CN106449183A - Preparation method of carbon nanotube-based supercapacitor electrode material - Google Patents
Preparation method of carbon nanotube-based supercapacitor electrode material Download PDFInfo
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- CN106449183A CN106449183A CN201611177570.3A CN201611177570A CN106449183A CN 106449183 A CN106449183 A CN 106449183A CN 201611177570 A CN201611177570 A CN 201611177570A CN 106449183 A CN106449183 A CN 106449183A
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- electrode material
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- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01G—CAPACITORS; CAPACITORS, RECTIFIERS, DETECTORS, SWITCHING DEVICES OR LIGHT-SENSITIVE DEVICES, OF THE ELECTROLYTIC TYPE
- H01G11/00—Hybrid capacitors, i.e. capacitors having different positive and negative electrodes; Electric double-layer [EDL] capacitors; Processes for the manufacture thereof or of parts thereof
- H01G11/84—Processes for the manufacture of hybrid or EDL capacitors, or components thereof
- H01G11/86—Processes for the manufacture of hybrid or EDL capacitors, or components thereof specially adapted for electrodes
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- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01G—CAPACITORS; CAPACITORS, RECTIFIERS, DETECTORS, SWITCHING DEVICES OR LIGHT-SENSITIVE DEVICES, OF THE ELECTROLYTIC TYPE
- H01G11/00—Hybrid capacitors, i.e. capacitors having different positive and negative electrodes; Electric double-layer [EDL] capacitors; Processes for the manufacture thereof or of parts thereof
- H01G11/22—Electrodes
- H01G11/30—Electrodes characterised by their material
- H01G11/32—Carbon-based
- H01G11/36—Nanostructures, e.g. nanofibres, nanotubes or fullerenes
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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
- Y02E60/13—Energy storage using capacitors
Abstract
The invention discloses a preparation method of a carbon nanotube-based supercapacitor electrode material. The preparation method comprises the following steps: refluxing carbon nanotubes in a mixed solution of nitric acid and sulfuric acid at the refluxing temperature of 70-100 DEG C for longer than 2 hours; centrifugally washing the pickled carbon nano-tubes with deionized water until pH of supernatant is equal to 7; re-dispersing the washed carbon nanotubes in the deionized water, and adding a surfactant to obtain carbon nanotube turbid liquid; adding thiourea and easily dissolved bivalent copper salts in the carbon nanotube turbid liquid, and stirring evenly; transferring the liquid into a hydrothermal reactor, carrying out temperature programming to the temperature of 160 DEG C from the room temperature, and reacting for 6-10 hours at the temperature of 160 DEG C; and filtering, washing, drying and roasting to obtain the carbon nanotube-based supercapacitor electrode material. The carbon nanotube-based supercapacitor electrode material has good electrochemical performance.
Description
Technical field
The present invention relates to electrode material field, and in particular to a kind of preparation of CNT based super capacitor electrode material
Method.
Background technology
The core parts of ultracapacitor are electrodes.At present, super capacitor anode material is mainly Carbon Materials, commercialization
The negative pole Carbon Materials for using are mainly graphite.The aperture of porous carbon material typically wants 2nm and above space form double electricity
Layer, so as to carry out effective energy storage.The surface functional group of Carbon Materials, conductivity, apparent density etc. are to capacitor performance
Have an impact.And CNT possesses that degree of crystallinity height, good conductivity, specific surface area be big, aperture concentrate within the specific limits and controlled
Advantageous characteristic, be a kind of preferable electrode material for super capacitor, await exploring preferably preparation method for improving
The ratio electric capacity of ultracapacitor.
Content of the invention
It is an object of the invention to provide a kind of preparation method of CNT based super capacitor electrode material, obtains tool
The ultracapacitor having compared with high specific capacitance.
Technical scheme is as follows：
A kind of preparation method of CNT based super capacitor electrode material, comprises the following steps：
(1) CNT is carried out in the mixed solution of nitric acid and sulphuric acid under 70 DEG C～100 DEG C of reflux temperature big
Reflux operation in 2h；
(2) CNT after the pickling of deionized water centrifuge washing is until supernatant pH=7；
(3) CNT after washing is scattered in deionized water again, and adds surfactant to obtain CNT
Suspension；
(4) thiourea and readily soluble cupric salt are added in above-mentioned carbon nanotube suspension, stirs；
(5) above-mentioned solution being transferred in water heating kettle from room temperature and temperature programming is proceeded by 160 DEG C, is kept for 160 DEG C instead
Answer 6h～10h；
(6) filter, washing, dry, after roasting CNT based super capacitor electrode material.
