CN110136972A - A kind of preparation method of multilayer hierarchical structure supercapacitor composite material - Google Patents
A kind of preparation method of multilayer hierarchical structure supercapacitor composite material Download PDFInfo
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- CN110136972A CN110136972A CN201910338941.9A CN201910338941A CN110136972A CN 110136972 A CN110136972 A CN 110136972A CN 201910338941 A CN201910338941 A CN 201910338941A CN 110136972 A CN110136972 A CN 110136972A
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- 239000002131 composite material Substances 0.000 title claims abstract description 56
- 238000002360 preparation method Methods 0.000 title claims abstract description 27
- PXHVJJICTQNCMI-UHFFFAOYSA-N Nickel Chemical compound [Ni] PXHVJJICTQNCMI-UHFFFAOYSA-N 0.000 claims abstract description 98
- 229910052759 nickel Inorganic materials 0.000 claims abstract description 49
- CSCPPACGZOOCGX-UHFFFAOYSA-N Acetone Chemical compound CC(C)=O CSCPPACGZOOCGX-UHFFFAOYSA-N 0.000 claims abstract description 40
- 239000006260 foam Substances 0.000 claims abstract description 38
- 239000007772 electrode material Substances 0.000 claims abstract description 32
- 238000003756 stirring Methods 0.000 claims abstract description 32
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 27
- 229910000422 cerium(IV) oxide Inorganic materials 0.000 claims abstract description 25
- 239000008367 deionised water Substances 0.000 claims abstract description 25
- 229910021641 deionized water Inorganic materials 0.000 claims abstract description 25
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 claims abstract description 21
- 238000002604 ultrasonography Methods 0.000 claims abstract description 20
- 239000007864 aqueous solution Substances 0.000 claims abstract description 17
- 238000001354 calcination Methods 0.000 claims abstract description 12
- 239000002041 carbon nanotube Substances 0.000 claims abstract description 12
- 229910021393 carbon nanotube Inorganic materials 0.000 claims abstract description 12
- 239000000243 solution Substances 0.000 claims abstract description 12
- 229910052684 Cerium Inorganic materials 0.000 claims abstract description 11
- GWXLDORMOJMVQZ-UHFFFAOYSA-N cerium Chemical compound [Ce] GWXLDORMOJMVQZ-UHFFFAOYSA-N 0.000 claims abstract description 11
- DBMJMQXJHONAFJ-UHFFFAOYSA-M Sodium laurylsulphate Chemical compound [Na+].CCCCCCCCCCCCOS([O-])(=O)=O DBMJMQXJHONAFJ-UHFFFAOYSA-M 0.000 claims abstract description 10
- XSQUKJJJFZCRTK-UHFFFAOYSA-N Urea Chemical compound NC(N)=O XSQUKJJJFZCRTK-UHFFFAOYSA-N 0.000 claims abstract description 10
- 239000004202 carbamide Substances 0.000 claims abstract description 10
- 238000010438 heat treatment Methods 0.000 claims abstract description 4
- 238000001035 drying Methods 0.000 claims description 16
- 206010013786 Dry skin Diseases 0.000 claims description 12
- 239000003990 capacitor Substances 0.000 claims description 9
- 238000010792 warming Methods 0.000 claims description 8
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims description 7
- 238000013019 agitation Methods 0.000 claims description 6
- VYLVYHXQOHJDJL-UHFFFAOYSA-K cerium trichloride Chemical compound Cl[Ce](Cl)Cl VYLVYHXQOHJDJL-UHFFFAOYSA-K 0.000 claims description 6
- 239000000758 substrate Substances 0.000 claims description 6
- KBJMLQFLOWQJNF-UHFFFAOYSA-N nickel(ii) nitrate Chemical compound [Ni+2].[O-][N+]([O-])=O.[O-][N+]([O-])=O KBJMLQFLOWQJNF-UHFFFAOYSA-N 0.000 claims description 5
- 229910021586 Nickel(II) chloride Inorganic materials 0.000 claims description 4
- QMMRZOWCJAIUJA-UHFFFAOYSA-L nickel dichloride Chemical compound Cl[Ni]Cl QMMRZOWCJAIUJA-UHFFFAOYSA-L 0.000 claims description 4
- HSJPMRKMPBAUAU-UHFFFAOYSA-N cerium(3+);trinitrate Chemical compound [Ce+3].[O-][N+]([O-])=O.[O-][N+]([O-])=O.[O-][N+]([O-])=O HSJPMRKMPBAUAU-UHFFFAOYSA-N 0.000 claims description 3
- 239000002048 multi walled nanotube Substances 0.000 claims description 2
- 235000019441 ethanol Nutrition 0.000 claims 2
- 238000005530 etching Methods 0.000 claims 1
- 239000000126 substance Substances 0.000 abstract description 6
- 229910052799 carbon Inorganic materials 0.000 description 10
