CN106006614A - Preparation method of self-support nitrogen-doped porous graphene for super-capacitor - Google Patents
Preparation method of self-support nitrogen-doped porous graphene for super-capacitor Download PDFInfo
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- CN106006614A CN106006614A CN201610351306.0A CN201610351306A CN106006614A CN 106006614 A CN106006614 A CN 106006614A CN 201610351306 A CN201610351306 A CN 201610351306A CN 106006614 A CN106006614 A CN 106006614A
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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
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01B—NON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
- C01B2204/00—Structure or properties of graphene
- C01B2204/04—Specific amount of layers or specific thickness
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01B—NON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
- C01B2204/00—Structure or properties of graphene
- C01B2204/20—Graphene characterized by its properties
- C01B2204/22—Electronic properties
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01B—NON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
- C01B2204/00—Structure or properties of graphene
- C01B2204/20—Graphene characterized by its properties
- C01B2204/30—Purity
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01B—NON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
- C01B2204/00—Structure or properties of graphene
- C01B2204/20—Graphene characterized by its properties
- C01B2204/32—Size or surface area
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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 self-support nitrogen-doped porous graphene for a super-capacitor, which is characterized by comprising the following steps: 1) dispersing nano nickel powder into a buffer solution of dopamine/Tris-HCl, carrying out ultrasonic oscillation, and then carrying out mechanical stirring at room temperature for reacting and heating; after paste is formed, pressing the paste into a sheet by using a roller press of which the roller diameter is 50cm, so as to obtain a sheet-shaped nitrogen-doped porous graphene precursor; 2) by taking polydopamine in the sheet-shaped nitrogen-doped porous graphene precursor prepared in the step 1) as a solid precursor and taking nickel as a catalyst and a template, carrying out high temperature sintering in an inert gas sintering furnace, and finally, cooling the sintering product to room temperature in the inert gas, so as to obtain a nickel powder coated sheet of a nitrogen-doped graphene product; and 3) putting the nickel powder coated sheet of the nitrogen-doped graphene product, prepared in the step 2), into strong acid for etching off the nano nickel powder template by the acid, and then, cleaning and drying the sheet in ultra-pure water repeatedly, so as to obtain self-support nitrogen-doped porous graphene. The used raw materials are non-toxic and cheap and are easy to obtain, the process is simple, the cost is low, and nitrogen-doped graphene with a high specific surface area and high quality can be prepared.
Description
Technical field
The present invention relates to field of graphene technology, a kind of ultracapacitor self-supporting N doping porous stone is particularly provided
The preparation method of ink alkene.
Background technology
Ultracapacitor makes again double layer capacitor (Electrical Double-Layer Capacitor) be a kind of new
Type energy storage device, the feature such as it has, and the charging interval is short, length in service life, good temp characteristic, the saving energy and environmental protection.Super
Level capacitor is of many uses.Power balance power supply as hoisting apparatus, it is possible to provide the electric power of super-large current;As vehicle launch
Power supply, starting efficiency and reliability are all high than traditional accumulator, can completely or partially substitute traditional accumulator;As car
The traction energy can produce electric automobile, substitute traditional internal combustion engine, transform existing trolleybus;With militarily may be used
Ensure the startup smoothly (especially in cold winter) of the battlebus such as tank, panzer, the pulse energy as laser weapon.