Step (1) is used for residue in the removal of intraluminal catalyst in CNT preparation process and in CNT table
Face is introduced into hydroxyl and carboxyl oxy radical to improve its dispersibility in water.The addition of surfactant is conducive to CNT
Dispersed.Thiourea can generate the CuS of electro-chemical activity as sulphur source and bivalent cupric ion combination.Choosing in step (5)
Select and react in water heating kettle, be that being fed with of high-energy is beneficial to due to accelerating the carrying out that reacts in the environment of High Temperature High Pressure
Reactant is promoted to cross reaction energy barrier, and then the chemical reaction for occurring to carry out at ambient pressure.
Wherein, described in step (1) in nitric acid and the mixed solution of sulphuric acid, the concentration of nitric acid is the dense of 5mol/L, sulphuric acid
Spend for 3mol/L.Nitric acid and sulphuric acid under this concentration is concentrated sulphuric acid and concentrated nitric acid, is conducive in CNT table in reflux course
Face introduces oxy radical.
Preferably, reflux temperature described in step (1) is 80 DEG C, and return time is 3h.
Wherein, surfactant described in step (3) is cationic surfactant or anion surfactant.
Wherein, the cationic surfactant is Cetyltrimethylammonium bromide, the anion surfactant
For sodium lauryl sulphate.
Wherein, readily soluble cupric salt described in step (4) is copper chloride or copper nitrate.
Preferably, the speed of temperature programming described in step (5) is 2 DEG C/min.Suitable heating rate is conducive to control
The speed of chemical reaction, it is to avoid reaction is excessively fierce.
Preferably, the temperature of roasting described in step (6) is 350 DEG C.The selection of this temperature is the impurity such as foundation copper nitrate
Decomposition temperature set.
The present invention compared with prior art, has the following advantages and advantages：CNT base in the present invention surpasses
Level capacitor electrode material has good chemical property, and wherein, under conditions of embodiment 4, resulting materials in scanning speed are
Ratio electric capacity during 5mV/s is 600F/g.
Specific embodiment
For making the object, technical solutions and advantages of the present invention become more apparent, with reference to embodiment, the present invention is made
Further detailed description, the exemplary embodiment of the present invention and its explanation are only used for explaining the present invention, are not intended as to this
The restriction of invention.
Embodiment 1
A kind of preparation method of CNT based super capacitor electrode material, comprises the following steps：By 10g CNT
Flow back in the nitric acid of 5mol/L and the mixed solution of the sulphuric acid composition of 3mol/L under 70 DEG C of reflux temperature 3.5h；Spend from
CNT after sub- water centrifuge washing pickling is until supernatant pH=7；CNT after washing is scattered in 200mL again
In deionized water, and 0.785g cationic surfactant Cetyltrimethylammonium bromide is added to obtain carbon nanotube suspension；
By 7.612g thiourea and 24.156g Cu (NO3)2·3H2O is added in above-mentioned carbon nanotube suspension, is stirred；Will be above-mentioned molten
Liquid is transferred in the water heating kettle of 250mL and starts to be warming up to 160 DEG C with the rate program of 2 DEG C/min from room temperature, keeps 160 DEG C of reactions
10h；After the completion of reaction, natural cooling is cooled to room temperature, filters, washs, dries and obtains CNT base after roasting at 350 DEG C
Electrode material for super capacitor.
Electrochemical property test is carried out to this capacitor, electrolyte used is the KOH solution of 6mol/L, measure in scanning speed
It is 500F/g to spend for ratio electric capacity during 5mV/s.
Embodiment 2
A kind of preparation method of CNT based super capacitor electrode material, comprises the following steps：By 10g CNT
Flow back in the nitric acid of 5mol/L and the mixed solution of the sulphuric acid composition of 3mol/L under 80 DEG C of reflux temperature 3h；Use deionization
CNT after water centrifuge washing pickling is until supernatant pH=7；CNT after washing is scattered in 200mL again
In ionized water, and 0.785g cationic surfactant Cetyltrimethylammonium bromide is added to obtain carbon nanotube suspension；Will
7.612g thiourea and 24.156g Cu (NO3)2·3H2O is added in above-mentioned carbon nanotube suspension, is stirred；By above-mentioned solution
Being transferred in the water heating kettle of 250mL from room temperature and start 160 DEG C to be warming up to the rate program of 2 DEG C/min, keeps 160 DEG C of reactions
10h；After the completion of reaction, natural cooling is cooled to room temperature, filters, washs, dries and obtains CNT base after roasting at 350 DEG C
Electrode material for super capacitor.
