CN108878176A - A kind of technology of preparing of supercapacitor N doping mesoporous carbon composite metal oxide electrode material - Google Patents
A kind of technology of preparing of supercapacitor N doping mesoporous carbon composite metal oxide electrode material Download PDFInfo
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- CN108878176A CN108878176A CN201810722612.XA CN201810722612A CN108878176A CN 108878176 A CN108878176 A CN 108878176A CN 201810722612 A CN201810722612 A CN 201810722612A CN 108878176 A CN108878176 A CN 108878176A
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- metal oxide
- mesoporous carbon
- electrode material
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- supercapacitor
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- 239000002131 composite material Substances 0.000 title claims abstract description 70
- VNWKTOKETHGBQD-UHFFFAOYSA-N methane Chemical compound C VNWKTOKETHGBQD-UHFFFAOYSA-N 0.000 title claims abstract description 43
- 229910044991 metal oxide Inorganic materials 0.000 title claims abstract description 40
- 150000004706 metal oxides Chemical class 0.000 title claims abstract description 39
- 239000007772 electrode material Substances 0.000 title claims abstract description 34
- 238000005516 engineering process Methods 0.000 title claims abstract description 18
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 claims abstract description 36
- VKYKSIONXSXAKP-UHFFFAOYSA-N hexamethylenetetramine Chemical compound C1N(C2)CN3CN1CN2C3 VKYKSIONXSXAKP-UHFFFAOYSA-N 0.000 claims abstract description 32
- 238000001354 calcination Methods 0.000 claims abstract description 25
- 229910052799 carbon Inorganic materials 0.000 claims abstract description 25
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 claims abstract description 22
- 229910052757 nitrogen Inorganic materials 0.000 claims abstract description 19
- 238000002360 preparation method Methods 0.000 claims abstract description 19
- XSQUKJJJFZCRTK-UHFFFAOYSA-N Urea Chemical compound NC(N)=O XSQUKJJJFZCRTK-UHFFFAOYSA-N 0.000 claims abstract description 17
- 239000004202 carbamide Substances 0.000 claims abstract description 17
- 239000004312 hexamethylene tetramine Substances 0.000 claims abstract description 16
- 235000010299 hexamethylene tetramine Nutrition 0.000 claims abstract description 16
- 229910052751 metal Inorganic materials 0.000 claims abstract description 15
- 229920001343 polytetrafluoroethylene Polymers 0.000 claims abstract description 13
- 239000004810 polytetrafluoroethylene Substances 0.000 claims abstract description 13
- 239000011261 inert gas Substances 0.000 claims abstract description 11
- 239000000463 material Substances 0.000 claims abstract description 10
- 239000002184 metal Substances 0.000 claims abstract description 10
- 239000012266 salt solution Substances 0.000 claims abstract description 9
- -1 polytetrafluoroethylene Polymers 0.000 claims abstract description 3
- 239000006229 carbon black Substances 0.000 claims abstract 2
- 239000002905 metal composite material Substances 0.000 claims abstract 2
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 37
- PXHVJJICTQNCMI-UHFFFAOYSA-N Nickel Chemical compound [Ni] PXHVJJICTQNCMI-UHFFFAOYSA-N 0.000 claims description 32
- VEXZGXHMUGYJMC-UHFFFAOYSA-N Hydrochloric acid Chemical compound Cl VEXZGXHMUGYJMC-UHFFFAOYSA-N 0.000 claims description 22
- 238000002156 mixing Methods 0.000 claims description 21
- QAOWNCQODCNURD-UHFFFAOYSA-N sulfuric acid Substances OS(O)(=O)=O QAOWNCQODCNURD-UHFFFAOYSA-N 0.000 claims description 15
- 229910052759 nickel Inorganic materials 0.000 claims description 14
- 239000000126 substance Substances 0.000 claims description 11
- BOTDANWDWHJENH-UHFFFAOYSA-N Tetraethyl orthosilicate Chemical compound CCO[Si](OCC)(OCC)OCC BOTDANWDWHJENH-UHFFFAOYSA-N 0.000 claims description 10
- 238000001035 drying Methods 0.000 claims description 10
- 239000002105 nanoparticle Substances 0.000 claims description 10
- XEEYBQQBJWHFJM-UHFFFAOYSA-N Iron Chemical compound [Fe] XEEYBQQBJWHFJM-UHFFFAOYSA-N 0.000 claims description 9
- 239000000243 solution Substances 0.000 claims description 8
- 239000006260 foam Substances 0.000 claims description 7
- 238000007598 dipping method Methods 0.000 claims description 6
- 238000001027 hydrothermal synthesis Methods 0.000 claims description 6
- 239000000203 mixture Substances 0.000 claims description 6
- 229910052760 oxygen Inorganic materials 0.000 claims description 6
- 238000002604 ultrasonography Methods 0.000 claims description 6
- 238000004140 cleaning Methods 0.000 claims description 5
- 229910017052 cobalt Inorganic materials 0.000 claims description 5
- 239000010941 cobalt Substances 0.000 claims description 5
- 239000000843 powder Substances 0.000 claims description 5
- 238000003756 stirring Methods 0.000 claims description 5
- 238000010792 warming Methods 0.000 claims description 5
- 238000005406 washing Methods 0.000 claims description 5
- GUTLYIVDDKVIGB-UHFFFAOYSA-N cobalt atom Chemical compound [Co] GUTLYIVDDKVIGB-UHFFFAOYSA-N 0.000 claims description 4
- UFMZWBIQTDUYBN-UHFFFAOYSA-N cobalt dinitrate Chemical compound [Co+2].[O-][N+]([O-])=O.[O-][N+]([O-])=O UFMZWBIQTDUYBN-UHFFFAOYSA-N 0.000 claims description 4
- 229910052742 iron Inorganic materials 0.000 claims description 4