According to Mechanism of electrochemical behaviors of anhydrous, ultracapacitor can be divided into double layer capacitor and pseudocapacitors.Double layer capacitor mainly uses
Carbon-based material, the electrode material of pseudocapacitors mainly has transition metal oxide and conducting polymer.With electronic product to electricity
The requirements at the higher level of source device, the self-supporting super capacitor material without any binding agent and conductive agent is increasingly subject to extensively
Concern and research.Two-dimensional graphene paper because of its good electric conductivity and higher specific surface area, is a kind of ideal whole
Body, self-supporting super capacitor electrode material, but in actual applications, the accumulation of graphene sheet layer makes to form electric double layer
Effective area reduce.Therefore, whether research can overcome this defect to its modification.Ruoff et al. is at Graphene-Based
Chemical modification grapheme material is applied in electrode material for super capacitor by Ultracapacitors mono-literary composition first, but
Being to find that the ratio capacitance of water system and organic system electrolyte is the most relatively low, it thinks the master causing quality more undesirable than electric capacity
The reason is wanted to be: the chemical modification Graphene electrodes material of reduction preparation is again reunited and caused its effective ratio area significantly to drop
Low, it is impossible to adsorb substantial amounts of electrolyte ion.It addition, the electric property of original material with carbon element is relatively weak, so far, send out
Existing carbon based energy source is all the nano-carbon material being doped, i.e. exotic atom doping material with carbon element.This is because, doping different former
Son, especially nitrogen-atoms, be possible not only to provide lone pair electrons, additionally it is possible to changes spin density and the charge density of carbon atom, makes
It has the highest spin density.Meanwhile, electronics can be from adjacent carbon atom contribution to nitrogen-atoms, and electronics also can lead to simultaneously
Cross in the pz track that nitrogen-atoms feeds back to carbon atom, thus improve its electric property.In existing Graphene N doping method mostly
Use in nitrogen atom doping to the lattice of Graphene in gas phase system by the method for high temperature or arc discharge, but these methods
The professional equipments such as high vacuum system need to be used, also need to use the hydrogen of high risk, corrosive ammonia etc., its preparation condition
Harshness, cost are high, dangerous big, and the porous of Graphene can not be guaranteed, therefore are not suitable for large-scale production.Therefore, send out
Open up the study hotspot that the synthetic method of quick, green, easy N doping porous graphene remains current.
Summary of the invention
In view of this, the present invention is directed to the disappearance of prior art existence, it is an object of the invention to provide a kind of super electricity
The container preparation method of self-supporting N doping porous graphene, its advantages of nontoxic raw materials, cheap and easily-available used, technique is simple, becomes
This is cheap, and can prepare the high-quality nitrogen-doped graphene of high-specific surface area.
For achieving the above object, the present invention uses such as purgation technical scheme: a kind of ultracapacitor self-supporting N doping
The preparation method of porous graphene, comprises the steps:
1) 3-10 g nano-nickel powder powder is dispersed in dopamine that 300-1000 mL concentration are 0.1-5mg/mL/
In the buffer solution of Tris-HCl, sonic oscillation 1 h, then room temperature mechanical stirring reaction 5-10h, heats under the conditions of 50 DEG C
1-4h;After becoming pasty state, it is pressed into lamellar with the roll squeezer that roller footpath is 50cm, obtains flake N doping porous graphene forerunner
Body;
2) using 1) the laminar N doping porous graphene presoma poly-dopamine therein prepared makees as solid precursor, nickel
For catalyst and template, high temperature sintering in the noble gas sintering furnace of temperature 800-1000 DEG C, finally in noble gas
It is cooled to room temperature, obtains the nickel sheet body of nitrogen-doped graphene coating product;
3) by 2) the nickel sheet body of nitrogen-doped graphene coating product prepared puts in strong acid, with harsh eating away wherein nano-nickel powder
After template, cleaning-drying in ultra-pure water repeatedly, obtain self-supporting N doping porous graphene.
Preferably, pH=8.5 of the buffer solution of dopamine/Tris-HCl described in described step 1);Described roll squeezer
Pressure is 0.2-0.4 MPa)
Preferably, described step 2) described in nano-nickel powder granularity less than purity >=99%, mean diameter≤0.5 um.
Preferably, described step 2) described in noble gas be purity be argon or the nitrogen of >=99%.
Preferably, at least one during the strong acid described in described step 3) is hydrochloric acid, nitric acid, perchloric acid.
The present invention compared with prior art has clear advantage and beneficial effect, particularly as follows: use technique scheme,
The present invention can obtain high-quality nitrogen-doped graphene, and the thickness of gained nitrogen-doped graphene material is about 2 ~ 7 layers, and nitrogen contains
Amount is more than 7%, and specific surface area is in 1000 more than m2/g, specific capacity 250-350F/g.Nitrogen-doped graphene of the present invention
It is to utilize the strong adsorptivity of poly-dopamine and caking property and nikel powder to be bonded to a block, under the high temperature conditions, is wrapped in nikel powder
Poly-dopamine precursor around thermally decomposes, and generates nitrogen-doped graphene material, simultaneously in block under the catalytic action of nickel
Nano-nickel powder remove after the nano-void that formed ensure that the porous of Graphene, in this technical scheme, demand equipment is few, system
Preparation Method is simple and easy to do, and course of reaction is easily controllable, dangerous little, low cost, can be mass, and easily large-scale promotion makes
With.
