CN108735517A - A kind of basic zinc carbonate electrode material for super capacitor and preparation method thereof - Google Patents
A kind of basic zinc carbonate electrode material for super capacitor and preparation method thereof Download PDFInfo
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- CN108735517A CN108735517A CN201810534409.XA CN201810534409A CN108735517A CN 108735517 A CN108735517 A CN 108735517A CN 201810534409 A CN201810534409 A CN 201810534409A CN 108735517 A CN108735517 A CN 108735517A
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- nickel foam
- preparation
- electrode material
- super capacitor
- urea
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- 239000007772 electrode material Substances 0.000 title claims abstract description 22
- 238000002360 preparation method Methods 0.000 title claims abstract description 21
- 239000003990 capacitor Substances 0.000 title claims abstract description 18
- UOURRHZRLGCVDA-UHFFFAOYSA-D pentazinc;dicarbonate;hexahydroxide Chemical compound [OH-].[OH-].[OH-].[OH-].[OH-].[OH-].[Zn+2].[Zn+2].[Zn+2].[Zn+2].[Zn+2].[O-]C([O-])=O.[O-]C([O-])=O UOURRHZRLGCVDA-UHFFFAOYSA-D 0.000 title claims abstract description 17
- PXHVJJICTQNCMI-UHFFFAOYSA-N Nickel Chemical compound [Ni] PXHVJJICTQNCMI-UHFFFAOYSA-N 0.000 claims abstract description 80
- 239000006260 foam Substances 0.000 claims abstract description 41
- 229910052759 nickel Inorganic materials 0.000 claims abstract description 40
- ONDPHDOFVYQSGI-UHFFFAOYSA-N zinc nitrate Chemical compound [Zn+2].[O-][N+]([O-])=O.[O-][N+]([O-])=O ONDPHDOFVYQSGI-UHFFFAOYSA-N 0.000 claims abstract description 32
- BNGXYYYYKUGPPF-UHFFFAOYSA-M (3-methylphenyl)methyl-triphenylphosphanium;chloride Chemical compound [Cl-].CC1=CC=CC(C[P+](C=2C=CC=CC=2)(C=2C=CC=CC=2)C=2C=CC=CC=2)=C1 BNGXYYYYKUGPPF-UHFFFAOYSA-M 0.000 claims abstract description 16
- XSQUKJJJFZCRTK-UHFFFAOYSA-N Urea Chemical compound NC(N)=O XSQUKJJJFZCRTK-UHFFFAOYSA-N 0.000 claims abstract description 16
- 239000004202 carbamide Substances 0.000 claims abstract description 16
- 239000011259 mixed solution Substances 0.000 claims abstract description 15
- 239000000243 solution Substances 0.000 claims abstract description 10
- 238000001027 hydrothermal synthesis Methods 0.000 claims abstract description 8
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 5
- 238000006243 chemical reaction Methods 0.000 claims abstract description 4
- 230000007935 neutral effect Effects 0.000 claims abstract description 4
- 239000008367 deionised water Substances 0.000 claims abstract description 3
- 229910021641 deionized water Inorganic materials 0.000 claims abstract description 3
- 238000005554 pickling Methods 0.000 claims abstract description 3
- 238000011065 in-situ storage Methods 0.000 claims description 15
- VEXZGXHMUGYJMC-UHFFFAOYSA-N Hydrochloric acid Chemical compound Cl VEXZGXHMUGYJMC-UHFFFAOYSA-N 0.000 claims description 10
- 238000002604 ultrasonography Methods 0.000 claims description 4
- 239000003513 alkali Substances 0.000 claims description 3
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 claims 1
- HCHKCACWOHOZIP-UHFFFAOYSA-N Zinc Chemical compound [Zn] HCHKCACWOHOZIP-UHFFFAOYSA-N 0.000 claims 1
- 229910052799 carbon Inorganic materials 0.000 claims 1
- 239000011701 zinc Substances 0.000 claims 1
- 229910052725 zinc Inorganic materials 0.000 claims 1
- 238000000034 method Methods 0.000 abstract description 4
- 238000011031 large-scale manufacturing process Methods 0.000 abstract description 2
- FMRLDPWIRHBCCC-UHFFFAOYSA-L Zinc carbonate Chemical compound [Zn+2].[O-]C([O-])=O FMRLDPWIRHBCCC-UHFFFAOYSA-L 0.000 description 14
- 239000000463 material Substances 0.000 description 13
- 230000005611 electricity Effects 0.000 description 4
