CN108467038A - A kind of preparation method of ultracapacitor nitrogen-doped carbon nano net - Google Patents

A kind of preparation method of ultracapacitor nitrogen-doped carbon nano net Download PDF

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Publication number
CN108467038A
CN108467038A CN201810536069.4A CN201810536069A CN108467038A CN 108467038 A CN108467038 A CN 108467038A CN 201810536069 A CN201810536069 A CN 201810536069A CN 108467038 A CN108467038 A CN 108467038A
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China
Prior art keywords
nitrogen
carbon nano
doped carbon
nano net
anthracene
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CN201810536069.4A
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Inventor
何孝军
魏风
吴胜华
宋章训
余谟鑫
费伦
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Anhui University of Technology AHUT
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Anhui University of Technology AHUT
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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
    • C01B32/00—Carbon; Compounds thereof
    • C01B32/30—Active carbon
    • C01B32/312—Preparation
    • C01B32/342—Preparation characterised by non-gaseous activating agents
    • C01B32/348—Metallic compounds
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B82—NANOTECHNOLOGY
    • B82Y—SPECIFIC USES OR APPLICATIONS OF NANOSTRUCTURES; MEASUREMENT OR ANALYSIS OF NANOSTRUCTURES; MANUFACTURE OR TREATMENT OF NANOSTRUCTURES
    • B82Y40/00—Manufacture or treatment of nanostructures
    • C—CHEMISTRY; METALLURGY
    • C01—INORGANIC CHEMISTRY
    • C01B—NON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
    • C01B32/00—Carbon; Compounds thereof
    • C01B32/15—Nano-sized carbon materials
    • 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
    • H01G11/24—Electrodes characterised by structural features of the materials making up or comprised in the electrodes, e.g. form, surface area or porosity; characterised by the structural features of powders or particles used therefor
    • 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
    • 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
    • H01G11/38—Carbon pastes or blends; Binders or additives therein
    • 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 kind of ultracapacitor preparation methods of nitrogen-doped carbon nano net, belong to technical field of carbon material preparation.This method is using ammonia as nitrogen source, respectively using magnesium hydroxide and potassium hydroxide as template and activator, using anthracene as carbon source.Anthracene is first added in magnesium hydroxide and potassium hydroxide after mixing, mixture of three's ground and mixed after uniform is transferred in corundum boat later, is positioned in horizontal pipe furnace, and under ammonia atmosphere, heats and nitrogen-doped carbon nano net is made.The specific surface area of gained nitrogen-doped carbon nano net is between 1522~2018m2Between/g, total pore volume is between 0.86~1.16cm3Between/g.As electrode material for super capacitor, in 6mol/L KOH electrolyte, when current density is 0.05A/g, specific volume reaches 362.9F/g；When current density increases to 20A/g, specific volume remains 252.9F/g, it is shown that the specific volume of superelevation and good rate capability.

