteen nineties, material with carbon element has promoted greatly developing of ultracapacitor, lithium ion battery as the use of energy storage material.And carbon nano-tube is as a kind of material with carbon element of one dimension, there is very high conductivity, and the very easy derivatization of carbon nano-tube, its derivative is also subject to researcher's extensive concern.
Carbon nano tube derivative mainly contains nitrogen-doped carbon nanometer pipe and boron doped carbon nanometer pipe at present.Wherein nitrogen doping, due to the many electronics of boron atom ratio carbon atom skin, is the doping of N-type, have better energy-storage property, and the nitrogen content of nitrogen-doped carbon nanometer pipe is higher so compare carbon nano-tube, and energy storage site is more, and energy-storage property is also just better.At present, the larger problem that carbon nano-tube application runs into, easily reunites, and this has reduced the energy-storage property of carbon nano-tube to a certain extent.Therefore, the reunion of the quantity in increase carbon nano-tube energy storage site and reduction carbon nano-tube just seems very important.
Summary of the invention
The object of the invention is to solve the problem and shortage that above-mentioned prior art exists, a kind of nitrogen-doped carbon nanometer pipe/ionic liquid laminated film is provided, utilize the higher nitrogen content of this nitrogen-doped carbon nanometer pipe/ionic liquid laminated film, while making this nitrogen-doped carbon nanometer pipe/ionic liquid laminated film be used as the electrode material of capacitor, there is excellent energy-storage property.
The technical scheme that the present invention is directed to above-mentioned technical problem and propose is: a kind of preparation method of nitrogen-doped carbon nanometer pipe/ionic liquid laminated film, comprises the steps:
(a) carbon nano-tube and nitrating agent are mixed and are placed in reactor in 1:0.5～3 in mass ratio, dry after fully stirring, in described reactor, pass into inert gas subsequently, make to form inert environments in described reactor, then be warming up to 750～900 ℃, keep being down to room temperature after 1～2h, the solid product of gained is cleaned and is dried, obtain described nitrogen-doped carbon nanometer pipe;
(b) prepare nitrogen-doped carbon nanometer pipe/ionic liquid laminated film: described nitrogen-doped carbon nanometer pipe is placed in to ionic liquid, be configured to the mixed solution that concentration is 20mg/ml, ultrasonic after mixing, again mixed solution is placed under vacuum environment dry, then suction filtration goes out unnecessary described ionic liquid, obtains nitrogen-doped carbon nanometer pipe/ionic liquid laminated film; Wherein, brace "/" represents compound.
Described nitrating agent is ammoniacal liquor or urea.
In described step (a), the time of described stirring is 4～8h, and described stirring afterwards dry temperature is 60 ℃, and dry time is 12h afterwards in described stirring.
Described inert gas is argon gas, nitrogen or helium, and flow velocity when described inert gas passes into is 400ml/min.
Temperature-rise period, its heating rate is 5～20 ℃/min.
As follows to the cleaning of described solid product dry operation: described solid product is placed in to HCl solution by mass volume ratio 20mg:1ml, stir suction filtration after 2 hours, with solid product described in washed with de-ionized water to pH value, be neutral again, finally described solid product be placed in to the dry 12h of 60 ℃ of baking ovens.
Described ionic liquid is the two fluoroform sulfimide salt of 1-ethyl-3-methylimidazole, 1-ethyl-3-methylimidazole hexafluorophosphate, the two fluoroform sulfimide salt of 1-butyl-3-methylimidazole or 1-butyl-3-methylimidazole hexafluorophosphate.
In described step (b), described ultrasonic time is 2h, and described mixture is to process 24h under the described vacuum environment of 100 ℃.
The present invention also comprises the nitrogen-doped carbon nanometer pipe/ionic liquid laminated film that utilizes above-mentioned preparation method to make.