- BASFCYQUMIYNBI-UHFFFAOYSA-N platinum Chemical compound [Pt] BASFCYQUMIYNBI-UHFFFAOYSA-N 0.000 description 4
- 239000003792 electrolyte Substances 0.000 description 3
- 239000011149 active material Substances 0.000 description 2
- 239000011230 binding agent Substances 0.000 description 2
- 239000003575 carbonaceous material Substances 0.000 description 2
- 239000003153 chemical reaction reagent Substances 0.000 description 2
- 238000002484 cyclic voltammetry Methods 0.000 description 2
- ZOMNIUBKTOKEHS-UHFFFAOYSA-L dimercury dichloride Chemical class Cl[Hg][Hg]Cl ZOMNIUBKTOKEHS-UHFFFAOYSA-L 0.000 description 2
- 238000005516 engineering process Methods 0.000 description 2
- 229910052751 metal Inorganic materials 0.000 description 2
- 239000002184 metal Substances 0.000 description 2
- 229910052697 platinum Inorganic materials 0.000 description 2
- 229910000010 zinc carbonate Inorganic materials 0.000 description 2
- 235000004416 zinc carbonate Nutrition 0.000 description 2
- 239000011667 zinc carbonate Substances 0.000 description 2
- 230000000903 blocking effect Effects 0.000 description 1
- 239000002131 composite material Substances 0.000 description 1
- 239000004020 conductor Substances 0.000 description 1
- 125000004122 cyclic group Chemical group 0.000 description 1
- 238000002242 deionisation method Methods 0.000 description 1
- 238000010586 diagram Methods 0.000 description 1
- 238000000840 electrochemical analysis Methods 0.000 description 1
- 239000002001 electrolyte material Substances 0.000 description 1
- 238000004146 energy storage Methods 0.000 description 1
- 238000005530 etching Methods 0.000 description 1
- 239000002803 fossil fuel Substances 0.000 description 1
- 150000002500 ions Chemical class 0.000 description 1
- 239000007788 liquid Substances 0.000 description 1
- 229910044991 metal oxide Inorganic materials 0.000 description 1
- 150000004706 metal oxides Chemical class 0.000 description 1
- 239000000203 mixture Substances 0.000 description 1
- 239000002135 nanosheet Substances 0.000 description 1
- 230000001376 precipitating effect Effects 0.000 description 1
- 238000003860 storage Methods 0.000 description 1
- 238000010301 surface-oxidation reaction Methods 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
- H01G11/84—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
Landscapes
- Engineering & Computer Science (AREA)
- Power Engineering (AREA)
- Microelectronics & Electronic Packaging (AREA)
- Chemical & Material Sciences (AREA)
- Materials Engineering (AREA)
- Manufacturing & Machinery (AREA)
- Electric Double-Layer Capacitors Or The Like (AREA)
- Fixed Capacitors And Capacitor Manufacturing Machines (AREA)
Abstract
The invention discloses a kind of basic zinc carbonate electrode material for super capacitor and preparation method thereof, and method includes the following steps:(1) nickel foam is removed into surface film oxide through pickling;Deionized water is washed to neutral and dry;(2) it prepares zinc nitrate, aluminum nitrate and urea to obtain mixed solution.The molar ratio of the molar concentration 0.05-0.15mol/L of urea in solution, zinc nitrate and aluminum nitrate is 5~1:1, urea and zinc nitrate, aluminum nitrate total amount molar ratio be 5~2:1;(3) nickel foam after processing is put into the mixed solution of step (2) ultrasonic;(4) mixed solution and nickel foam are put into reaction kettle and carry out hydro-thermal process;Hydrothermal temperature is 100-140 DEG C, and the hydro-thermal time is 1-20 hours.(5) hydro-thermal reaction completes postcooling, takes out nickel foam, washs, dry.The preparation method of the present invention is simple, environmental-friendly at low cost, is easy to large-scale production.