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 claims description 3
- 210000002421 cell wall Anatomy 0.000 claims description 3
- 230000005611 electricity Effects 0.000 claims description 3
- 239000007788 liquid Substances 0.000 claims description 3
- 239000001301 oxygen Substances 0.000 claims description 3
- 238000004321 preservation Methods 0.000 claims description 3
- 238000009938 salting Methods 0.000 claims description 3
- 229910002554 Fe(NO3)3·9H2O Inorganic materials 0.000 claims description 2
- 239000002253 acid Substances 0.000 claims description 2
- 239000004615 ingredient Substances 0.000 claims description 2
- NINIDFKCEFEMDL-UHFFFAOYSA-N Sulfur Chemical compound [S] NINIDFKCEFEMDL-UHFFFAOYSA-N 0.000 claims 1
- 239000005864 Sulphur Substances 0.000 claims 1
- 239000011248 coating agent Substances 0.000 claims 1
- 238000000576 coating method Methods 0.000 claims 1
- 229910000314 transition metal oxide Inorganic materials 0.000 abstract description 7
- 238000000034 method Methods 0.000 abstract description 5
- 238000009826 distribution Methods 0.000 abstract description 4
- 238000004146 energy storage Methods 0.000 abstract description 3
- 239000011232 storage material Substances 0.000 abstract description 3
- 239000002245 particle Substances 0.000 abstract description 2
- 150000001720 carbohydrates Chemical class 0.000 abstract 1
- 235000014633 carbohydrates Nutrition 0.000 abstract 1
- 239000003795 chemical substances by application Substances 0.000 abstract 1
- 239000002808 molecular sieve Substances 0.000 abstract 1
- URGAHOPLAPQHLN-UHFFFAOYSA-N sodium aluminosilicate Chemical compound [Na+].[Al+3].[O-][Si]([O-])=O.[O-][Si]([O-])=O URGAHOPLAPQHLN-UHFFFAOYSA-N 0.000 abstract 1
- KRHYYFGTRYWZRS-UHFFFAOYSA-N Fluorane Chemical compound F KRHYYFGTRYWZRS-UHFFFAOYSA-N 0.000 description 12
- HEMHJVSKTPXQMS-UHFFFAOYSA-M Sodium hydroxide Chemical compound [OH-].[Na+] HEMHJVSKTPXQMS-UHFFFAOYSA-M 0.000 description 12
- 229910003266 NiCo Inorganic materials 0.000 description 11
- 239000003575 carbonaceous material Substances 0.000 description 11
- 239000008367 deionised water Substances 0.000 description 8
- 229910021641 deionized water Inorganic materials 0.000 description 8
- 229910005949 NiCo2O4 Inorganic materials 0.000 description 7
- 229930006000 Sucrose Natural products 0.000 description 7
- CZMRCDWAGMRECN-UGDNZRGBSA-N Sucrose Chemical compound O[C@H]1[C@H](O)[C@@H](CO)O[C@@]1(CO)O[C@@H]1[C@H](O)[C@@H](O)[C@H](O)[C@@H](CO)O1 CZMRCDWAGMRECN-UGDNZRGBSA-N 0.000 description 7
- 230000009286 beneficial effect Effects 0.000 description 7
- 239000011148 porous material Substances 0.000 description 7
- 239000005720 sucrose Substances 0.000 description 7
- 235000013339 cereals Nutrition 0.000 description 6
- 238000013019 agitation Methods 0.000 description 5
- 229910052723 transition metal Inorganic materials 0.000 description 5
- 150000003624 transition metals Chemical class 0.000 description 5
- 238000002484 cyclic voltammetry Methods 0.000 description 4
- 238000010408 sweeping Methods 0.000 description 4
- OKKJLVBELUTLKV-UHFFFAOYSA-N Methanol Chemical group OC OKKJLVBELUTLKV-UHFFFAOYSA-N 0.000 description 3
- 239000003990 capacitor Substances 0.000 description 3
- UPWOEMHINGJHOB-UHFFFAOYSA-N cobalt(III) oxide Inorganic materials O=[Co]O[Co]=O UPWOEMHINGJHOB-UHFFFAOYSA-N 0.000 description 3
- 238000002242 deionisation method Methods 0.000 description 3
- 230000000694 effects Effects 0.000 description 3
- 239000011259 mixed solution Substances 0.000 description 3
- 125000004433 nitrogen atom Chemical group N* 0.000 description 3
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical group CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 description 2
- 229910003264 NiFe2O4 Inorganic materials 0.000 description 2
- 230000015572 biosynthetic process Effects 0.000 description 2
- 150000001721 carbon Chemical group 0.000 description 2
- 125000005842 heteroatom Chemical group 0.000 description 2
- 150000002500 ions Chemical class 0.000 description 2
- QJGQUHMNIGDVPM-UHFFFAOYSA-N nitrogen group Chemical group [N] QJGQUHMNIGDVPM-UHFFFAOYSA-N 0.000 description 2
- 230000003647 oxidation Effects 0.000 description 2
- 238000007254 oxidation reaction Methods 0.000 description 2
- 238000001179 sorption measurement Methods 0.000 description 2
- 230000007704 transition Effects 0.000 description 2
- VHUUQVKOLVNVRT-UHFFFAOYSA-N Ammonium hydroxide Chemical compound [NH4+].[OH-] VHUUQVKOLVNVRT-UHFFFAOYSA-N 0.000 description 1
- UFHFLCQGNIYNRP-UHFFFAOYSA-N Hydrogen Chemical compound [H][H] UFHFLCQGNIYNRP-UHFFFAOYSA-N 0.000 description 1
- 229910001030 Iron–nickel alloy Inorganic materials 0.000 description 1
- PWHULOQIROXLJO-UHFFFAOYSA-N Manganese Chemical compound [Mn] PWHULOQIROXLJO-UHFFFAOYSA-N 0.000 description 1
- 240000007594 Oryza sativa Species 0.000 description 1
- 235000007164 Oryza sativa Nutrition 0.000 description 1
- OAICVXFJPJFONN-UHFFFAOYSA-N Phosphorus Chemical compound [P] OAICVXFJPJFONN-UHFFFAOYSA-N 0.000 description 1
- 238000010521 absorption reaction Methods 0.000 description 1
- 230000004913 activation Effects 0.000 description 1
- 239000012670 alkaline solution Substances 0.000 description 1
- 239000000908 ammonium hydroxide Substances 0.000 description 1
- 230000005540 biological transmission Effects 0.000 description 1
- 239000003054 catalyst Substances 0.000 description 1