- 239000000463 material Substances 0.000 description 7
- 238000000034 method Methods 0.000 description 5
- 238000003860 storage Methods 0.000 description 4
- 238000006243 chemical reaction Methods 0.000 description 3
- 229960000935 dehydrated alcohol Drugs 0.000 description 3
- 238000009826 distribution Methods 0.000 description 3
- 238000005516 engineering process Methods 0.000 description 3
- IDGUHHHQCWSQLU-UHFFFAOYSA-N ethanol;hydrate Chemical compound O.CCO IDGUHHHQCWSQLU-UHFFFAOYSA-N 0.000 description 3
- 239000007788 liquid Substances 0.000 description 3
- 239000002245 particle Substances 0.000 description 3
- 230000008569 process Effects 0.000 description 3
- 239000002994 raw material Substances 0.000 description 3
- 150000001768 cations Chemical class 0.000 description 2
- 239000002322 conducting polymer Substances 0.000 description 2
- 229920001940 conductive polymer Polymers 0.000 description 2
- 238000011161 development Methods 0.000 description 2
- 239000003792 electrolyte Substances 0.000 description 2
- 238000004146 energy storage Methods 0.000 description 2
- 150000002500 ions Chemical class 0.000 description 2
- 238000005457 optimization Methods 0.000 description 2
- BASFCYQUMIYNBI-UHFFFAOYSA-N platinum Chemical compound [Pt] BASFCYQUMIYNBI-UHFFFAOYSA-N 0.000 description 2
- 238000006479 redox reaction Methods 0.000 description 2
- 230000002441 reversible effect Effects 0.000 description 2
- 239000002023 wood Substances 0.000 description 2
- 238000010521 absorption reaction Methods 0.000 description 1
- 150000001450 anions Chemical class 0.000 description 1
- 229940075397 calomel Drugs 0.000 description 1
- 239000002134 carbon nanofiber Substances 0.000 description 1
- 239000003575 carbonaceous material Substances 0.000 description 1
- 230000008859 change Effects 0.000 description 1
- 238000004140 cleaning Methods 0.000 description 1
- 150000001875 compounds Chemical class 0.000 description 1
- 125000004122 cyclic group Chemical group 0.000 description 1
- 238000000280 densification Methods 0.000 description 1
- 230000008021 deposition Effects 0.000 description 1
- 238000003795 desorption Methods 0.000 description 1
- 238000001514 detection method Methods 0.000 description 1
- 230000006866 deterioration Effects 0.000 description 1
- 238000010586 diagram Methods 0.000 description 1
- 238000009792 diffusion process Methods 0.000 description 1
- ZOMNIUBKTOKEHS-UHFFFAOYSA-L dimercury dichloride Chemical compound Cl[Hg][Hg]Cl ZOMNIUBKTOKEHS-UHFFFAOYSA-L 0.000 description 1
- 238000007599 discharging Methods 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 230000005611 electricity Effects 0.000 description 1
- 230000005518 electrochemistry Effects 0.000 description 1
- 230000007613 environmental effect Effects 0.000 description 1
- 239000002803 fossil fuel Substances 0.000 description 1
- 229910021389 graphene Inorganic materials 0.000 description 1
- XLYOFNOQVPJJNP-UHFFFAOYSA-M hydroxide Chemical compound [OH-] XLYOFNOQVPJJNP-UHFFFAOYSA-M 0.000 description 1
- 230000007246 mechanism Effects 0.000 description 1
- 229910000000 metal hydroxide Inorganic materials 0.000 description 1
- 229910044991 metal oxide Inorganic materials 0.000 description 1
- 150000004706 metal oxides Chemical class 0.000 description 1
- VNWKTOKETHGBQD-UHFFFAOYSA-N methane Chemical compound C VNWKTOKETHGBQD-UHFFFAOYSA-N 0.000 description 1
- 230000003647 oxidation Effects 0.000 description 1
- 238000007254 oxidation reaction Methods 0.000 description 1
- 229910052697 platinum Inorganic materials 0.000 description 1
- 239000011148 porous material Substances 0.000 description 1
- 238000011160 research Methods 0.000 description 1
- 238000001179 sorption measurement Methods 0.000 description 1
- 230000006641 stabilisation Effects 0.000 description 1
- 238000011105 stabilization Methods 0.000 description 1
- 238000006467 substitution reaction Methods 0.000 description 1
- 238000012360 testing method Methods 0.000 description 1
- 238000012546 transfer Methods 0.000 description 1
- 229910000314 transition metal oxide Inorganic materials 0.000 description 1
- -1 xerogel Chemical compound 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