Electrochemical property test is carried out to this capacitor, electrolyte used is the KOH solution of 6mol/L, measure in scanning speed
It is 550F/g to spend for ratio electric capacity during 5mV/s.
Embodiment 3
A kind of preparation method of CNT based super capacitor electrode material, comprises the following steps：By 10g CNT
Flow back in the nitric acid of 5mol/L and the mixed solution of the sulphuric acid composition of 3mol/L under 100 DEG C of reflux temperature 2.5h；Spend
CNT after ionized water centrifuge washing pickling is until supernatant pH=7；CNT after washing is scattered in again
In 200mL deionized water, and it is outstanding to add 0.785g cationic surfactant Cetyltrimethylammonium bromide to obtain CNT
Turbid liquid；By 7.612g thiourea and 24.156g Cu (NO3)2·3H2O is added in above-mentioned carbon nanotube suspension, is stirred；Will
Above-mentioned solution is transferred in the water heating kettle of 250mL and starts to be warming up to 160 DEG C with the rate program of 2 DEG C/min from room temperature, keeps 160
DEG C reaction 10h；After the completion of reaction, natural cooling is cooled to room temperature, filters, washs, dries and obtain carbon after roasting at 350 DEG C and receives
Mitron based super capacitor electrode material.
Electrochemical property test is carried out to this capacitor, electrolyte used is the KOH solution of 6mol/L, measure in scanning speed
It is 540F/g to spend for ratio electric capacity during 5mV/s.
Embodiment 4
A kind of preparation method of CNT based super capacitor electrode material, comprises the following steps：By 10g CNT
Flow back in the nitric acid of 5mol/L and the mixed solution of the sulphuric acid composition of 3mol/L under 80 DEG C of reflux temperature 3h；Use deionization
CNT after water centrifuge washing pickling is until supernatant pH=7；CNT after washing is scattered in 200mL again
In ionized water, and 0.785g cationic surfactant Cetyltrimethylammonium bromide is added to obtain carbon nanotube suspension；Will
7.612g thiourea and 24.156g Cu (NO3)2·3H2O is added in above-mentioned carbon nanotube suspension, is stirred；By above-mentioned solution
Being transferred in the water heating kettle of 250mL from room temperature and start 160 DEG C to be warming up to the rate program of 2 DEG C/min, keeps 160 DEG C of reactions
6h；After the completion of reaction, natural cooling is cooled to room temperature, filters, washs, dries and obtains CNT base after roasting at 350 DEG C
Electrode material for super capacitor.
Electrochemical property test is carried out to this capacitor, electrolyte used is the KOH solution of 6mol/L, measure in scanning speed
It is 600F/g to spend for ratio electric capacity during 5mV/s.
Embodiment 5
A kind of preparation method of CNT based super capacitor electrode material, comprises the following steps：By 10g CNT
Flow back in the nitric acid of 5mol/L and the mixed solution of the sulphuric acid composition of 3mol/L under 80 DEG C of reflux temperature 3h；Use deionization
CNT after water centrifuge washing pickling is until supernatant pH=7；CNT after washing is scattered in 200mL again
In ionized water, and 0.576g anionic is added to obtain carbon nanotube suspension；By 7.612g
Thiourea and 17.048g CuCl2·2H2O is added in above-mentioned carbon nanotube suspension, is stirred；Above-mentioned solution is transferred to
Starting 160 DEG C to be warming up to the rate program of 2 DEG C/min from room temperature in the water heating kettle of 250mL, keeps 160 DEG C of reaction 6h；Reaction
After the completion of natural cooling be cooled to room temperature, filter, washing, dry simultaneously after the roasting at 350 DEG C CNT base super capacitor
Device electrode material.
Electrochemical property test is carried out to this capacitor, electrolyte used is the KOH solution of 6mol/L, measure in scanning speed
It is 590F/g to spend for ratio electric capacity during 5mV/s.
Above-described specific embodiment, has been carried out to the purpose of the present invention, technical scheme and beneficial effect further
Describe in detail, the specific embodiment that the foregoing is only the present invention is should be understood that, is not intended to limit the present invention
Protection domain, all any modification, equivalent substitution and improvement that within the spirit and principles in the present invention, is done etc., all should include
Within protection scope of the present invention.