- 238000006555 catalytic reaction Methods 0.000 description 1
- 210000003850 cellular structure Anatomy 0.000 description 1
- 230000008859 change Effects 0.000 description 1
- 150000001875 compounds Chemical class 0.000 description 1
- 238000010276 construction Methods 0.000 description 1
- 239000013078 crystal Substances 0.000 description 1
- 230000002950 deficient Effects 0.000 description 1
- 238000011161 development Methods 0.000 description 1
- 238000010586 diagram Methods 0.000 description 1
- 150000002148 esters Chemical class 0.000 description 1
- 235000019441 ethanol Nutrition 0.000 description 1
- 125000000524 functional group Chemical group 0.000 description 1
- 239000007789 gas Substances 0.000 description 1
- 229910002804 graphite Inorganic materials 0.000 description 1
- 239000010439 graphite Substances 0.000 description 1
- 239000001257 hydrogen Substances 0.000 description 1
- 229910052739 hydrogen Inorganic materials 0.000 description 1
- 238000010348 incorporation Methods 0.000 description 1
- 230000003993 interaction Effects 0.000 description 1
- 239000002608 ionic liquid Substances 0.000 description 1
- 229910052748 manganese Inorganic materials 0.000 description 1
- 239000011572 manganese Substances 0.000 description 1
- 238000004519 manufacturing process Methods 0.000 description 1
- 239000013335 mesoporous material Substances 0.000 description 1
- 150000002739 metals Chemical class 0.000 description 1
- 125000001434 methanylylidene group Chemical group [H]C#[*] 0.000 description 1
- 239000013081 microcrystal Substances 0.000 description 1
- 239000003002 pH adjusting agent Substances 0.000 description 1
- 230000000737 periodic effect Effects 0.000 description 1
- 229910052698 phosphorus Inorganic materials 0.000 description 1
- 239000011574 phosphorus Substances 0.000 description 1
- 239000002994 raw material Substances 0.000 description 1
- 230000027756 respiratory electron transport chain Effects 0.000 description 1
- 230000002441 reversible effect Effects 0.000 description 1
- 235000009566 rice Nutrition 0.000 description 1
- 238000000926 separation method Methods 0.000 description 1
- RMAQACBXLXPBSY-UHFFFAOYSA-N silicic acid Chemical compound O[Si](O)(O)O RMAQACBXLXPBSY-UHFFFAOYSA-N 0.000 description 1
- 235000012239 silicon dioxide Nutrition 0.000 description 1
- 238000000967 suction filtration Methods 0.000 description 1
- 238000012360 testing method Methods 0.000 description 1
- AGGKEGLBGGJEBZ-UHFFFAOYSA-N tetramethylenedisulfotetramine Chemical compound C1N(S2(=O)=O)CN3S(=O)(=O)N1CN2C3 AGGKEGLBGGJEBZ-UHFFFAOYSA-N 0.000 description 1
- 230000010148 water-pollination Effects 0.000 description 1
Classifications
-
- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01G—CAPACITORS; CAPACITORS, RECTIFIERS, DETECTORS, SWITCHING DEVICES, LIGHT-SENSITIVE OR TEMPERATURE-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
-
- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01G—CAPACITORS; CAPACITORS, RECTIFIERS, DETECTORS, SWITCHING DEVICES, LIGHT-SENSITIVE OR TEMPERATURE-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, LIGHT-SENSITIVE OR TEMPERATURE-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
-
- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01G—CAPACITORS; CAPACITORS, RECTIFIERS, DETECTORS, SWITCHING DEVICES, LIGHT-SENSITIVE OR TEMPERATURE-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
-
- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01G—CAPACITORS; CAPACITORS, RECTIFIERS, DETECTORS, SWITCHING DEVICES, LIGHT-SENSITIVE OR TEMPERATURE-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
- H01G11/46—Metal oxides
-
- 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
Landscapes
- Engineering & Computer Science (AREA)
- Power Engineering (AREA)
- Microelectronics & Electronic Packaging (AREA)
- Chemical & Material Sciences (AREA)
- Materials Engineering (AREA)
- Manufacturing & Machinery (AREA)
- Battery Electrode And Active Subsutance (AREA)
- Electric Double-Layer Capacitors Or The Like (AREA)
Abstract
The invention discloses a kind of supercapacitor technologies of preparing of N doping mesoporous carbon composite metal oxide electrode material, and wherein preparation method is as follows：First using mesoporous molecular sieve SBA-15 as template, sugary carbohydrates are carbon source, and urea and hexamethylenetetramine are nitrogen source, calcine through inert gas, after template agent removing, obtain N doping mesoporous carbon；Then metal salt solution is added, is passed through inert gas calcining, obtains N doping mesoporous carbon metal composite oxide composite material；After above-mentioned material is mixed with polytetrafluoroethylene (PTFE) (PTFE), carbon black again, coated, compacting, dry, obtained supercapacitor N doping mesoporous carbon composite metal oxide electrode material.Preparation method disclosed by the invention is low in cost, easy to operate.The duct of the N doping mesoporous carbon of the method for the present invention preparation is clear, aperture is suitable for, large specific surface area, and transition metal oxide nano even particle distribution, load capacity are big thereon.The electrochemical performance of N doping mesoporous carbon composite metal oxide electrode material has vast market prospect in the energy storage materials such as supercapacitor field.