Description
Technical field
The present invention relates to a kind of basic zinc carbonate electrode material for super capacitor and preparation method thereof.
Background technology
Energy storage system is the important link of peak load regulation network and generation of electricity by new energy, and the continuous exhaustion of fossil fuel is again into one
Step have stimulated effective storage research of solar energy and wind energy.Ultracapacitor has high-specific-power, quick charge/discharge, Yi Jichang
The characteristics of cycle life, and receive significant attention.
Electrode material for super capacitor includes carbon-based material, metal oxide-type and its composite material.Carbon material electrode fills
Discharge rate, but specific capacitance is relatively small, metal oxide electrode, and specific capacitance is high but electric conductivity is poor.On the other hand, usually
Electrode of super capacitor be to be made of active material, conductive material and binder, the internal resistance of ultracapacitor carrys out self-electrode material
Diffusional resistance and the electrolyte electricity that the electron drag of material, the contact resistance of electrode and current collector, ion move in micropore
Resistance etc..Wherein on the one hand the presence of binder increases electrode resistance, while also blocking the effective of electrolyte and active material
Contact, itself also has certain weight, forms certain dead volume.
Invention content
For the technology above problem, the present invention provides a kind of preparation side of basic zinc carbonate electrode material for super capacitor
Method includes the following steps:
(1) nickel foam is removed into surface film oxide through pickling;Deionized water is washed to neutral and dry;
(2) it prepares zinc nitrate, aluminum nitrate and urea to obtain mixed solution.The molar concentration 0.05- of urea in solution
The molar ratio of 0.15mol/L, zinc nitrate and aluminum nitrate is 5~1:1, urea and zinc nitrate, aluminum nitrate total amount molar ratio be 5~
2:1;
(3) nickel foam after processing is put into the mixed solution of step (2) ultrasonic;
(4) mixed solution and nickel foam are put into reaction kettle and carry out hydro-thermal process;Hydrothermal temperature is 100-140 DEG C, water
The hot time is 1-20 hours.
(5) hydro-thermal reaction completes postcooling, takes out nickel foam, washs, dry, obtains the alkali of nickel foam surface in situ growth
Formula zinc carbonate combination electrode material.
Further, in the above-mentioned technical solutions, in step (1), nickel foam is put into hydrochloric acid and impregnates ultrasound, remove table
Surface oxidation film, hydrochloric acid molar concentration are 0.5-2mol/L, ultrasonic time 10-30 minutes.
Further, in the above-mentioned technical solutions, in step (3), ultrasonic time be 10-30 minutes, nickel foam with mix
The volume ratio of solution is 1:2~5.
Further, in the above-mentioned technical solutions, in step (4), nickel foam is with mixed solution product than being 1:2~5.
The present invention provides the basic zinc carbonate electrode material for super capacitor that above-mentioned preparation method obtains.
The preparation method of the present invention is simple, and zinc nitrate, aluminum nitrate and precipitating reagent urea are industrialization conventional reagent, environment
It is friendly at low cost, it is easy to large-scale production.The basic zinc carbonate of nickel foam surface in situ growth is two-dimentional sawtooth piece to orderly just
Hexagonal nanosheet shape, this combination electrode material show higher specific capacitance and cyclical stability in electro-chemical test.
Description of the drawings
Fig. 1 is the SEM figures that nickel foam surface in situ prepared by the embodiment of the present invention 1 grows basic carbonate Zinc material;
Fig. 2 is basic carbonate Zinc material XRD diagram prepared by embodiment 1;
Fig. 3 is that the nickel foam surface in situ of preparation prepared by embodiment 2 grows the SEM figures of basic carbonate Zinc material;
Fig. 4 is that nickel foam surface in situ prepared by embodiment 1 grows basic carbonate Zinc material under different scanning rates
Cyclic voltammetry curve figure;
Fig. 5 is that embodiment 2 prepares nickel foam surface in situ growth basic carbonate Zinc material following under different scanning rates
Ring volt-ampere curve figure;
Fig. 6 is the constant current charge-discharge curve that nickel foam surface in situ prepared by embodiment 1 grows basic carbonate Zinc material;
Fig. 7 is the SEM figures that nickel foam surface in situ prepared by the embodiment of the present invention 3 grows basic carbonate Zinc material;
Fig. 8 is the SEM figures that nickel foam surface in situ prepared by the embodiment of the present invention 4 grows basic carbonate Zinc material;
Fig. 9 is the SEM figures that nickel foam surface in situ prepared by the embodiment of the present invention 5 grows basic carbonate Zinc material.