- H01G11/22—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
- H01G11/36—Nanostructures, e.g. nanofibres, nanotubes or fullerenes
-
- 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
-
- 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
-
- 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
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- Engineering & Computer Science (AREA)
- Power Engineering (AREA)
- Chemical & Material Sciences (AREA)
- Microelectronics & Electronic Packaging (AREA)
- Materials Engineering (AREA)
- Crystallography & Structural Chemistry (AREA)
- Nanotechnology (AREA)
- Manufacturing & Machinery (AREA)
- Electric Double-Layer Capacitors Or The Like (AREA)
Abstract
The invention discloses a kind of preparation methods of multilayer hierarchical structure supercapacitor composite material, comprising the following steps: and S1, nickel foam is etched, is rinsed, ultrasound is cleaned, and it is dry, obtain foam nickel base；S2, nickel source, dodecyl sodium sulfate and urea are dissolved in deionized water, stir, the aqueous solution containing cerium source is then added, stirred, add foam nickel base, be stirred to react, obtain presoma；S3, presoma is filtered, dry, calcining obtains NiO-CeO2Electrode material；S4, by NiO-CeO2Electrode material is mixed with acetone soln, and carbon nanotube is added in stirring, is stirred, and heating volatilizees completely to solution, obtains multilayer hierarchical structure supercapacitor composite material.The invention proposes a kind of preparation methods of multilayer hierarchical structure supercapacitor composite material to effectively increase the chemical property of composite material while reducing composite material preparation cost.
Description
Technical field
The present invention relates to supercapacitor technologies field more particularly to a kind of multilayer hierarchical structure supercapacitor composite woods
The preparation method of material.
Background technique
In recent years, with the exhaustion of fossil fuel and the deterioration of environmental problem, energy problem becomes the master of facing mankind
Problem is wanted, so there is an urgent need for exploitation cleanings, efficient, the sustainable energy.And rechargeable battery and supercapacitor can be with
Conversion and the storage problem of energy are solved very well, so needing to obtain in terms of rechargeable battery and supercapacitor science and technology
It breaks through, to meet the future development of low-carbon and sustainable economy.The charge storage of supercapacitor is based on electrode material and electricity
Solve the electrochemical process between liquid interface.According to energy storage mechanism, supercapacitor can be divided into electric double layer capacitance (EDLCs) and
Fake capacitance.In double layer capacitor, capacitor comes from anion and cation in electrode/electrolyte Interfacial Adsorption capacitor, therefore leads
Wanting influence factor is the specific surface area of electrode material.During the charging process, electronics moves on to anode from cathode, passes through external circuit, yin
Ion is moved to anode, and cation is then mobile to cathode, and during discharge, the direction of motion of electronics and ion can occur inverse
Turn.The electrode material of typical electric double layer capacitance includes porous carbon, such as active carbon, xerogel, carbon nanotube, carbon nano-fiber, Jie
Hole carbon, graphene, carbide.Research shows that the several key factors for influencing electric double layer capacitance performance include the ratio table of carbon-based electrode
Area, electric conductivity and pore size distribution.In most cases, porous carbon materials show specific surface area height and electric conductivity is good
The advantages that good.Compared with electric double layer capacitance, fake capacitance merely with absorption/desorption process of the electrode material of electrode surface and is not owed
Potential deposition realizes charge storage, also realizes charge storage by the quick and reversible redox reaction in electrode body phase.