Description
Technical field
The present invention relates to mesoporous carbon composite material preparation technical fields, are used for super capacitor more particularly to one kind
The N doping ordered mesopore carbon composite metal oxide electrode material and its technology of preparing of device.
Background technique
Carbon material has many advantages, such as abundant raw material, large specific surface area, high temperature resistant, acid and alkali-resistance and good electric conductivity.Aperture
Meso-porous carbon material of the range in 2 ~ 50 nm as an important branch of porous carbon materials is a kind of receiving for metasable state carbon crystal
Rice structural material, specific surface area is larger, even aperture distribution, three-dimensional connection in duct is orderly, chemical and thermal stability is good, can make
Standby catalyst carrier, hydrogen storage material, adsorbing separation and electrode material for super capacitor etc..However, carbon material surface has chemistry lazy
Property, activation degree are limited, limit the extensive use of its more areas.
In recent years, by introducing the hetero atoms such as nitrogen, oxygen, phosphorus in carbon skeleton, become a kind of chemistry to porous carbon surface
Properties modifying important channel.Wherein, N doping is because extensively, easily doping due to is gradually concerned by people in its source.Nitrogen-atoms exists
Be in carbon atom the adjacent position of same period in the periodic table of elements, similar atomic radius be conducive to replace carbon atom and
It is doped.Material surface chemistries can effectively be changed by the carbon material of N doping and form certain official group, make it
With certain acid-base property and hydrophily, and effectively improve the application range of material.In addition, the lone pair electrons of nitrogen-atoms act as
The effect of carrier, electron density increases and enabled band narrows, and shows conductive capability more superior than pure carbon material, may be used also
Make graphite microcrystal plane occur it is many misplace, be bent, offing normal etc. there is the defective bit of asymmetric electronics, so as to improve cellular structure
And electron transfer rate.After nitrogen-atoms is introduced carbon material, the difference of the higher electron density in part and surface energy, Neng Gouzeng
Add carbon material to the adsorption capacity of ion, enhance the interaction between metallic and carrier, promote the evenly dispersed of metal,
Change material pore structure and surface nature, while the introducing of nitrogen also changes the alkalinity, oxidation stability, catalysis of carbon material
Many properties such as activity.
The metal oxide of the formation such as transiting group metal elements such as nickel, iron, cobalt capacitive property with higher and fake capacitance
Property, suitable negative potential operation interval the advantages that, and it is resourceful, cheap, environmental-friendly, be that a kind of great development is latent
The high performance electrode material of power.However, its electrical conductance is weaker, energy density and power density is relatively low and stability is poor.In nitrogen
Addition there is the transition elements of redox ability to produce transition metal oxide compound in doping ordered mesoporous material skeleton
Material, the composite material that this preparation method obtains have more active sites and higher energy-conserving character, can be very big
The chemical property for improving composite material, before there is wide market in the fields such as super capacitor energy storage electrode material
Scape.
Therefore, in conjunction with the above problem, a kind of mesoporous carbon composite metal oxidation of supercapacitor N doping is prepared in production
Object electrode material is the energy storage material problem of those skilled in the art's urgent need to resolve.
Summary of the invention
In view of this, the present invention provides the N doping mesoporous carbon composite metal oxide electrode materials of technology preparation
Duct is clear, load capacity is big, electrochemical performance.
To achieve the goals above, the technical solution adopted by the present invention is as follows.
A kind of supercapacitor technology of preparing of N doping mesoporous carbon composite metal oxide electrode material, specifically includes
Following steps：
（1）Prepare SBA-15：Concentrated hydrochloric acid and deionized water are added in P123, magnetic agitation is uniform, and it is mixed that ethyl orthosilicate is added
It is even, after hydro-thermal reaction, suction filtration, washing, drying and high-temperature roasting, obtain white powder SBA-15；
（2）Prepare presoma N doping ordered mesopore carbon：
A, in step（1）Sugar, the concentrated sulfuric acid, water, ultrasound premixing are added in the SBA-15 of acquisition；
B, the mixed liquor of urea and hexamethylenetetramine is added, ultrasonic mixing simultaneously heats；
C, these four substances of the mixed liquor of sugar, the concentrated sulfuric acid, water, urea and hexamethylenetetramine are sequentially added, ultrasonic mixing simultaneously adds
Heat；
D, it is passed through inert gas calcining, template is removed and obtains presoma N doping ordered mesopore carbon NMC after cleaning, drying；
（3）Dipping：Step is added in the mixed liquor of the various metals salting liquid prepared（2）In the NMC of acquisition, metal salt solution with
The mass ratio of NMC is 1:0.1 ~ 0.2, it stirs evenly, impregnates, adjusting solution is alkalinity, pH 9.0；
（4）Calcining：By step（3）After the mixture of acquisition is filtered, washed, dries, it is passed through inert gas calcining, obtains N doping
Mesoporous carbon composite metal oxide electrode material；
（5）Electrode preparation：By step（4）The N doping mesoporous carbon composite metal oxide electrode material of acquisition, it is mixed with PTFE, water
It closes, is coated uniformly in nickel foam, it is dry after compacting.