The present invention also comprises the application of described nitrogen-doped carbon nanometer pipe/ionic liquid laminated film in capacitor.This capacitor comprise by electrode film, barrier film, negative electrode plate in order the stacked battery core forming, for installing the closed shell of described battery core, and annotate at the electrolyte of closed shell, described electrode film and negative electrode plate are made by described nitrogen-doped carbon nanometer pipe/ionic liquid laminated film.
Compared with prior art, nitrogen-doped carbon nanometer pipe/ionic liquid laminated film of the present invention and preparation method thereof, there is following advantage: the nitrogen content of inventing prepared nitrogen-doped carbon nanometer pipe/ionic liquid laminated film is higher, nitrogen-doped carbon nanometer pipe and ionic liquid compound, reduced the reunion of nitrogen-doped carbon nanometer pipe, improve the wettability of nitrogen-doped carbon nanometer pipe to electrolyte simultaneously, thereby while making this nitrogen-doped carbon nanometer pipe/ionic liquid laminated film be used as the electrode material of capacitor, there is excellent energy-storage property, and the preparation method's equipment adopting, technique is simple, easily realize large-scale production.
Embodiment
Below in conjunction with embodiment, the present invention is given to elaboration further.
Nitrogen-doped carbon nanometer pipe/Ionic Liquid Films preparation technology flow process of the present invention is as follows:
Carbon nano-tube → nitrogen-doped carbon nanometer pipe → nitrogen-doped carbon nanometer pipe/Ionic Liquid Films.
Specifically be divided into following steps:
(a) carbon nano-tube that is 99% by purity and nitrating agent in mass ratio 1:0.5～3 mix and are placed in reactor, fully stir after 4～8h vacuumize 12h at 60 ℃, in reactor, pass into the inert gas that flow velocity is 400ml/min subsequently, make to form in reactor inert environments, then the heating rate with 5～20 ℃/min is warming up to 750～900 ℃, keep being down to room temperature after 1～2h, solid product is placed in to HCl solution by mass volume ratio 20mg:1ml, stir suction filtration after 2 hours, the solid product obtaining is placed in again to the HCl solution of the mass fraction 3.6% of same volume, stir 2 hours, suction filtration, with deionized water, wash solid product to pH value and be neutral, finally be placed in the dry 12h of 60 ℃ of baking ovens, obtain nitrogen-doped carbon nanometer pipe,
(b) described nitrogen-doped carbon nanometer pipe is placed in to ionic liquid, be configured to the mixed solution that concentration is 20mg/ml, ultrasonic 2h after mixing, again mixed solution is placed under the vacuum environment of 100 ℃ and processes 24h, suction filtration goes out after unnecessary ionic liquid, obtains nitrogen-doped carbon nanometer pipe/ionic liquid laminated film.
Wherein, nitrating agent is ammoniacal liquor or urea.Inert gas is argon gas, nitrogen or helium.Ionic liquid is a kind of in the two fluoroform sulfimide salt of 1-ethyl-3-methylimidazole, 1-ethyl-3-methylimidazole hexafluorophosphate, the two fluoroform sulfimide salt of 1-butyl-3-methylimidazole or 1-butyl-3-methylimidazole hexafluorophosphate.Reactor is not limited, be preferably test tube.
The present invention also comprises the nitrogen-doped carbon nanometer pipe/ionic liquid laminated film that utilizes above-mentioned preparation method to make.
Nitrogen-doped carbon nanometer pipe/ionic liquid laminated film of the present invention can be used as the electrode material of capacitor, and concrete manufacture method is as follows:
1, nitrogen-doped carbon nanometer pipe/ionic liquid laminated film is dried to 2 hours at 80 ℃, then is dried slicing treatment after 2 hours at 250 ℃, make the electrode slice of capacitor;
2, by nitrogen-doped carbon nanometer pipe/ionic liquid composite film electrode sheet, barrier film, nitrogen-doped carbon nanometer pipe/ionic liquid composite film electrode sheet in order stack of laminations dress up battery core, use again battery housing seal battery core, toward the liquid injection port being arranged on battery container, in battery container, inject electrolyte subsequently, this electrolyte is ionic liquid, it is identical with the ionic liquid of preparing nitrogen-doped carbon nanometer pipe/ionic liquid laminated film, after sealing liquid injection port, obtains capacitor.