Description

A kind of preparation method of ultracapacitor nitrogen-doped carbon nano net
Technical field
The invention belongs to technical field of carbon material preparation, and in particular to a kind of ultracapacitor nitrogen-doped carbon nano net Preparation method.
Background technology
Ultracapacitor is a kind of new type of energy storage device, with following for fast charge/discharge rates, high power density and length The ring service life has wide practical use in fields such as traffic, the energy, electric vehicles.According to storing up electricity mechanism, ultracapacitor can be with It is divided into pseudocapacitors and double layer capacitor.Electrode material plays a key role in ultracapacitor, and ultracapacitor is used Electrode material includes carbon material, metal oxide and conducting polymer.Carbon-based material is because of its good conductivity, high specific surface area Cause the extensive concern of people with high specific volume.Pure carbon material surface is hydrophobic, increases connecing for electrolyte ion and carbon material Internal resistance is touched, its capacity and rate capability are largely affected.By the method pair for introducing functional group in carbon material surface Its surface is modified, its wetability can not only be effectively improved, and can improve its conductivity, to which carbon materials be greatly improved The capacity and rate capability of material.Currently used method of modifying is that hetero atom N, P, S, B etc. are introduced into carbon skeleton, is made in carbon-coating Graphite microcrystal generate defective bit, while Heteroatom doping is modified carbon material surface in the local area of carbonaceous network, To achieve the purpose that improve carbon material chemical property.
Coal tar is a kind of black obtained during coking of coal or dark brown viscous liquid.Coal tar composition is complicated, Mainly it is made of the compound etc. of the oxygen-containing nitrogenous sulfur-bearing of the aromatic hydrocarbons such as benzene,toluene,xylene, naphthalene, anthracene, phenanthrene, pyrene and aromatic series.Anthracene It is coal tar high temperature distillation object from the distillation of coal tar, is the raw material examined and determine indenes and produce anthraquinone, tannin, can also use Come synthetic pesticide, dyestuff, napalm etc..
Invention content
In order to overcome the deficiencies of the prior art, the present invention provides one kind using ammonia as nitrogen source, using anthracene as carbon source, respectively with honest and clean The magnesium hydroxide and potassium hydroxide of valence are template and activator, directly prepare the side of ultracapacitor nitrogen-doped carbon nano net Method.This method is as follows：
(1) pretreatment of reactant：The magnesium hydroxide of sheet is ground respectively with potassium hydroxide first, then carries out the two Mixing, it is after mixing, the mixture of gained and anthracene ground and mixed is uniform, obtain reactant；Wherein, the quality of potassium hydroxide Account for anthracene, magnesium hydroxide and potassium hydroxide three's mixture gross mass 1/4~4/7, the mass ratio of potassium hydroxide and anthracene is between 1/1 Between~4/1.
(2) preparation of nitrogen-doped carbon nano net：The reactant that step (1) obtains is put into corundum boat, it then will be described Corundum boat is positioned over the centre position of horizontal pipe furnace, is passed through ammonia to exclude the air in stove, with the heating rate of 5 DEG C/min By diamond heating to 220 DEG C, constant temperature 30min, continue with identical heating rate be heated to 300 DEG C holding 30min, then with Identical heating rate is by diamond heating to 900 DEG C, and constant temperature 1h is down to room temperature naturally after reaction, the product that will be obtained It takes out, grind, through pickling, distillation water washing to neutrality, be placed in air dry oven in 110 DEG C of freeze-day with constant temperature 12h, obtain Nitrogen-doped carbon nano net.
Further, the quality of the anthracene is 5g, and the quality of magnesium hydroxide is 10g, and the quality of potassium hydroxide is 15g.This When the nitrogen-doped carbon nano net for preparing be used as symmetric form electrode material for super capacitor, in 6mol/LKOH electrolyte, Under 0.05A/g current densities, specific volume 362.9F/g；Under 20A/g current densities, specific volume 252.9F/g.
Compared with prior art, the present invention has the following technical effects：
1, the present invention be using ammonia as nitrogen source, using pure anthracene as carbon source, respectively using magnesium hydroxide and potassium hydroxide as template and Ultracapacitor nitrogen-doped carbon nano net is directly made in activator.The specific surface area of prepared nitrogen-doped carbon nano net can Reach 2018m2/ g, total pore volume can reach 1.16cm3/g。
2, it present invention eliminates tedious steps such as prior art preparation nano-metal-oxide templates, also eliminates and first synthesizes Carbon nano net, then the complex steps of N doping are carried out, have many advantages, such as simple for process, at low cost.Realize armaticity anthracene simultaneously High value added utilization.
3, the nitrogen-doped carbon nano net electrode material prepared by the present invention, in 6mol/L KOH aqueous electrolytes, in electricity When current density is 0.05A/g, specific volume reaches 362.9F/g；When current density increases to 20A/g, specific volume remains 252.9F/g, it is shown that very high capacity and fabulous rate capability.