When reaching specific potential, Reversible redox reaction can occur for electrode material, generate charge to make faradic currents pass through
Supercapacitor.Current main fake capacitance electrode material includes conducting polymer and transition metal oxide/hydroxide.With
Electric double layer capacitance is compared, and fake capacitance can obtain higher energy density, because they can provide a variety of oxidation state, to realize
Efficient redox electric charge transfer, to meet the needs of high-energy ultracapacitor.The energy stores of fake capacitance are mainly
It is completed by the quick faraday's reaction of specific voltage lower electrode material, since faraday's capacitor is to pass through faraday's reaction
Reach high energy storage characteristic with electric double layer collective effect, therefore there is biggish capacitance, large capacity compared to double layer capacitor
Capacitor more tend to using faraday's capacitor, common fake capacitance electrode material has conducting polymer and metal oxide.
Wherein NiO has 2584Fg-1The theoretical capacity of (potential window of 0.5V), good chemical stability and thermal stability, valence
Lattice are cheap, environmental-friendly, easily preparation the advantages that and be widely studied.But its development is hindered due to its low conductivity,
It is modified so studying always in recent years.And due to micrometer/nanometer material have quick redox ability, can contract
Short diffusion path and increasing specific surface area, so being used widely in electrochemistry.
Summary of the invention
Technical problems based on background technology, the invention proposes a kind of multilayer hierarchical structure supercapacitor is compound
The preparation method of material, raw material sources are extensive, easy to operate, controllability is good, reproducibility is high, obtained composite material granular compared with
Small, particle diameter distribution uniformly, large specific surface area effectively increase composite material while reducing composite material preparation cost
Chemical property.
A kind of preparation method of multilayer hierarchical structure supercapacitor composite material proposed by the present invention, including following step
It is rapid:
S1, nickel foam being etched, is rinsed, ultrasound is cleaned, and it is dry, obtain foam nickel base；
S2, nickel source, dodecyl sodium sulfate and urea are dissolved in deionized water, are stirred, be then added and contain cerium source
Aqueous solution, stirring, add foam nickel base, be stirred to react, obtain presoma；
S3, presoma is filtered, dry, calcining obtains NiO-CeO2Electrode material；
S4, by NiO-CeO2Electrode material is mixed with acetone soln, and carbon nanotube is added in stirring, is stirred, heating, to molten
Liquid volatilizees completely, obtains multilayer hierarchical structure supercapacitor composite material.
Preferably, in S1, nickel foam is etched into 10-25min with the HCL aqueous solution that concentration is 2-4mol/L, is then spent
Ionized water rinses, the ultrasound 10-20min in dehydrated alcohol, then the ultrasound 10-20min in acetone soln, clear with deionized water
It washes, in 60-65 DEG C of drying, obtains foam nickel base.
Preferably, in S1, nickel foam is etched into 15min with the HCL aqueous solution that concentration is 3mol/L, then uses deionized water
It rinsing, the ultrasound 15min in dehydrated alcohol, then the ultrasound 15min in acetone soln is cleaned with deionized water, in 60 DEG C of dryings,
Obtain foam nickel base.
Preferably, in S2, nickel source, dodecyl sodium sulfate and urea are dissolved in deionized water, stir 25-35min,
Then the aqueous solution containing cerium source is added dropwise, magnetic agitation 165-185min adds foam nickel base, stirs at 155-165 DEG C
23-25h is reacted, presoma is obtained.