As can be seen from the above technical solutions, compared with prior art, beneficial effects of the present invention are as follows：
Ionic liquid, template SBA-15 are mixed with containing polyazin in the technical solution adopted by the present invention, are passed through inertia
Gas calcining prepares presoma N doping meso-porous carbon material, and N doping Jie is prepared in calcining after introducing transition metal salt solution dipping
Hole carbon composite metal oxide electrode material.Due to the doping of nitrogen, nitrogen-containing functional group is increased, makes the NiCo to be formed2O4Nanometer
Grain is more tiny, increases specific surface area, and increase redox active site, improves electrode capacity, preparation process
It is easy to operate, low in cost, product size is controllable, be easy to go into operation on a large scale.
Preferably, the step（1）Middle concentrated hydrochloric acid:Water:P123:The mass ratio of ethyl orthosilicate is 1: 0.2-0.4 :
0.025- 0.045 : 0.07-0.09。
By using above-mentioned preferred embodiment, the beneficial effects of the present invention are：Suitable hydrochloric acid, water, P123, positive silicic acid second
The mass ratio of ester can guarantee to prepare the template SBA-15 in suitable aperture, be conducive to the later period and construct regular mesopore orbit
The composite material of structure.
Preferably, the step（1）Middle magnetic agitation temperature is 40 DEG C, and mixing time is 4 h, and hydro-thermal reaction temperature control exists
100 ~ 120 DEG C of 24 h of heat preservation, maturing temperature are 500 DEG C, and calcining time is 6 h;
Preferably, the step（1）In water energy replaced with methanol or ethyl alcohol;
Preferably, the step（2）Middle water:The concentrated sulfuric acid:Sugar:The mass ratio of the mixed liquor of urea and hexamethylenetetramine is 1:
0.02 -0.04 :0.15 -0.33 :0.22 -0.42。
By using above-mentioned preferred embodiment, the beneficial effects of the present invention are：Water, the concentrated sulfuric acid, sugar, urea and six methines
Between tetramine mixed liquor suitable mass ratio help to prepare large specific surface area, it is mesoporous be suitable for, the N doping that nitrogen content is high has
Sequence mesoporous carbon.
Preferably, the time of ultrasound premixing is 20 ~ 30 min in the step a;
Preferably, the ultrasonic mixing of the step b and c and heat condition be：5-7 h is first kept the temperature under the conditions of 100 DEG C, then
It is warming up to 160 DEG C of heat preservation 5-7 h;
Preferably, 750-850 DEG C of temperature control of the step d is passed through inert gas calcining 5-6 h.
By using above-mentioned preferred embodiment, the beneficial effects of the present invention are：Select suitable incorporation time, calcination time
Be conducive to prepare that duct is clear, is evenly distributed, the N doping mesoporous carbon that nitrogen content is high with temperature condition.
Preferably, hydrofluoric acid is selected to remove removing template in the step d, hydrofluoric acid concentration is 6% ~ 22%, and hydrofluoric acid volume is
40 mL；
Preferably, the step（2）The sugar of middle selection includes but is not limited to sucrose；
Preferably, the step（3）In metal salt solution include but is not limited to Ni (NO3)2·6H2O、Fe(NO3)3·9H2O、
Co(NO3)2·6H2O。
By using above-mentioned preferred embodiment, the beneficial effects of the present invention are：The formation such as metallic element such as nickel, iron, cobalt
Metal oxide chemical property with higher and capacitive property and suitable negative potential operation interval.
Preferably, the step（3）Middle dip time is 12 h;
Preferably, the step（3）Described in pH adjusting agent include but is not limited to sodium hydroxide, ammonium hydroxide;
Preferably, the step（4）In be passed through inert gas calcining temperature control at 400-550 DEG C, calcination time is 2-4 h.
By using above-mentioned preferred embodiment, the beneficial effects of the present invention are：By step（4）The N doping mesoporous carbon of acquisition
Composite metal oxide electrode material is mixed with PTFE, water, is coated uniformly in nickel foam, dry after compacting, electricity needed for being made
Pole.
Preferably, the step（5）Middle N doping mesoporous carbon composite metal oxide electrode material and PTFE, water mixing ratio
Example is 8: 1 : 1;
Preferably, the step（5）In be coated uniformly in nickel foam, and apply 5-10 MPa pressure, in 60-80 DEG C of drying
6-8 h。
By using above-mentioned preferred embodiment, the beneficial effects of the present invention are：Suitable calcination temperature and calcination time have
Conducive to the characteristic and structure for improving transition metal oxide Yu N doping mesoporous carbon composite material, it is higher to prepare stability
The composite material.
Preferably, the water selected in the preparation method is deionized water；
Preferably, the inert gas in the preparation method includes but is not limited to nitrogen.
The invention also discloses a kind of supercapacitor systems of N doping mesoporous carbon composite metal oxide electrode material
Standby technology.The composite material has the composite construction including N doping mesoporous carbon and metal oxide, the composite material
Main group becomes NiCo2O3(by NiO and Co2O3Composition) and two-dimentional six sidesp6mmCarbon, metal oxide nanoparticles NiCo2O3's
Average grain diameter is 7.5-9.0 nm, and transition metal oxide is supported on carbon surface, therefore obtains the ratio table of prepared composite material
Area is 550-700 m2/ g, mesoporous average pore size are 5.0-6.0 nm；By CV measurement when sweeping speed is 10 mV/s, specific capacitance
Amount is 350-450 F/g.