Claims (8)
1. a kind of preparation method of CNT based super capacitor electrode material, it is characterised in that comprise the following steps：
(1) CNT is carried out more than 2h in the mixed solution of nitric acid and sulphuric acid under 70 DEG C～100 DEG C of reflux temperature
Reflux operation；
(2) CNT after the pickling of deionized water centrifuge washing is until supernatant pH=7；
(3) CNT after washing is scattered in deionized water again, and it is suspended to add surfactant to obtain CNT
Liquid；
(4) thiourea and readily soluble cupric salt are added in above-mentioned carbon nanotube suspension, stirs；
(5) above-mentioned solution being transferred in water heating kettle from room temperature and temperature programming is proceeded by 160 DEG C, keeps 160 DEG C of reaction 6h
～10h；
(6) filter, washing, dry, after roasting CNT based super capacitor electrode material.
2. the preparation method of a kind of CNT based super capacitor electrode material according to claim 1, its feature exists
In, in nitric acid described in step (1) and the mixed solution of sulphuric acid the concentration of nitric acid be the concentration of 5mol/L, sulphuric acid be 3mol/
L.
3. the preparation method of a kind of CNT based super capacitor electrode material according to claim 1 and 2, its feature
It is, it is 3h that reflux temperature described in step (1) is 80 DEG C, return time.
4. the preparation method of a kind of CNT based super capacitor electrode material according to claim 3, its feature exists
In surfactant described in step (3) is cationic surfactant or anion surfactant.
5. the preparation method of a kind of CNT based super capacitor electrode material according to claim 4, its feature exists
In it is dodecyl that the cationic surfactant is Cetyltrimethylammonium bromide, the anion surfactant
Sodium sulfate.
6. the preparation method of a kind of CNT based super capacitor electrode material according to claim 5, its feature exists
In readily soluble cupric salt described in step (4) is copper chloride or copper nitrate.
7. the preparation method of a kind of CNT based super capacitor electrode material according to claim 6, its feature exists
In the speed of temperature programming described in step (5) is 2 DEG C/min.
8. the preparation method of a kind of CNT based super capacitor electrode material according to claim 7, its feature exists
In the temperature of roasting described in step (6) is 350 DEG C.
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| CN201611177570.3A CN106449183A (en) | 2016-12-19 | 2016-12-19 | Preparation method of carbon nanotube-based supercapacitor electrode material |
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| CN201611177570.3A CN106449183A (en) | 2016-12-19 | 2016-12-19 | Preparation method of carbon nanotube-based supercapacitor electrode material |
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Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101049924A (en) * | 2007-03-29 | 2007-10-10 | 浙江大学 | Method for producing Nano carbon tube clad by metallic sulfide |
| CN101503560A (en) * | 2009-01-16 | 2009-08-12 | 上海师范大学 | Carbon nano-tube / polymer / metallic sulfide nano composite material and preparation thereof |
| CN102212252A (en) * | 2011-05-11 | 2011-10-12 | 天津大学 | Poly(ethylenedioxythiophene)/carbon nanotube composite material and preparation method thereof |
| CN106024408A (en) * | 2016-07-26 | 2016-10-12 | 电子科技大学 | Ruthenium oxide-copper sulfide composite material, application thereof and electrode plate for supercapacitor |
-
2016
- 2016-12-19 CN CN201611177570.3A patent/CN106449183A/en active Pending
Patent Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101049924A (en) * | 2007-03-29 | 2007-10-10 | 浙江大学 | Method for producing Nano carbon tube clad by metallic sulfide |
| CN101503560A (en) * | 2009-01-16 | 2009-08-12 | 上海师范大学 | Carbon nano-tube / polymer / metallic sulfide nano composite material and preparation thereof |
| CN102212252A (en) * | 2011-05-11 | 2011-10-12 | 天津大学 | Poly(ethylenedioxythiophene)/carbon nanotube composite material and preparation method thereof |
| CN106024408A (en) * | 2016-07-26 | 2016-10-12 | 电子科技大学 | Ruthenium oxide-copper sulfide composite material, application thereof and electrode plate for supercapacitor |
Non-Patent Citations (2)
| Title |
|---|
| KE-JING HUANG等: ""One-step synthesis of layered CuS/multi-walled carbon nanotube nanocomposites for supercapacitor electrode material with ultrahigh specific capacitance"", 《ELECTROCHIMICA ACTA》 * |
| TING ZHU等: ""Arrays of ultrafine CuS nanoneedles supported on a CNT backbone for application in supercapacitors"", 《JOURNAL OF MATERIALS CHEMISTRY》 * |
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Application publication date: 20170222 |