Detailed description of the invention
Embodiment 1
The preparation method of a kind of ultracapacitor self-supporting N doping porous graphene, comprises the steps:
1) 3 g nano-nickel powder powder are dispersed in the buffering of dopamine/Tris-HCl that 300 mL concentration are 0.1mg/mL
In solution, sonic oscillation 1 h, then room temperature mechanical stirring reaction 5 h, heat 1h under the conditions of 50 DEG C;After becoming pasty state,
It is pressed into lamellar with the roll squeezer that roller footpath is 50cm, obtains flake N doping porous graphene presoma;Described dopamine/
PH=8.5 of the buffer solution of Tris-HCl;The pressure of described roll squeezer is 0.2 MPa.
2) using 1) the laminar N doping porous graphene presoma poly-dopamine therein prepared as solid precursor,
Nickel is as catalyst and template, and high temperature sintering in the noble gas sintering furnace of temperature 800 DEG C, finally in noble gas
It is cooled to room temperature, obtains the nickel sheet body of nitrogen-doped graphene coating product;Described nano-nickel powder granularity is less than purity >=99%,
Mean diameter≤0.5 um;Described noble gas be purity be the argon of >=99%.
3) by 2) the nickel sheet body of nitrogen-doped graphene coating product prepared puts in strength hydrochloric acid, wherein receives with harsh eating away
After rice nikel powder template, cleaning-drying in ultra-pure water repeatedly, obtain self-supporting N doping porous graphene.
Embodiment 2
The preparation method of a kind of ultracapacitor self-supporting N doping porous graphene, comprises the steps:
1) buffering that 10 g nano-nickel powder powder are dispersed in dopamine/Tris-HCl that 1000 mL concentration are 5mg/mL is molten
In liquid, sonic oscillation 1 h, then room temperature mechanical stirring reaction 10 h, heat 4h under the conditions of 50 DEG C;After becoming pasty state, use
Roller footpath is that the roll squeezer of 50cm is pressed into lamellar, obtains flake N doping porous graphene presoma;Described dopamine/Tris-
PH=8.5 of the buffer solution of HCl;The pressure of described roll squeezer is 0.4 MPa.
2) using 1) the laminar N doping porous graphene presoma poly-dopamine therein prepared as solid precursor,
Nickel is as catalyst and template, and high temperature sintering in the noble gas sintering furnace of temperature 1000 DEG C, finally in noble gas
It is cooled to room temperature, obtains the nickel sheet body of nitrogen-doped graphene coating product;Described nano-nickel powder granularity is less than purity >=99%,
Mean diameter≤0.5 um;Described noble gas be purity be the nitrogen of >=99%.
3) by 2) the nickel sheet body of nitrogen-doped graphene coating product prepared puts in strong nitric acid, wherein receives with harsh eating away
After rice nikel powder template, cleaning-drying in ultra-pure water repeatedly, obtain self-supporting N doping porous graphene.
Embodiment 3
The preparation method of a kind of ultracapacitor self-supporting N doping porous graphene, comprises the steps:
1) 6 g nano-nickel powder powder are dispersed in the buffer solution of dopamine/Tris-HCl that 500 mL concentration are 3mg/mL
In, sonic oscillation 1 h, then room temperature mechanical stirring reaction 7 h, heat 3h under the conditions of 50 DEG C;After becoming pasty state, use roller footpath
Roll squeezer for 50cm is pressed into lamellar, obtains flake N doping porous graphene presoma;Described dopamine/Tris-HCl's
PH=8.5 of buffer solution;The pressure of described roll squeezer is 0.3MPa.
2) using 1) the laminar N doping porous graphene presoma poly-dopamine therein prepared as solid precursor,
Nickel, as catalyst and template, high temperature sintering in the noble gas sintering furnace of temperature 900 DEG C, finally drops in noble gas
Warm to room temperature, obtain the nickel sheet body of nitrogen-doped graphene coating product;Described nano-nickel powder granularity is less than purity >=99%, flat
All particle diameter≤0.5 um;Described noble gas be purity be the argon of >=99%.