The N doping ordered mesopore carbon composite metal oxide material duct that above-mentioned technique obtains is clear, nitrogen content is high, golden
Belong to oxide nano particles load capacity greatly and be evenly distributed, wherein introducing hetero-atoms nitrogen, enhances absorption of the carbon material to ion
Ability optimizes material pore structure and surface characteristic.A variety of transition metal salt solutions of different ratio are added, both improve transition
The disadvantage that metallic conductance is weak, stability is poor, and make composite material that there is superior electro-chemical activity and chemical property.
Preferably, metallic element includes but is not limited to nickel, cobalt in the composite material, can also be iron, manganese etc..
In conclusion preparation method disclosed by the invention have many advantages, such as it is low in cost, easy to operate.The method of the present invention system
Standby composite material duct is clear, metal oxide nanoparticles are evenly distributed, electrochemical performance.
Detailed description of the invention
In order to more clearly explain the embodiment of the invention or the technical proposal in the existing technology, to embodiment or will show below
There is attached drawing needed in technical description to be briefly described, it should be apparent that, the accompanying drawings in the following description is only this
The embodiment of invention for those of ordinary skill in the art without creative efforts, can also basis
The attached drawing of offer obtains other attached drawings.
NiCo in Fig. 1 example 12O4The XRD diagram of/NMC composite material.
NiCo in Fig. 2 example 12O4The TEM of/NMC composite material schemes.
NiCo in Fig. 3 example 12O4NiO-Fe in/NMC composite material2O3Nano particle diameter distribution map.
NiCo in Fig. 4 example 12O4The EDS of/NMC composite material schemes.
NiCo in Fig. 5 example 12O4The N2 adsorption of/NMC composite material is desorbed and graph of pore diameter distribution.
NiCo in Fig. 6 example 12O4The CV of/NMC composite material schemes.
Specific embodiment
The following is a clear and complete description of the technical scheme in the embodiments of the invention, it is clear that described embodiment
Only a part of the embodiments of the present invention, instead of all the embodiments.Based on the embodiments of the present invention, this field is common
Technical staff's every other embodiment obtained without making creative work belongs to the model that the present invention protects
It encloses.The embodiment of the invention discloses a kind of preparations of N doping mesoporous carbon composite metal oxide electrode material of supercapacitor
The specific process step of technology.
[embodiment 1]
（1）Prepare SBA-15：Concentrated hydrochloric acid and deionized water are added in P123, temperature control magnetic agitation 4 under conditions of 40 DEG C
H is added ethyl orthosilicate and mixes, concentrated hydrochloric acid:Deionized water: P123 :The mass ratio of ethyl orthosilicate is 1: 0.2:
0.025:0.07-0.09, temperature control filter, washing, dry and 500 DEG C of high temperature roastings in 100 DEG C of progress 24 h of hydro-thermal reaction
After burning 6 h, white powder SBA-15 is obtained；
（2）Prepare presoma N doping ordered mesopore carbon：
A, in step（1）Sugar, the concentrated sulfuric acid, water, 20 min of ultrasound premixing are added in the SBA-15 of acquisition；
B, the mixed liquor of urea and hexamethylenetetramine is added, ultrasonic mixing simultaneously heats；
C, these four substances of the mixed liquor of sucrose, the concentrated sulfuric acid, water, urea and hexamethylenetetramine are sequentially added, wherein deionization
Water:The concentrated sulfuric acid:Sucrose:The mass ratio of the mixed liquor of urea and hexamethylenetetramine is 1:0.02 :0.15 :0.22, first exist
6 h of ultrasonic mixing under the conditions of 100 DEG C, then it is warming up to 160 DEG C of 6 h of ultrasonic mixing；
D, nitrogen 5 h of calcining are passed through for 800 DEG C of temperature control, taking 40 mL concentration is that 6% hydrofluoric acid removes removing template, after cleaning, drying,
Obtain presoma N doping ordered mesopore carbon NMC；
（3）Dipping：By molar ratio 1:1 Ni (NO3)2·6H2O and Co (NO3)2·6H2Step is added in the mixed solution of O（2）It obtains
In the NMC obtained, the mass ratio of transition metal salt solution and NMC are 1:0.1, it stirs evenly, 12 h is impregnated, with sodium hydroxide tune
Solution is alkalinity, pH 9.0；
（4）Calcining：By step（3）After the mixture of acquisition is filtered, washed, dries, temperature control is passed through nitrogen under the conditions of 500 DEG C
3 h are calcined, transition metal oxide/N doping ordered mesoporous carbon composite material is obtained；
（5）Electrode preparation：By step（4）The N doping mesoporous carbon composite metal oxide electrode material of acquisition and PTFE, water with
8:1:1 ratio mixes mixing, is coated uniformly in nickel foam, suppresses at 8 MPa and in 80 DEG C of dry 8 h.
NiCo is prepared by [embodiment 1]2O4/ NMC composite material (NiCo2O4As NiO, Co2O3), NiCo2O4Nanometer
Particle is embedded in the fake capacitance behavior with higher in alkaline solution as electrode of nitrogen-containing ordered mesopore carbon composite material, not only may be used
To realize quick, reversible electron transmission, and there is at nanoparticle and the surface NOMC and cell walls the Electro Sorb mistake of proton
Journey, to greatly realize the redox of composite material.
By testing it is found that it is mainly organized as NiCo2O4With two-dimentional six sidesp6mm carbon；Metal oxide nanoparticles
NiCo2O4Average grain diameter be 7.5-9.0 nm；Its specific surface area is 550-700 m2/ g, mesoporous average pore size are 5.0-6.0
nm；By CV measurement when sweeping speed is 10 mV/s, specific capacitance is 350 ~ 450 F/g.