Preparation process with 1～4 pair of nitrogen-doped carbon nanometer pipe/ionic liquid laminated film of the present invention of embodiment is specifically described below:
Embodiment 1
1, the carbon nano-tube that is 99% by purity joins in the test tube of the ethanolic solution that is dissolved with urea (solubility of carbon nano-tube is 10mg/ml), the mass ratio of carbon nano-tube and urea is 1:1, under room temperature, mixture is stirred 4 hours, and mixture is placed in to dry 12 hours of the vacuum drying oven of 60 ℃, it is the argon gas of 400ml/ minute that dried mixture is passed into flow, make to form in test tube argon gas atmosphere, with the heating rates of 10 ℃/min, make the ambient temperature of mixture rise to 800 ℃ from room temperature, and keep 2 hours, then under being the argon atmosphere of 400ml/ minute, flow is naturally down to room temperature, reacted mixture is placed in to the HCl solution (mass volume ratio of mixture and HCl is 1mg:1ml) of mass fraction 3.6%, stir 2 hours, suction filtration, the solid product obtaining is placed in again to the HCl solution of the mass fraction 3.6% of same volume, stir 2 hours, suction filtration, with deionized water, wash solid product to pH value and be neutral, finally be placed in the dry 12h of 60 ℃ of baking ovens, obtain nitrogen-doped graphene,
2, nitrogen-doped carbon nanometer pipe is placed in to the two fluoroform sulfimide salt of 1-ethyl-3-methylimidazole and (is abbreviated as [EMIM] [Tf
2n]) ionic liquid in, be configured to the mixed solution that concentration is 20mg/ml, ultrasonic 2 hours, then mixed solution be placed under the vacuum environment of 100 ℃ and process 24 hours, finally unnecessary ionic liquid suction filtration is removed, obtained nitrogen-doped carbon nanometer pipe/ionic liquid laminated film.
Embodiment 2
1, the carbon nano-tube that is 99% by purity joins in the test tube of the ethanolic solution that is dissolved with ammoniacal liquor (solubility of carbon nano-tube is 5mg/ml), the mass ratio of carbon nano-tube and ammoniacal liquor is 1:2, to mixture being stirred 6 hours under room temperature, and mixture is placed in to dry 12 hours of the vacuum drying oven of 60 ℃, it is the nitrogen of 400ml/ minute that dried mixture is passed into flow, make to form in test tube nitrogen atmosphere, with the heating rates of 15 ℃/min, make the ambient temperature of mixture rise to 900 ℃ from room temperature, and keep 1 hour, then under being the nitrogen atmosphere of 400ml/ minute, flow is naturally down to room temperature, reacted mixture is placed in to the HCl solution (mass volume ratio of mixture and HCl is 1mg:1ml) of mass fraction 3.6%, stir 2 hours, suction filtration, the solid product obtaining is placed in again to the HCl solution of the mass fraction 3.6% of same volume, stir 2 hours, suction filtration, with deionized water, wash solid product to pH value and be neutral, finally be placed in the dry 12h of 60 ℃ of baking ovens, obtain nitrogen-doped graphene,
2, nitrogen-doped carbon nanometer pipe is placed in to 1-ethyl-3-methylimidazole hexafluorophosphate and (is abbreviated as [EMIM] [PF
6]) ionic liquid in, be configured to the mixed solution that concentration is 20mg/ml, ultrasonic 2 hours, then mixed solution be placed under the vacuum environment of 100 ℃ and process 24 hours, finally unnecessary ionic liquid suction filtration is removed, obtained nitrogen-doped carbon nanometer pipe/ionic liquid laminated film.