Description of the drawings
Fig. 1 is the nitrogen Adsorption and desorption isotherms of nitrogen-doped carbon nano net prepared by the embodiment of the present invention 1,2,3,4.
Fig. 2 is the transmission electron microscope photo of nitrogen-doped carbon nano net prepared by the embodiment of the present invention 3.
Fig. 3 is the nitrogen composition figure of nitrogen-doped carbon nano net prepared by the embodiment of the present invention 3.
Fig. 4 is the structural schematic diagram of nitrogen-doped carbon nano net prepared by the embodiment of the present invention 3.
Fig. 5 is the nitrogen-doped carbon nano net electrode material of the preparation of the embodiment of the present invention 1,2,3,4 in 6mol/LKOH electrolyte In, specific volume under different current densities with current density variation diagram.
Specific implementation mode
In order to better understand the present invention, the present invention will be further described with reference to the accompanying drawings and examples, but this Invention scope of protection is not limited to the range that embodiment illustrates, it should be understood that at example, those skilled in the art Member can be changed and modified on the basis of without prejudice to spirit and scope of the invention, and all such changes and modifications are included in In the scope of the invention.
Embodiment 1
Nitrogen-doped carbon nano net NCN1Specific preparation process it is as follows：
(1) pretreatment of reactant：It weighs 5g potassium hydroxide solids to be put into mortar, grind, it is powdered that 10g is added The two is uniformly mixed by magnesium hydroxide, the mixed powder of gained is gradually put into the mortar for filling 5g anthracenes, ground and mixed is equal It is even, mixture is obtained, gained mixture is stood into 12h, obtains reactant；
(2) preparation of nitrogen-doped carbon nano net：The reactant that step (1) obtains is put into corundum porcelain boat, it will be described rigid Yu Zhou is positioned in horizontal pipe furnace, and being passed through ammonia with the flow of 30mL/min empties the air in tube furnace, using electric furnace Heating, with the heating rate of 5 DEG C/min by diamond heating to 220 DEG C, constant temperature 30min, continuation is added with identical heating rate Heat to 300 DEG C holding 30min, then with identical heating rate by diamond heating to 900 DEG C, be down to naturally after reaction Then obtained product is taken out, is put into beaker after grinding by room temperature, addition 2mol/L dilute hydrochloric acid, ultrasonic vibration 1h, then 12h is stirred at room temperature with magnetic stirring apparatus, is then neutral with 80 DEG C or so of distillation water washing to filtrate, after washing Sample is placed in air dry oven in 110 DEG C of freeze-day with constant temperature ground 325 mesh sieve rear for 24 hours, obtains the carbon nano net of N doping.Institute The carbon nano net for obtaining N doping is labeled as NCN1, XPS test results show its nitrogen content be 6.86%.NCN1It is super as symmetric form Grade capacitor electrode material, in 6mol/L KOH electrolyte, under 0.05A/g current densities, NCN1Specific volume be 302.7F/ Under g, 20A/g current density, NCN1Specific volume be 184.9F/g.
Embodiment 2
Nitrogen-doped carbon nano net NCN2Specific preparation process it is as follows：
(1) pretreatment of reactant：Implement according to the same method of step (1) in embodiment 1, difference exists In the quality of potassium hydroxide is 10g；
(2) preparation of nitrogen-doped carbon nano net：Implement according to the same method of step (2) in embodiment 1.Gained nitrogen Doped carbon nano net is labeled as NCN2, XPS test results show its nitrogen content be 4.57%.NCN2As symmetric form super capacitor Device electrode material, in 6mol/L KOH electrolyte, under 0.05A/g current densities, specific volume 329.3F/g；In 20A/g Under current density, specific volume 227.7F/g.
Embodiment 3
Nitrogen-doped carbon nano net NCN3Specific preparation process it is as follows：
(1) pretreatment of reactant：Implement according to the same method of step (1) in embodiment 1.Difference exists In the quality of potassium hydroxide is 15g；
(2) preparation of nitrogen-doped carbon nano net：Implement according to the same method of step (2) in embodiment 1.Gained nitrogen Doped carbon nano net is labeled as NCN3, nitrogen content 5.66%.NCN3As symmetric form electrode material for super capacitor, In 6mol/L KOH electrolyte, under 0.05A/g current densities, specific volume 362.9F/g；Under 20A/g current densities, Specific volume is 252.9F/g.
Embodiment 4
Nitrogen-doped carbon nano net NCN4Specific preparation process it is as follows：
(1) pretreatment of reactant：Implement according to the same method of step (1) in embodiment 1.Difference exists In the quality of potassium hydroxide is 20g；
(2) preparation of nitrogen-doped carbon nano net：Implement according to the same method of step (2) in embodiment 1.Gained nitrogen Doped carbon nano net is labeled as NCN4, XPS test results show its nitrogen content be 4.62%.NCN4As symmetric form super capacitor Device electrode material, in 6mol/L KOH electrolyte, under 0.05A/g current densities, specific volume 335.1F/g；In 20A/g Under current density, specific volume 234.7F/g.
Pore structure parameter and the element composition and content difference of nitrogen-doped carbon nano net prepared by above-described embodiment 1~4 Refer to Tables 1 and 2.
The pore structure parameter of table 1, nitrogen-doped carbon nano net of the present invention
Table 2, the element composition of nitrogen-doped carbon nano net and content