Preferably, in S2, nickel source, cerium source, the molar ratio between foam nickel base are 1.2-1.8:0.036-0.054:2-
4。
Preferably, in S2, nickel source is one of nickel nitrate, nickel chloride.
Preferably, in S2, cerium source is one of cerous nitrate, cerium chloride.
Preferably, in S3, presoma is filtered, in 60-65 DEG C of drying, then in 290-310 DEG C of calcining 2.8-3.2h, is obtained
To NiO-CeO2Electrode material.
Preferably, in S3, presoma is filtered, in 60 DEG C of dryings, then in 300 DEG C of calcining 3h, obtains NiO-CeO2Electricity
Pole material.
Preferably, in S4, by weight by 450-550 parts of NiO-CeO2Electrode material is mixed with acetone soln, and stirring adds
Enter 10-50 parts of carbon nanotubes, stir 1-1.5h, be warming up to 78-82 DEG C, volatilize completely to solution, it is super to obtain multilayer hierarchical structure
Grade capacitor composite.
Preferably, in S4, by weight by 500 parts of NiO-CeO2Electrode material is mixed with acetone soln, and stirring is added 30
Part carbon nanotube, stirs 1h, is warming up to 80 DEG C, volatilizees completely to solution, obtain multilayer hierarchical structure supercapacitor composite wood
Material.
Preferably, in S4, carbon nanotube is multi-walled carbon nanotube, and diameter is 30~50 μm, and heap density is 0.1~0.2g/
cm3。
By optimizing raw material component in the present invention, raw material sources are extensive, then pass through optimization preparation process, operation letter
Just, controllability is good, reproducibility is high, and composite material preparation cost is effectively reduced, and obtained composite material granular is smaller, particle diameter distribution
Uniformly, large specific surface area, wherein carbon nanotube plays the role of skeletal support, NiO-CeO in the composite2Carbon is filled in receive
In the Three Dimensional Cavities of mitron building, perfect NiO-CeO2Gap between particle, so that entire composite substance point
Uniform, densification is dissipated, the stabilization and high conductivity of electrode structure are maintained；Resulting materials have layered structure and high-ratio surface simultaneously
Product, keeps electrode material and electrolyte contacts area bigger, reacts more abundant, to realize the optimization of chemical property.
Detailed description of the invention
Fig. 1 is the SEM figure of gained multilayer hierarchical structure supercapacitor composite material in the embodiment of the present invention 1；
Fig. 2 is that the constant current charge-discharge of gained multilayer hierarchical structure supercapacitor composite material in the embodiment of the present invention 1 is bent
Figure；
Fig. 3 is gained multilayer hierarchical structure supercapacitor composite material in the embodiment of the present invention 1 in different current densities
Under specific discharge capacity curve；
Fig. 4 is gained multilayer hierarchical structure supercapacitor composite material in the embodiment of the present invention 1 in 3mVs-1Sweep speed
Under CV curve.
Specific embodiment
In the following, technical solution of the present invention is described in detail by specific embodiment.
Embodiment 1
A kind of preparation method of multilayer hierarchical structure supercapacitor composite material proposed by the present invention, including following step
It is rapid:
S1, nickel foam is etched into 15min with the HCL aqueous solution that concentration is 3mol/L, is then rinsed with deionized water, in nothing
Ultrasound 15min in water-ethanol, then the ultrasound 15min in acetone soln, are cleaned with deionized water, in 60 DEG C of dryings, obtain foam
Nickel substrate；
S2,1.5mol nickel nitrate, 0.1081g dodecyl sodium sulfate and 0.1081g urea are dissolved in deionized water,
30min is stirred, the aqueous solution containing 0.045mol cerous nitrate is then slowly added dropwise, magnetic agitation 180min adds 3mol bubble
Foam nickel substrate is stirred to react for 24 hours at 160 DEG C, obtains presoma；
S3, presoma is filtered, in 60 DEG C of dryings, then in 300 DEG C of calcining 3h, obtains NiO-CeO2Electrode material；
S4, by weight by 500mgNiO-CeO2Electrode material is mixed with acetone soln, and 30mg carbon nanometer is added in stirring
Pipe stirs 1h, is warming up to 80 DEG C, volatilizees completely to solution, obtain multilayer hierarchical structure supercapacitor composite material.