Embodiment 3
1, the carbon nano-tube that is 99% by purity joins in the test tube of the ethanolic solution that is dissolved with ammoniacal liquor (solubility of carbon nano-tube is 10mg/ml), the mass ratio of carbon nano-tube and ammoniacal liquor is 1:3, under room temperature, mixture is stirred 4 hours, and mixture is placed in to dry 12 hours of the vacuum drying oven of 60 ℃, it is the helium of 400ml/ minute that dried mixture is passed into flow, make to form in test tube helium atmosphere, make to form in reactor inert environments, with the heating rates of 5 ℃/min, make the ambient temperature of mixture rise to 850 ℃ from room temperature, and keep 1 hour, then under being the helium atmosphere of 400ml/ minute, flow is naturally down to room temperature, reacted mixture is placed in to the HCl solution (mass volume ratio of mixture and HCl is 1mg:1ml) of mass fraction 3.6%, stir 2 hours, suction filtration, the solid product obtaining is placed in again to the HCl solution of the mass fraction 3.6% of same volume, stir 2 hours, suction filtration, with deionized water, wash solid product to pH value and be neutral, finally be placed in the dry 12h of 60 ℃ of baking ovens, obtain nitrogen-doped graphene,
2, nitrogen-doped carbon nanometer pipe is placed in to the two fluoroform sulfimide salt of 1-butyl-3-methylimidazole and (is abbreviated as [BMIM] [Tf
2n]) in ionic liquid, be configured to the mixed solution that concentration is 20mg/ml, ultrasonic 2 hours, then mixed solution be placed under the vacuum environment of 100 ℃ and process 24 hours, finally unnecessary ionic liquid suction filtration is removed, obtained nitrogen-doped carbon nanometer pipe/ionic liquid laminated film.
Embodiment 4
1, the carbon nano-tube that is 99% by purity joins in the test tube of the ethanolic solution that is dissolved with urea (solubility of carbon nano-tube is 20mg/ml), the mass ratio of carbon nano-tube and urea is 2:1, under room temperature, mixture is stirred 8 hours, and mixture is placed in to dry 12 hours of the vacuum drying oven of 60 ℃, it is the argon gas of 400ml/ minute that dried mixture is passed into flow, make to form in test tube argon gas atmosphere, with the heating rates of 20 ℃/min, make the ambient temperature of mixture rise to 750 ℃ from room temperature, and keep 2 hours, then under being the nitrogen atmosphere of 400ml/ minute, flow is naturally down to room temperature, reacted mixture is placed in to the HCl solution (mass volume ratio of mixture and HCl is 1mg:1ml) of mass fraction 3.6%, stir 2 hours, suction filtration, the solid product obtaining is placed in again to the HCl solution of the mass fraction 3.6% of same volume, stir 2 hours, suction filtration, with washed with de-ionized water solid product to pH value, be neutral, finally be placed in the dry 12h of 60 ℃ of baking ovens, obtain nitrogen-doped graphene,
2, nitrogen-doped carbon nanometer pipe is placed in to 1-butyl-3-methylimidazole hexafluorophosphate and (is abbreviated as [BMIM] [PF
6]) in ionic liquid, be configured to the mixed solution that concentration is 20mg/ml, ultrasonic 2 hours, then mixed solution be placed under the vacuum environment of 100 ℃ and process 24 hours, finally unnecessary ionic liquid suction filtration is removed, obtained nitrogen-doped carbon nanometer pipe/ionic liquid laminated film.
Following table 1 is the determination data of each essential element content of nitrogen-doped carbon nanometer pipe/ionic liquid laminated film of embodiment 1～4 preparation.
Table 1
| Carbon (%) | Nitrogen element (%) | Oxygen element (%) | |
| Embodiment 1 | 84.2 | 8.6 | 6.4 |
| Embodiment 2 | 83 | 9.6 | 5.8 |
| Embodiment 3 | 82.4 | 10.6 | 6.1 |
| Embodiment 4 | 81.5 | 11.8 | 7.2 |
Data from above table are known, and the nitrogen content of nitrogen-doped carbon nanometer pipe/ionic liquid laminated film that the present invention is prepared is higher, all, more than 8%, is up to 11.8%.