Specific implementation mode
Nickel foam contains foam metal factory, thickness 1.5mm purchased from Jiangsu good hundred million in embodiment.
Embodiment 1
A kind of basic zinc carbonate electrode material for super capacitor and preparation method thereof, implements according to the following steps.
(1) nickel foam is put into a concentration of 2mol/L hydrochloric acid and impregnates ultrasound 10 minutes, remove surface film oxide, deionization
Water is washed to neutral and dry;
(2) zinc nitrate, aluminum nitrate and urea is taken to prepare to obtain mixed solution.A concentration of 0.01mol/ of zinc nitrate in solution
L, a concentration of 0.002mol/L of aluminum nitrate, the molar concentration 0.06mol/L of urea.
(3) nickel foam after processing is put into ultrasound 10 minutes in the mixed solution of step (2).Nickel foam and above-mentioned mixed liquor
Volume ratio be 1:3.
(4) mixed solution and nickel foam are put into reaction kettle and carry out hydro-thermal process;Nickel foam is with etching liquid volume ratio
1:3, hydrothermal temperature is 120 DEG C, and the hydro-thermal time is 2 hours.
(5) hydro-thermal reaction completes postcooling, takes out nickel foam, washs, dry, obtains the alkali of nickel foam surface in situ growth
Formula zinc carbonate combination electrode material.
Fig. 4 is that the nickel foam surface in situ prepared grows cyclic voltammetric of the basic carbonate Zinc material under different scanning rates
Curve graph;Fig. 6 is the constant current charge-discharge curve of the nickel foam surface in situ growth basic carbonate Zinc material prepared;Test process is
Three-electrode system is to electrode, using the combination electrode of preparation as work electricity with platinum electrode using saturated calomel electrode as reference electrode
Pole, electrolyte are 6M KOH, and the constant current charge-discharge under 1A/g current densities, specific capacitance is up to 1600F/g.
Embodiment 2
A kind of basic zinc carbonate electrode material for super capacitor and preparation method thereof, step with embodiment 1, unlike,
In step (4), the hydro-thermal time is 8 hours.Fig. 5 is that the nickel foam surface in situ growth basic carbonate Zinc material prepared is swept in difference
Retouch the cyclic voltammetry curve figure under rate.Test process is three-electrode system, using saturated calomel electrode as reference electrode, with platinum electricity
Extremely to electrode, using the combination electrode of preparation as working electrode, electrolyte is 6M KOH, when sweep speed is 50mV/s, than
Capacitance is up to 1100F/g.
Embodiment 3
A kind of basic zinc carbonate electrode material for super capacitor and preparation method thereof, step with embodiment 1, unlike,
In step (4), the hydro-thermal time is 12 hours.
Embodiment 4
A kind of basic zinc carbonate electrode material for super capacitor and preparation method thereof, step with embodiment 1, unlike,
In step (2), zinc nitrate, aluminum nitrate and urea is taken to prepare to obtain mixed solution.A concentration of 0.01mol/ of zinc nitrate in solution
L, a concentration of 0.005mol/L of aluminum nitrate, the molar concentration 0.075mol/L of urea.
Embodiment 5
A kind of basic zinc carbonate electrode material for super capacitor and preparation method thereof, step with embodiment 1, unlike,
In step (2), zinc nitrate, aluminum nitrate and urea is taken to prepare to obtain mixed solution.A concentration of 0.01mol/ of zinc nitrate in solution
L, a concentration of 0.01mol/L of aluminum nitrate, the molar concentration 0.1mol/L of urea.