Performance detection is carried out to multilayer hierarchical structure supercapacitor composite material obtained in the embodiment of the present invention 1, is obtained
To Fig. 1, Fig. 2, Fig. 3 and Fig. 4；Wherein, Fig. 1 is gained multilayer hierarchical structure supercapacitor composite wood in the embodiment of the present invention 1
The SEM of material schemes；Fig. 2 is the constant current charge-discharge of gained multilayer hierarchical structure supercapacitor composite material in the embodiment of the present invention 1
Diagram；Fig. 3 is gained multilayer hierarchical structure supercapacitor composite material in the embodiment of the present invention 1 under different current densities
Specific discharge capacity curve；Fig. 4 is gained multilayer hierarchical structure supercapacitor composite material in the embodiment of the present invention 1 in 3mV
The CV curve of s-1 swept under speed.
As shown in Figure 1, multilayer hierarchical structure supercapacitor composite material is flaky nanometer structure.
By Fig. 2, Fig. 3 it is found that by will obtained multilayer hierarchical structure supercapacitor composite material as working electrode,
Using platinized platinum as auxiliary electrode, calomel electrode is reference electrode, with 1Ag-1、2A·g-1Current density carried out between 0-0.5V
Constant current charge-discharge obtains Fig. 2 and Fig. 3, by Fig. 2, Fig. 3 it is found that its discharge capacity is respectively 1512.88Fg-1、1463F·g-1, it is known that the good specific discharge capacity of multilayer hierarchical structure supercapacitor composite material and fast charging and discharging ability.
As shown in Figure 4, multilayer hierarchical structure supercapacitor composite material is in 3mVs-1Sweep and carry out cyclic voltammetric under speed
Test obtains CV curve, has a pair of symmetrical redox peaks, is located at 0.308V, 0.492V, shows multilayer point
Level structure supercapacitor composite material has good invertibity and chemical property.
Embodiment 2
A kind of preparation method of multilayer hierarchical structure supercapacitor composite material proposed by the present invention, including following step
It is rapid:
S1, nickel foam is etched into 20min with the HCL aqueous solution that concentration is 2.5mol/L, is then rinsed with deionized water,
Ultrasound 16min in dehydrated alcohol, then the ultrasound 16min in acetone soln, are cleaned with deionized water, in 64 DEG C of dryings, are steeped
Foam nickel substrate；
S2,1.6mol nickel source, dodecyl sodium sulfate and urea are dissolved in deionized water, stir 32min, then drips
Add the aqueous solution containing 0.05mol cerium source, magnetic agitation 170min adds 3.5mol foam nickel base, anti-in 158 DEG C of stirrings
24.5h is answered, presoma is obtained；
S3, presoma is filtered, in 64 DEG C of dryings, then in 205 DEG C of calcining 2.9h, obtains NiO-CeO2Electrode material；
S4, by weight by 480 parts of NiO-CeO2Electrode material is mixed with acetone soln, and 30 parts of carbon nanometers are added in stirring
Pipe stirs 1.2h, is warming up to 80 DEG C, volatilizees completely to solution, obtain multilayer hierarchical structure supercapacitor composite material.
Embodiment 3
A kind of preparation method of multilayer hierarchical structure supercapacitor composite material proposed by the present invention, including following step
It is rapid:
S1, nickel foam being etched, is rinsed, ultrasound is cleaned, and it is dry, obtain foam nickel base；
S2, nickel source, dodecyl sodium sulfate and urea are dissolved in deionized water, are stirred, be then added and contain cerium source
Aqueous solution, stirring, add foam nickel base, be stirred to react, obtain presoma；
S3, presoma is filtered, dry, calcining obtains NiO-CeO2Electrode material；
S4, by NiO-CeO2Electrode material is mixed with acetone soln, and carbon nanotube is added in stirring, is stirred, heating, to molten
Liquid volatilizees completely, obtains multilayer hierarchical structure supercapacitor composite material.