The preparation of capacitor
Embodiment 5 to 8 is respectively and adopts nitrogen-doped carbon nanometer pipe/ionic liquid laminated film of embodiment 1 to 4 preparation to prepare the concrete steps in capacitor:
Embodiment 5
1, the nitrogen-doped carbon nanometer pipe/ionic liquid laminated film obtaining in embodiment 1 is placed at 80 ℃ and is dried 2 hours, cut into slices, make the electrode slice of capacitor;
2, by nitrogen-doped carbon nanometer pipe/ionic liquid laminated film, barrier film, nitrogen-doped carbon nanometer pipe/ionic liquid laminated film in order stack of laminations dress up battery core, use again battery housing seal battery core, toward being arranged on liquid injection port on battery container, toward injecting the two fluoroform sulfimide salt of 1-ethyl-3-methylimidazole in battery container, (be abbreviated as [EMIM] [Tf subsequently
2n]), after sealing liquid injection port, obtain capacitor.
Embodiment 6
1, the nitrogen-doped carbon nanometer pipe/ionic liquid laminated film obtaining in embodiment 2 is placed at 80 ℃ and is dried 2 hours, cut into slices, make the electrode slice of capacitor;
2, by nitrogen-doped carbon nanometer pipe/ionic liquid laminated film, barrier film, nitrogen-doped carbon nanometer pipe/ionic liquid laminated film in order stack of laminations dress up battery core, use again battery housing seal battery core, toward being arranged on liquid injection port on battery container, toward injecting 1-ethyl-3-methylimidazole hexafluorophosphate in battery container, (be abbreviated as [EMIM] [PF subsequently
6]), after sealing liquid injection port, obtain capacitor.
Embodiment 7
1, the nitrogen-doped carbon nanometer pipe/ionic liquid laminated film obtaining in embodiment 3 is placed at 80 ℃ and is dried 2 hours, cut into slices, make the electrode slice of capacitor;
2, by nitrogen-doped carbon nanometer pipe/ionic liquid laminated film, barrier film, nitrogen-doped carbon nanometer pipe/ionic liquid laminated film in order stack of laminations dress up battery core, use again battery housing seal battery core, toward being arranged on liquid injection port on battery container, toward injecting the two fluoroform sulfimide salt of 1-butyl-3-methylimidazole in battery container, (be abbreviated as [BMIM] [Tf subsequently
2n]), after sealing liquid injection port, obtain capacitor.
Embodiment 8
1, the nitrogen-doped carbon nanometer pipe/ionic liquid laminated film obtaining in embodiment 4 is placed at 80 ℃ and is dried 2 hours, cut into slices, make the electrode slice of capacitor;
2, by nitrogen-doped carbon nanometer pipe/ionic liquid laminated film, barrier film, nitrogen-doped carbon nanometer pipe/ionic liquid laminated film in order stack of laminations dress up battery core, use again battery housing seal battery core, toward being arranged on liquid injection port on battery container, toward injecting 1-butyl-3-methylimidazole hexafluorophosphate in battery container, (be abbreviated as [BMIM] [PF subsequently
6]), after sealing liquid injection port, obtain capacitor.
To nitrogen-doped carbon nanometer pipe/ionic liquid laminated film of the present invention in above-described embodiment 5～8, for the carrying out after capacitor, voltage window is 4V.Table 2 carries out the specific capacity of charge-discharge test for capacitor under 1A/g electric current:
Table 2
| Specific capacity (F/g) | |
| Embodiment 5 | 212 |
| Embodiment 6 | 226 |
| Embodiment 7 | 241 |
| Embodiment 8 | 257 |
From table 2 data, draw, under 1A/g current density, the specific capacity of each capacitor all, more than 210F/g, is up to 257F/g, all has excellent energy-storage property.