3) by 2) the nickel sheet body of nitrogen-doped graphene coating product prepared puts in perchloric acid, wherein receives with harsh eating away
After rice nikel powder template, cleaning-drying in ultra-pure water repeatedly, obtain self-supporting N doping porous graphene.
Embodiment 4
The preparation method of a kind of ultracapacitor self-supporting N doping porous graphene, comprises the steps:
1) buffering that 8g nano-nickel powder powder is dispersed in dopamine/Tris-HCl that 650 mL concentration are 3.5mg/mL is molten
In liquid, sonic oscillation 1h, then room temperature mechanical stirring reaction 8 h, heat 4h under the conditions of 50 DEG C;After becoming pasty state, use roller footpath
Roll squeezer for 50cm is pressed into lamellar, obtains flake N doping porous graphene presoma;Described dopamine/Tris-HCl's
PH=8.5 of buffer solution;The pressure of described roll squeezer is 0.4 MPa.
2) using 1) the laminar N doping porous graphene presoma poly-dopamine therein prepared as solid precursor,
Nickel is as catalyst and template, and high temperature sintering in the noble gas sintering furnace of temperature 1000 DEG C, finally in noble gas
It is cooled to room temperature, obtains the nickel sheet body of nitrogen-doped graphene coating product;Described nano-nickel powder granularity is less than purity >=99%,
Mean diameter≤0.5 um;Described noble gas be purity be the nitrogen of >=99%.
3) by 2) the nickel sheet body of nitrogen-doped graphene coating product prepared puts in strength hydrochloric acid, wherein receives with harsh eating away
After rice nikel powder template, cleaning-drying in ultra-pure water repeatedly, obtain self-supporting N doping porous graphene.
Specific surface area and specific capacity to the Graphene that above-described embodiment 1 ~ 4 prepares detect, with N2 as adsorbate,
The graphene film adsorption isotherm when 77 K is measured with automatic absorbing instrument (Micromeritics ASAP 2020 M),
Measure its specific surface area.
The method of testing of specific capacity is as follows: self-supporting N doping porous graphene is cut into the disk of a diameter of 1cm, choosing
Take two tablet qualities close as electrode material, glass fibre membrane is as barrier film, 1M Na2SO4Aqueous solution is electrolyte, uses
Swagelok type battery assembles two electrode super capacitors, carries out constant current charge-discharge test, and voltage is 0.01~1.0 V, records
Its specific capacity under 100 mA/g electric current densities.
By above test, the data obtained are as shown in table 1 below:
Table 1
Embodiment | Nitrogen content/% | Specific surface area/m2/g | 100mA/g electric current density specific capacity/F/g | 1000 mA/g electric current density specific capacities/F/g | 1000 mA/g electric current density 500 times circulation volume conservation rates/% |
Embodiment 1 | 9 | 1323 | 301 | 162 | 94 |
Embodiment 2 | 9 | 1443 | 286 | 169 | 93 |
Embodiment 3 | 10 | 1521 | 327 | 187 | 95 |
Embodiment 4 | 10 | 1487 | 341 | 173 | 95 |
As can be seen from Table I, the N doping porous graphene self-supporting super capacitor electrode material nitrogen prepared by the present invention
Content is high, specific surface area is big, higher than electric capacity, high rate performance is excellent, good cycling stability, is highly suitable for various fine electronic device
Part etc..
The above, be only presently preferred embodiments of the present invention, not impose any restrictions the technical scope of the present invention,
Therefore every technical spirit according to the present invention is to any trickle amendment made for any of the above embodiments, equivalent variations and modification, the most still
Belong in the range of technical solution of the present invention.