Embodiment 4
A kind of preparation method of multilayer hierarchical structure supercapacitor composite material proposed by the present invention, including following step
It is rapid:
S1, nickel foam is etched into 25min with the HCL aqueous solution that concentration is 2mol/L, is then rinsed with deionized water, in nothing
Ultrasound 10min in water-ethanol, then the ultrasound 20min in acetone soln, are cleaned with deionized water, in 65 DEG C of dryings, obtain foam
Nickel substrate；
S2, nickel chloride, dodecyl sodium sulfate and urea are dissolved in deionized water, stir 25min, be then added dropwise and contain
There is the aqueous solution of cerium chloride, magnetic agitation 185min adds foam nickel base, is stirred to react 25h at 155 DEG C, obtains forerunner
Body；Wherein, nickel chloride, cerium chloride, the molar ratio between foam nickel base are 1.2:0.04:2.4；
S3, presoma is filtered, in 65 DEG C of dryings, then in 290 DEG C of calcining 3.2h, obtains NiO-CeO2Electrode material；
S4, by weight by 450 parts of NiO-CeO2Electrode material is mixed with acetone soln, and 10 parts of carbon nanometers are added in stirring
Pipe stirs 1h, is warming up to 78 DEG C, volatilizees completely to solution, obtain multilayer hierarchical structure supercapacitor composite material.
Embodiment 5
A kind of preparation method of multilayer hierarchical structure supercapacitor composite material proposed by the present invention, including following step
It is rapid:
S1, nickel foam is etched into 10min with the HCL aqueous solution that concentration is 4mol/L, is then rinsed with deionized water, in nothing
Ultrasound 20min in water-ethanol, then the ultrasound 10min in acetone soln, are cleaned with deionized water, in 62 DEG C of dryings, obtain foam
Nickel substrate；
S2, nickel nitrate, dodecyl sodium sulfate and urea are dissolved in deionized water, stir 35min, be then added dropwise and contain
There is the aqueous solution of cerium chloride, magnetic agitation 165min adds foam nickel base, is stirred to react 23h at 165 DEG C, obtains forerunner
Body；Wherein, nickel nitrate, cerium chloride, the molar ratio between foam nickel base are 1.8:0.054:3.5；
S3, presoma is filtered, in 62 DEG C of dryings, then in 295 DEG C of calcining 3.1h, obtains NiO-CeO2Electrode material；
S4, by weight by 520 parts of NiO-CeO2Electrode material is mixed with acetone soln, and 40 parts of carbon nanometers are added in stirring
Pipe stirs 1.4h, is warming up to 80 DEG C, volatilizees completely to solution, obtain multilayer hierarchical structure supercapacitor composite material.
The foregoing is only a preferred embodiment of the present invention, but scope of protection of the present invention is not limited thereto,
Anyone skilled in the art in the technical scope disclosed by the present invention, according to the technique and scheme of the present invention and its
Inventive concept is subject to equivalent substitution or change, should be covered by the protection scope of the present invention.
Claims (10)
1. a kind of preparation method of multilayer hierarchical structure supercapacitor composite material, which comprises the following steps:
S1, nickel foam being etched, is rinsed, ultrasound is cleaned, and it is dry, obtain foam nickel base；
S2, nickel source, dodecyl sodium sulfate and urea are dissolved in deionized water, stir, the water containing cerium source is then added
Solution, stirring, adds foam nickel base, is stirred to react, obtain presoma；
S3, presoma is filtered, dry, calcining obtains NiO-CeO2Electrode material；
S4, by NiO-CeO2Electrode material is mixed with acetone soln, and carbon nanotube is added in stirring, is stirred, and heating is complete to solution
Volatilization, obtains multilayer hierarchical structure supercapacitor composite material.
2. the preparation method of multilayer hierarchical structure supercapacitor composite material according to claim 1, which is characterized in that S1
In, nickel foam is etched into 10-25min with the HCL aqueous solution that concentration is 2-4mol/L, is then rinsed with deionized water, anhydrous
Ultrasound 10-20min in ethyl alcohol, then the ultrasound 10-20min in acetone soln, are cleaned with deionized water, in 60-65 DEG C of drying, are obtained
To foam nickel base.