From above test data, can find out, the nitrogen content of nitrogen-doped carbon nanometer pipe/ionic liquid laminated film that the present invention is prepared is higher, nitrogen-doped carbon nanometer pipe and ionic liquid compound, reduced the reunion of nitrogen-doped carbon nanometer pipe, improve the wettability of nitrogen-doped carbon nanometer pipe to electrolyte simultaneously, thereby while making this nitrogen-doped carbon nanometer pipe/ionic liquid laminated film be used as the electrode material of capacitor, there is excellent energy-storage property, and the preparation method's equipment, the technique that adopt are simple, easily realize large-scale production.
Foregoing; it is only preferred embodiment of the present invention; not for limiting embodiment of the present invention; those of ordinary skills are according to main design of the present invention and spirit; can carry out very easily corresponding flexible or modification, therefore protection scope of the present invention should be as the criterion with the desired protection range of claims.
Claims (10)
1. a preparation method for nitrogen-doped carbon nanometer pipe/ionic liquid laminated film, is characterized in that, comprises the steps:
(a) prepare nitrogen-doped carbon nanometer pipe: carbon nano-tube and nitrating agent are mixed and are placed in reactor in 1:0.5 ~ 3 in mass ratio, dry after fully stirring, in described reactor, pass into inert gas subsequently, make to form inert environments in described reactor, then be warming up to 750 ~ 900 ℃, keep being down to room temperature after 1 ~ 2h, the solid product of gained is cleaned and is dried, obtain described nitrogen-doped carbon nanometer pipe;
(b) prepare nitrogen-doped carbon nanometer pipe/ionic liquid laminated film: described nitrogen-doped carbon nanometer pipe is placed in to ionic liquid, be configured to the mixed solution that concentration is 20mg/ml, ultrasonic after mixing, again mixed solution is placed under vacuum environment dry, then suction filtration goes out unnecessary described ionic liquid, obtains nitrogen-doped carbon nanometer pipe/ionic liquid laminated film.
2. preparation method according to claim 1, is characterized in that, described nitrating agent is ammoniacal liquor or urea.
3. preparation method according to claim 1, is characterized in that, in described step (a), the time of described stirring is 4 ~ 8h, and described stirring afterwards dry temperature is 60 ℃, and dry time is 12h afterwards in described stirring.
4. preparation method according to claim 1, is characterized in that, described inert gas is argon gas, nitrogen or helium, and flow velocity when described inert gas passes into is 400ml/min.
5. preparation method according to claim 1, is characterized in that, temperature-rise period, and its heating rate is 5 ~ 20 ℃/min.
6. preparation method according to claim 1, it is characterized in that, as follows to the cleaning of described solid product dry operation: described solid product is placed in to HCl solution by mass volume ratio 20mg:1ml, stir suction filtration after 2 hours, with solid product described in washed with de-ionized water to pH value, be neutral again, be finally placed in the dry 12h of 60 ℃ of baking ovens.
7. preparation method according to claim 1, it is characterized in that, described ionic liquid is the two fluoroform sulfimide salt of 1-ethyl-3-methylimidazole, 1-ethyl-3-methylimidazole hexafluorophosphate, the two fluoroform sulfimide salt of 1-butyl-3-methylimidazole or 1-butyl-3-methylimidazole hexafluorophosphate.
8. preparation method according to claim 1, is characterized in that, in described step (b), described ultrasonic time is 2h, and described mixture is to process 24h under the described vacuum environment of 100 ℃.
9. nitrogen-doped carbon nanometer pipe/ionic liquid laminated film that the arbitrary described preparation method of a claim 1 to 8 makes.
10. a capacitor, comprise by electrode film, barrier film, negative electrode plate in order the stacked battery core forming, for installing the closed shell of described battery core, and filling is at the electrolyte of closed shell, it is characterized in that, described electrode film and negative electrode plate are made by nitrogen-doped carbon nanometer pipe/ionic liquid laminated film claimed in claim 9.
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