The NiCo that [embodiment 1] is prepared is characterized by Fig. 1 ~ 62O4The physics and chemical property of/NMC composite material.Such as
Shown in Fig. 1, tested by XRD, composite material by ridge-like structure NiCo2O4Mutually formed with the NMC with hexagonal structure.Such as Fig. 2
It shown in ~ 4, is tested by TEM and EDS, average grain diameter is the NiCo of 8.3 nm in composite material2O4Nano particle is relatively uniformly
It is distributed on the surface and cell walls of NOMC, the essential element ingredient contained by composite material：Carbon C, oxygen O, nitrogen N, nickel, cobalt
Co, wherein the atomic percent of Ni, Co, N are respectively 6.29 %, 3.56 % and 1.32 %.The ratio table of composite material is measured by Fig. 5
Area is 638 m2/ g, aperture are 5.4 nm.It is tested through CV, the specific capacitance of composite material is 417 F/g in Fig. 6.
[embodiment 2]
（1）Prepare SBA-15：Concentrated hydrochloric acid and deionized water are added in P123, temperature control magnetic agitation 4 under conditions of 40 DEG C
H is added ethyl orthosilicate and mixes, concentrated hydrochloric acid:Deionized water:P123:The mass ratio of ethyl orthosilicate is 1: 0.2: 0.025:
0.07-0.09, temperature control filter, after washing, drying and 500 DEG C of high temperature 6 h of roasting in 100 DEG C of progress 24 h of hydro-thermal reaction,
Obtain white powder SBA-15；
（2）Prepare presoma N doping ordered mesopore carbon：
A, in step（1）Sugar, the concentrated sulfuric acid, water, 25 min of ultrasound premixing are added in the SBA-15 of acquisition；
B, the mixed liquor of urea and hexamethylenetetramine is added, ultrasonic mixing simultaneously heats；
C, these four substances of the mixed liquor of sucrose, the concentrated sulfuric acid, water, urea and hexamethylenetetramine are sequentially added, wherein deionization
Water:The concentrated sulfuric acid:Sucrose:The mass ratio of the mixed liquor of urea and hexamethylenetetramine is 1:0.03 :0.20 :0.32, first exist
5 h of ultrasonic mixing under the conditions of 100 DEG C, then it is warming up to 160 DEG C of 6 h of ultrasonic mixing；
D, nitrogen 5.5 h of calcining are passed through for 800 DEG C of temperature control, taking 40 mL concentration is that 8% hydrofluoric acid goes removing template, cleaning, drying
Afterwards, presoma N doping ordered mesopore carbon NMC is obtained；
（3）Dipping：By molar ratio 1:2 Ni (NO3)2·6H2O and Co (NO3)2·6H2Step is added in the mixed solution of O（2）It obtains
In the NMC obtained, the mass ratio of transition metal salt solution and NMC are 1:0.15, it stirs evenly, 12 h is impregnated, with sodium hydroxide tune
Solution is alkalinity, pH 9.0；
（4）Calcining：By step（3）After the mixture of acquisition is filtered, washed, dries, temperature control is passed through nitrogen under the conditions of 550 DEG C
3 h are calcined, transition metal oxide/N doping ordered mesoporous carbon composite material is obtained；
（5）Electrode preparation：By step（4）The N doping mesoporous carbon composite metal oxide electrode material of acquisition and PTFE, water with
8:1:1 ratio mixes mixing, is coated uniformly in nickel foam, suppresses at 8 MPa and in 80 DEG C of dry 8 h.
The NiCo prepared by [embodiment 2]2O4/ NOMC composite material is mainly organized as NiCo2O4With two-dimentional six sidesp6mmCarbon；Metal oxide nanoparticles NiCo2O4Average grain diameter be 8.6 nm；The specific surface area of composite material is 594 m2/
G, mesoporous average pore size is 5.7 nm；By CV measurement when sweeping speed is 10 mV/s, specific capacitance is 383 F/g.
[embodiment 3]
（1）Prepare SBA-15：Concentrated hydrochloric acid and deionized water are added in P123, temperature control magnetic agitation 4 under conditions of 40 DEG C
H is added ethyl orthosilicate and mixes, concentrated hydrochloric acid:Deionized water:P123:The mass ratio of ethyl orthosilicate is 1: 0.2: 0.025:
0.07-0.09, temperature control filter, after washing, drying and 500 DEG C of high temperature 6 h of roasting in 100 DEG C of progress 24 h of hydro-thermal reaction,
Obtain white powder SBA-15；
（2）Prepare presoma N doping ordered mesopore carbon：
A, in step（1）Sugar, the concentrated sulfuric acid, water, 30 min of ultrasound premixing are added in the SBA-15 of acquisition；
B, the mixed liquor of urea and hexamethylenetetramine is added, ultrasonic mixing simultaneously heats；
C, these four substances of the mixed liquor of sucrose, the concentrated sulfuric acid, water, urea and hexamethylenetetramine are sequentially added, wherein deionization
Water:The concentrated sulfuric acid:Sucrose:The mass ratio of the mixed liquor of urea and hexamethylenetetramine is 1:0.04 :0.30 :0.42, first exist
5 h of ultrasonic mixing under the conditions of 100 DEG C, then it is warming up to 160 DEG C of 6 h of ultrasonic mixing；
D, nitrogen 6 h of calcining are passed through for 800 DEG C of temperature control, taking 40 mL concentration is that 15% hydrofluoric acid goes removing template, cleaning, drying
Afterwards, presoma N doping ordered mesopore carbon NMC is obtained；
（3）Dipping：By molar ratio 2:1 Ni (NO3)2·6H2O and Co (NO3)2·6H2Step is added in the mixed solution of O（2）It obtains
In the NMC obtained, the mass ratio of transition metal salt solution and NMC are 1:0.2, it stirs evenly, 12 h is impregnated, with sodium hydroxide tune
Solution is alkalinity, pH 9.0；
（4）Calcining：By step（3）After the mixture of acquisition is filtered, washed, dries, temperature control is passed through nitrogen under the conditions of 450 DEG C
3 h are calcined, transition metal oxide/N doping ordered mesoporous carbon composite material is obtained；
（5）Electrode preparation：By step（4）The N doping mesoporous carbon composite metal oxide electrode material of acquisition and PTFE, water with
8:1:1 ratio mixes mixing, is coated uniformly in nickel foam, suppresses at 8 MPa and in 80 DEG C of dry 8 h.