3. the preparation method of multilayer hierarchical structure supercapacitor composite material according to claim 1 or claim 2, feature exist
In in S1, then the HCL aqueous solution etching 15min for being 3mol/L with concentration by nickel foam is rinsed with deionized water, anhydrous
Ultrasound 15min in ethyl alcohol, then the ultrasound 15min in acetone soln, are cleaned with deionized water, in 60 DEG C of dryings, obtain nickel foam
Substrate.
4. the preparation method of multilayer hierarchical structure supercapacitor composite material described in any one of -3 according to claim 1,
It is characterized in that, in S2, nickel source, dodecyl sodium sulfate and urea is dissolved in deionized water, stir 25-35min, then drip
Add the aqueous solution containing cerium source, magnetic agitation 165-185min adds foam nickel base, is stirred to react 23- at 155-165 DEG C
25h obtains presoma.
5. the preparation method of multilayer hierarchical structure supercapacitor composite material described in any one of -4 according to claim 1,
It is characterized in that, in S2, nickel source, cerium source, the molar ratio between foam nickel base are 1.2-1.8:0.036-0.054:2-4.
6. the preparation method of multilayer hierarchical structure supercapacitor composite material described in any one of -5 according to claim 1,
It is characterized in that, in S2, nickel source is one of nickel nitrate, nickel chloride.
7. the preparation method of multilayer hierarchical structure supercapacitor composite material described in any one of -6 according to claim 1,
It is characterized in that, in S2, cerium source is one of cerous nitrate, cerium chloride.
8. the preparation method of multilayer hierarchical structure supercapacitor composite material described in any one of -7 according to claim 1,
It is characterized in that, in S3, presoma is filtered, in 60-65 DEG C of drying, then in 290-310 DEG C of calcining 2.8-3.2h, obtain NiO-
CeO2Electrode material；Preferably, in S3, presoma is filtered, in 60 DEG C of dryings, then in 300 DEG C of calcining 3h, obtains NiO-
CeO2Electrode material.
9. the preparation method of multilayer hierarchical structure supercapacitor composite material described in any one of -8 according to claim 1,
It is characterized in that, in S4, by weight by 450-550 parts of NiO-CeO2Electrode material is mixed with acetone soln, and 10- is added in stirring
50 parts of carbon nanotubes stir 1-1.5h, are warming up to 78-82 DEG C, volatilize completely to solution, obtain multilayer hierarchical structure super capacitor
Device composite material；Preferably, by weight by 500 parts of NiO-CeO2Electrode material is mixed with acetone soln, and stirring is added 30 parts
Carbon nanotube stirs 1h, is warming up to 80 DEG C, volatilizees completely to solution, obtain multilayer hierarchical structure supercapacitor composite material.
10. the preparation method of multilayer hierarchical structure supercapacitor composite material described in any one of -9 according to claim 1,
It is characterized in that, in S4, carbon nanotube is multi-walled carbon nanotube, and diameter is 30~50 μm, and heap density is 0.1~0.2g/cm3。
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| CN111710531A (en) * | 2020-05-20 | 2020-09-25 | 上海应用技术大学 | Ce-NiO @ Ni-MOF composite material and preparation method and application thereof |
| CN112700969A (en) * | 2020-12-09 | 2021-04-23 | 大连理工大学 | Sheet CeO2/Co1.29Ni1.71O4 electrode material and preparation method thereof |
| CN113830838A (en) * | 2021-07-26 | 2021-12-24 | 江汉大学 | Preparation method and application of magnesium cobaltate |
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| CN112700969A (en) * | 2020-12-09 | 2021-04-23 | 大连理工大学 | Sheet CeO2/Co1.29Ni1.71O4 electrode material and preparation method thereof |
| CN112700969B (en) * | 2020-12-09 | 2022-04-08 | 大连理工大学 | Sheet CeO2/Co1.29Ni1.71O4 electrode material and preparation method thereof |
| CN113830838A (en) * | 2021-07-26 | 2021-12-24 | 江汉大学 | Preparation method and application of magnesium cobaltate |
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