Claims (2)

1. a kind of ultracapacitor preparation method of nitrogen-doped carbon nano net, it is characterised in that include the following steps：
(1) pretreatment of reactant：It weighs potassium hydroxide solid to be put into mortar, grind, powdered magnesium hydroxide is added, The two is uniformly mixed, the mixed powder of gained is gradually put into the beaker for filling anthracene, is placed on magnetic stirring apparatus and carries out It heats and is uniformly mixed with glass bar, obtain mixture, gained mixture is stood into 12h, obtains reactant；
Wherein, the quality of potassium hydroxide account for potassium hydroxide, magnesium hydroxide and anthracene three's mixture gross mass 1/4~4/7, hydrogen-oxygen The mass ratio of change potassium and anthracene is between 1/1~4/1；
(2) preparation of nitrogen-doped carbon nano net：The reactant that step (1) obtains is put into corundum boat, then by above-mentioned corundum Boat is positioned in horizontal pipe furnace, be passed through ammonia by tube furnace air empty after, continue using ammonia as nitrogen source, with 5 DEG C/ The heating rate of min by diamond heating to 220 DEG C, constant temperature 30min；Then 300 DEG C are heated to the heating rate of 5 DEG C/min 30min is kept, 900 DEG C of final temperature is then heated to the heating rate of 5 DEG C/min, constant temperature 1h is down to room naturally after reaction Temperature is taken out obtained product, grinding, and through pickling, distillation water washing to neutrality, nitrogen-doped carbon nano net is obtained after dry.
2. a kind of preparation method of ultracapacitor nitrogen-doped carbon nano net as described in claim 1, which is characterized in that In step (1), the quality of the anthracene is 5g, and the quality of magnesium hydroxide is 10g, and the quality of potassium hydroxide is 15g.
CN201810536069.4A 2018-05-30 2018-05-30 A kind of preparation method of ultracapacitor nitrogen-doped carbon nano net Pending CN108467038A (en)

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Cited By (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN110155981A (en) * 2019-05-23 2019-08-23 安徽工业大学 A kind of preparation method of the supercapacitor porous charcoal nanometer sheet of nitrogen sulphur codope
CN111540617A (en) * 2020-06-09 2020-08-14 华中农业大学 Preparation system and method of straw nitrogen-phosphorus-iron co-doped active carbon electrode material
CN112908718A (en) * 2021-01-22 2021-06-04 滁州学院 Three-dimensional mutual crosslinking nitrogen-doped acicular carbon, preparation method and application

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CN104108708A (en) * 2014-07-25 2014-10-22 深圳新宙邦科技股份有限公司 Nitrogen-doped graphene and preparation method thereof
CN104445141A (en) * 2014-11-07 2015-03-25 同济大学 Nitrogen-doped modified porous carbon with high specific surface area and preparation method thereof
CN105110325A (en) * 2015-08-25 2015-12-02 安徽工业大学 Method for preparing interconnected and folded graphene materials for super-capacitor
CN105366661A (en) * 2015-12-15 2016-03-02 安徽工业大学 Preparation method of curled porous carbon nanometer sheet for supercapacitor
CN105819419A (en) * 2016-03-09 2016-08-03 安徽工业大学 Preparation method of two-dimensional porous carbon nanosheet for super capacitors

Patent Citations (5)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN104108708A (en) * 2014-07-25 2014-10-22 深圳新宙邦科技股份有限公司 Nitrogen-doped graphene and preparation method thereof
CN104445141A (en) * 2014-11-07 2015-03-25 同济大学 Nitrogen-doped modified porous carbon with high specific surface area and preparation method thereof
CN105110325A (en) * 2015-08-25 2015-12-02 安徽工业大学 Method for preparing interconnected and folded graphene materials for super-capacitor
CN105366661A (en) * 2015-12-15 2016-03-02 安徽工业大学 Preparation method of curled porous carbon nanometer sheet for supercapacitor
CN105819419A (en) * 2016-03-09 2016-08-03 安徽工业大学 Preparation method of two-dimensional porous carbon nanosheet for super capacitors

Cited By (4)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN110155981A (en) * 2019-05-23 2019-08-23 安徽工业大学 A kind of preparation method of the supercapacitor porous charcoal nanometer sheet of nitrogen sulphur codope
CN110155981B (en) * 2019-05-23 2022-07-15 安徽工业大学 Preparation method of nitrogen and sulfur co-doped porous carbon nanosheet for supercapacitor
CN111540617A (en) * 2020-06-09 2020-08-14 华中农业大学 Preparation system and method of straw nitrogen-phosphorus-iron co-doped active carbon electrode material
CN112908718A (en) * 2021-01-22 2021-06-04 滁州学院 Three-dimensional mutual crosslinking nitrogen-doped acicular carbon, preparation method and application

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