The NiFe prepared by [embodiment 3]2O4/ NOMC composite material is mainly organized as NiFe2O4With two-dimentional six sidesp6mmCarbon；Metal oxide nanoparticles NiFe2O4Average grain diameter be 7.9 nm；The specific surface area of composite material is 702 m2/
G, mesoporous average pore size is 5.1 nm；By CV measurement when sweeping speed is 10 mV/s, specific capacitance is 447 F/g.
Claims (11)
1. a kind of supercapacitor technology of preparing of N doping mesoporous carbon composite metal oxide electrode material, feature exist
In including the following steps：
（1）Prepare SBA-15：Concentrated hydrochloric acid and water are added in P123, stirred evenly, ethyl orthosilicate is added and mixes, by hydro-thermal
Reaction filters, after washing, drying and high-temperature roasting, obtains white powder SBA-15；
（2）Prepare presoma N doping ordered mesopore carbon：A, in step（1）Sugar, the concentrated sulfuric acid, water are added in the SBA-15 of acquisition,
Ultrasound premixing；B, the mixed liquor of urea and hexamethylenetetramine is added, ultrasonic mixing simultaneously heats；C, sugar, dense sulphur are sequentially added
Acid, water, urea and the mixed liquor of hexamethylenetetramine these four substances, ultrasonic mixing simultaneously heat；D, it is passed through inert gas calcining,
It removes template and obtains presoma N doping mesoporous carbon NMC after cleaning, drying；
（3）Dipping：Step is added in the mixed liquor of the one or more nickel based metal salting liquids prepared（2）In the NMC of acquisition, metal
The mass ratio of salting liquid and NMC are 1:0.1 ~ 0.2, it stirs evenly, impregnates, adjusting solution is alkalinity, pH 9.0；
（4）Calcining：By step（3）After the mixture of acquisition is filtered, washed, dries, it is passed through inert gas calcining, obtains super electricity
The order mesoporous composite metal oxide electrode material of container N doping；
（5）Electrode preparation：By step（4）After obtained combination electrode material is mixed with polytetrafluoroethylene (PTFE) (PTFE), carbon black, warp
Coating, dry, obtained supercapacitor N doping mesoporous carbon complex metal oxide electrode.
2. a kind of supercapacitor according to claim 1 N doping mesoporous carbon composite metal oxide electrode material
Technology of preparing, which is characterized in that the step（1）Middle concentrated hydrochloric acid:Water: P123 :The mass ratio of ethyl orthosilicate is 1:
0.2-0.4 : 0.025- 0.045 : 0.07-0.09。
3. a kind of supercapacitor according to claim 1 N doping mesoporous carbon composite metal oxide electrode material
Technology of preparing, which is characterized in that the step（2）Middle water:The concentrated sulfuric acid:Sugar:The matter of the mixed liquor of urea and hexamethylenetetramine
Amount is than being 1: 0.02 -0.04 : 0.15 -0.33 : 0.22 -0.42.
4. a kind of supercapacitor according to claim 1 N doping mesoporous carbon composite metal oxide electrode material
Technology of preparing, which is characterized in that the condition heated after the ultrasonic mixing of the step b and c is：First ultrasonic mixing, uniformly after
5-7 h is kept the temperature under the conditions of 100 DEG C, then is warming up to 160 DEG C of heat preservation 5-7 h.
5. a kind of supercapacitor according to claim 1 N doping mesoporous carbon composite metal oxide electrode material
Technology of preparing, which is characterized in that the step d is passed through inert gas, and temperature control is 750-850 DEG C, calcination time 5-6
h。
6. a kind of supercapacitor according to claim 1 N doping mesoporous carbon composite metal oxide electrode material
Technology of preparing, which is characterized in that the step（3）In metal salt solution include but is not limited to Ni (NO3)2·6H2O、Fe
(NO3)3·9H2O、Co(NO3)2·6H2O。
7. a kind of supercapacitor according to claim 1 N doping mesoporous carbon composite metal oxide electrode material
Technology of preparing, which is characterized in that the step（4）In be passed through inert gas calcining temperature control at 400-550 DEG C, calcination time is
2-4 h。
8. the system of a kind of supercapacitor N doping mesoporous carbon composite metal oxide electrode material according to claim 1
Standby technology, which is characterized in that the step（5）Middle combination electrode material：PTFE：Water=8: 1 : 1.
9. the system of a kind of supercapacitor N doping mesoporous carbon composite metal oxide electrode material according to claim 1
Standby technology, which is characterized in that the step（5）It is middle that the electrode composite material of preparation is evenly applied in nickel foam, 5-10
In 60-80 DEG C of dry 6-8 h after MPa compacting.
10. the N doping mesoporous carbon metal composite oxide electricity of -9 described in any item preparation method preparations according to claim 1
Pole material, which is characterized in that the nano particle of the metal oxide of the composite material is supported on surface and the cell walls of NMC
On, the essential element ingredient that the composite material contains is：Carbon, oxygen, nitrogen and metallic element, the wherein atomic percent of metallic element
Than for the % of 10 % ~ 12.
11. N doping mesoporous carbon composite metal oxide material according to claim 10, which is characterized in that the metal
Including but not limited to one of iron, nickel, cobalt or a variety of.
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