Claims (5)
1. the ultracapacitor preparation method of self-supporting N doping porous graphene, it is characterised in that: include walking as follows
Rapid:
1) 3-10 g nano-nickel powder powder is dispersed in dopamine that 300-1000 mL concentration are 0.1-5mg/mL/
In the buffer solution of Tris-HCl, sonic oscillation 1 h, then room temperature mechanical stirring reaction 5-10 h, adds under the conditions of 50 DEG C
Hot 1-4h;After becoming pasty state, it is pressed into lamellar with the roll squeezer that roller footpath is 50cm, obtains flake N doping porous graphene forerunner
Body;
2) using 1) the laminar N doping porous graphene presoma poly-dopamine therein prepared makees as solid precursor, nickel
For catalyst and template, high temperature sintering in the noble gas sintering furnace of temperature 800-1000 DEG C, finally in noble gas
It is cooled to room temperature, obtains the nickel sheet body of nitrogen-doped graphene coating product;
3) by 2) the nickel sheet body of nitrogen-doped graphene coating product prepared puts in strong acid, with harsh eating away wherein nano-nickel powder
After template, cleaning-drying in ultra-pure water repeatedly, obtain self-supporting N doping porous graphene.
The preparation method of a kind of ultracapacitor self-supporting N doping porous graphene, it is special
Levy and be: pH=8.5 of the buffer solution of dopamine/Tris-HCl described in described step 1);The pressure of described roll squeezer is
0.2-0.4 Mpa。
The preparation method of a kind of ultracapacitor self-supporting N doping porous graphene, it is special
Levy and be: described step 2) described in nano-nickel powder granularity less than purity >=99%, mean diameter≤0.5 um.
The preparation method of a kind of ultracapacitor self-supporting N doping porous graphene, it is special
Levy and be: described step 2) described in noble gas be purity be argon or the nitrogen of >=99%.
The preparation method of a kind of ultracapacitor self-supporting N doping porous graphene, it is special
Levy and be: the strong acid described in described step 3) is at least one in hydrochloric acid, nitric acid, perchloric acid.
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Cited By (4)
Publication number | Priority date | Publication date | Assignee | Title |
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CN107235472A (en) * | 2017-05-24 | 2017-10-10 | 华中科技大学 | Porous vertical graphene nano wall array of N doping and preparation method and application |
CN108054021A (en) * | 2017-12-07 | 2018-05-18 | 南阳理工学院 | Bicarbonate nickel-poly-dopamine-graphene composite material and preparation method and application |
CN109336098A (en) * | 2018-09-30 | 2019-02-15 | 西安工业大学 | Porous N doped graphene of multilayer self-supporting and preparation method thereof |
CN112479187A (en) * | 2020-11-13 | 2021-03-12 | 深圳市翔丰华科技股份有限公司 | Improved self-supporting nitrogen-doped porous graphene for supercapacitor and preparation method thereof |
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CN105271217A (en) * | 2015-12-10 | 2016-01-27 | 湖南师范大学 | Method for preparing nitrogen-doped three-dimensional graphene |
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CN102107868A (en) * | 2011-03-01 | 2011-06-29 | 哈尔滨工程大学 | Method for preparing porous graphene material |
US20140141224A1 (en) * | 2012-11-08 | 2014-05-22 | William Marsh Rice University | Fabrication of carbon foams through solution processing in superacids |
CN103601181A (en) * | 2013-12-04 | 2014-02-26 | 南京大学扬州化学化工研究院 | Method for preparing nitrogen-doped graphene with polydopamine as raw material |
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Cited By (6)
Publication number | Priority date | Publication date | Assignee | Title |
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CN107235472A (en) * | 2017-05-24 | 2017-10-10 | 华中科技大学 | Porous vertical graphene nano wall array of N doping and preparation method and application |
CN107235472B (en) * | 2017-05-24 | 2019-03-08 | 华中科技大学 | Porous vertical graphene nano wall array of N doping and the preparation method and application thereof |
CN108054021A (en) * | 2017-12-07 | 2018-05-18 | 南阳理工学院 | Bicarbonate nickel-poly-dopamine-graphene composite material and preparation method and application |
CN108054021B (en) * | 2017-12-07 | 2019-08-23 | 南阳理工学院 | Bicarbonate nickel-poly-dopamine-graphene composite material and preparation method and application |
CN109336098A (en) * | 2018-09-30 | 2019-02-15 | 西安工业大学 | Porous N doped graphene of multilayer self-supporting and preparation method thereof |
CN112479187A (en) * | 2020-11-13 | 2021-03-12 | 深圳市翔丰华科技股份有限公司 | Improved self-supporting nitrogen-doped porous graphene for supercapacitor and preparation method thereof |
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