Claims (5)
1. a kind of preparation method of basic zinc carbonate electrode material for super capacitor, it is characterised in that include the following steps:
(1) nickel foam is removed into surface film oxide through pickling;Deionized water is washed to neutral and dry;
(2) it prepares zinc nitrate, aluminum nitrate and urea to obtain mixed solution.The molar concentration 0.05- of urea in solution
The molar ratio of 0.15mol/L, zinc nitrate and aluminum nitrate is 5~1:1, urea and zinc nitrate, aluminum nitrate total amount molar ratio be 5~
2:1;
(3) nickel foam after processing is put into the mixed solution of step (2) ultrasonic;
(4) mixed solution and nickel foam are put into reaction kettle and carry out hydro-thermal process;Hydrothermal temperature is 100-140 DEG C, when hydro-thermal
Between be 1-20 hours.
(5) hydro-thermal reaction completes postcooling, takes out nickel foam, washs, dry, obtains the alkali formula carbon of nickel foam surface in situ growth
Sour zinc combination electrode material.
2. a kind of preparation method of basic zinc carbonate electrode material for super capacitor according to claim 1, it is characterised in that:
In step (1), nickel foam is put into hydrochloric acid and impregnates ultrasound, remove surface film oxide, hydrochloric acid molar concentration is 0.5-2.0mol/
L, ultrasonic time 10-30 minutes.
3. a kind of preparation method of basic zinc carbonate electrode material for super capacitor according to claim 1, it is characterised in that:
In step (3), ultrasonic time is 10-30 minutes, and the volume ratio of nickel foam and mixed liquor is 1:2~5.
4. a kind of preparation method of basic zinc carbonate electrode material for super capacitor according to claim 1, it is characterised in that:
In step (4), nickel foam is 1 with mixed liquor volume ratio:2~5.
5. the basic zinc carbonate electrode material for super capacitor that the preparation method as described in Claims 1 to 4 any one obtains.
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CN201810534409.XA CN108735517B (en) | 2018-05-30 | 2018-05-30 | Basic zinc carbonate supercapacitor electrode material and preparation method thereof |
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CN108735517B CN108735517B (en) | 2020-09-25 |
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CN103887082A (en) * | 2014-03-17 | 2014-06-25 | 湖州师范学院 | Method for growing hexagonal Co(OH)2 on surface of metal foamed nickel |
CN104907036A (en) * | 2015-05-15 | 2015-09-16 | 燕山大学 | Graded dandelion-flower-shaped ZnO-Al2O3 compound and preparation method therefor |
CN104993106A (en) * | 2015-05-27 | 2015-10-21 | 三峡大学 | Zinc-based composite material basic zinc carbonate, preparation method and application thereof |
CN105819849A (en) * | 2016-05-04 | 2016-08-03 | 武汉工程大学 | Zinc aluminate nanometer powder and preparing method thereof |
CN105914046A (en) * | 2016-04-14 | 2016-08-31 | 深圳大学 | Preparation method for hydroxyl-cobalt-carbonate thin-film super capacitor electrode material |
JP2017043505A (en) * | 2015-08-25 | 2017-03-02 | 住友金属鉱山株式会社 | Manufacturing method of uv light shielding material particulates, uv light shielding material particulate dispersoid using uv light shielding material particulates, and uv light shielding body |
CN107051565A (en) * | 2017-05-24 | 2017-08-18 | 中国科学院化学研究所 | A kind of performance alkali formula carbonate electrolysis water catalyst and preparation method and application |
-
2018
- 2018-05-30 CN CN201810534409.XA patent/CN108735517B/en active Active
Patent Citations (7)
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---|---|---|---|---|
CN103887082A (en) * | 2014-03-17 | 2014-06-25 | 湖州师范学院 | Method for growing hexagonal Co(OH)2 on surface of metal foamed nickel |
CN104907036A (en) * | 2015-05-15 | 2015-09-16 | 燕山大学 | Graded dandelion-flower-shaped ZnO-Al2O3 compound and preparation method therefor |
CN104993106A (en) * | 2015-05-27 | 2015-10-21 | 三峡大学 | Zinc-based composite material basic zinc carbonate, preparation method and application thereof |
JP2017043505A (en) * | 2015-08-25 | 2017-03-02 | 住友金属鉱山株式会社 | Manufacturing method of uv light shielding material particulates, uv light shielding material particulate dispersoid using uv light shielding material particulates, and uv light shielding body |
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CN107051565A (en) * | 2017-05-24 | 2017-08-18 | 中国科学院化学研究所 | A kind of performance alkali formula carbonate electrolysis water catalyst and preparation method and application |
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