CN110395774A - A kind of preparation method and application of cobalt acid nickel porous material - Google Patents
A kind of preparation method and application of cobalt acid nickel porous material Download PDFInfo
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- CN110395774A CN110395774A CN201910656976.7A CN201910656976A CN110395774A CN 110395774 A CN110395774 A CN 110395774A CN 201910656976 A CN201910656976 A CN 201910656976A CN 110395774 A CN110395774 A CN 110395774A
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- cobalt
- cobalt acid
- preparation
- porous material
- acid nickel
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- PXHVJJICTQNCMI-UHFFFAOYSA-N Nickel Chemical compound [Ni] PXHVJJICTQNCMI-UHFFFAOYSA-N 0.000 title claims abstract description 95
- 229910017052 cobalt Inorganic materials 0.000 title claims abstract description 47
- 239000010941 cobalt Substances 0.000 title claims abstract description 47
- GUTLYIVDDKVIGB-UHFFFAOYSA-N cobalt atom Chemical compound [Co] GUTLYIVDDKVIGB-UHFFFAOYSA-N 0.000 title claims abstract description 47
- 229910052759 nickel Inorganic materials 0.000 title claims abstract description 45
- 239000002253 acid Substances 0.000 title claims abstract description 42
- 238000002360 preparation method Methods 0.000 title claims abstract description 29
- 239000011148 porous material Substances 0.000 title claims description 32
- 238000010438 heat treatment Methods 0.000 claims abstract description 18
- 150000001875 compounds Chemical class 0.000 claims abstract description 14
- 239000011259 mixed solution Substances 0.000 claims abstract description 13
- 238000001816 cooling Methods 0.000 claims abstract description 10
- 239000003153 chemical reaction reagent Substances 0.000 claims abstract description 7
- XLJKHNWPARRRJB-UHFFFAOYSA-N cobalt(2+) Chemical compound [Co+2] XLJKHNWPARRRJB-UHFFFAOYSA-N 0.000 claims abstract description 7
- 230000001376 precipitating effect Effects 0.000 claims abstract description 7
- 229910001429 cobalt ion Inorganic materials 0.000 claims abstract description 6
- FKNQFGJONOIPTF-UHFFFAOYSA-N Sodium cation Chemical compound [Na+] FKNQFGJONOIPTF-UHFFFAOYSA-N 0.000 claims abstract description 5
- 229910001453 nickel ion Inorganic materials 0.000 claims abstract description 5
- 229910001415 sodium ion Inorganic materials 0.000 claims abstract description 5
- 239000003960 organic solvent Substances 0.000 claims abstract description 4
- VWDWKYIASSYTQR-UHFFFAOYSA-N sodium nitrate Chemical compound [Na+].[O-][N+]([O-])=O VWDWKYIASSYTQR-UHFFFAOYSA-N 0.000 claims description 24
- 229940068918 polyethylene glycol 400 Drugs 0.000 claims description 13
- 239000004202 carbamide Substances 0.000 claims description 12
- 239000004317 sodium nitrate Substances 0.000 claims description 12
- 235000010344 sodium nitrate Nutrition 0.000 claims description 12
- XSQUKJJJFZCRTK-UHFFFAOYSA-N urea group Chemical group NC(=O)N XSQUKJJJFZCRTK-UHFFFAOYSA-N 0.000 claims description 12
- 238000000034 method Methods 0.000 claims description 8
- AOPCKOPZYFFEDA-UHFFFAOYSA-N nickel(2+);dinitrate;hexahydrate Chemical group O.O.O.O.O.O.[Ni+2].[O-][N+]([O-])=O.[O-][N+]([O-])=O AOPCKOPZYFFEDA-UHFFFAOYSA-N 0.000 claims description 8
- 239000000126 substance Substances 0.000 claims description 7
- 239000002202 Polyethylene glycol Substances 0.000 claims description 6
- 229920001223 polyethylene glycol Polymers 0.000 claims description 6
- UFMZWBIQTDUYBN-UHFFFAOYSA-N cobalt dinitrate Chemical compound [Co+2].[O-][N+]([O-])=O.[O-][N+]([O-])=O UFMZWBIQTDUYBN-UHFFFAOYSA-N 0.000 claims description 5
- 229910001981 cobalt nitrate Inorganic materials 0.000 claims description 5
- 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
- FGIUAXJPYTZDNR-UHFFFAOYSA-N potassium nitrate Chemical compound [K+].[O-][N+]([O-])=O FGIUAXJPYTZDNR-UHFFFAOYSA-N 0.000 claims description 5
- CDBYLPFSWZWCQE-UHFFFAOYSA-L Sodium Carbonate Chemical compound [Na+].[Na+].[O-]C([O-])=O CDBYLPFSWZWCQE-UHFFFAOYSA-L 0.000 claims description 4
- PMZURENOXWZQFD-UHFFFAOYSA-L Sodium Sulfate Chemical compound [Na+].[Na+].[O-]S([O-])(=O)=O PMZURENOXWZQFD-UHFFFAOYSA-L 0.000 claims description 4
- UIIMBOGNXHQVGW-UHFFFAOYSA-M Sodium bicarbonate Chemical compound [Na+].OC([O-])=O UIIMBOGNXHQVGW-UHFFFAOYSA-M 0.000 claims description 4
- 230000036571 hydration Effects 0.000 claims description 4
- 238000006703 hydration reaction Methods 0.000 claims description 4
- 238000002156 mixing Methods 0.000 claims description 4
- HBBGRARXTFLTSG-UHFFFAOYSA-N Lithium ion Chemical compound [Li+] HBBGRARXTFLTSG-UHFFFAOYSA-N 0.000 claims description 3
- 238000001354 calcination Methods 0.000 claims description 3
- 229910001416 lithium ion Inorganic materials 0.000 claims description 3
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 3
- 229910021446 cobalt carbonate Inorganic materials 0.000 claims description 2
- KTVIXTQDYHMGHF-UHFFFAOYSA-L cobalt(2+) sulfate Chemical compound [Co+2].[O-]S([O-])(=O)=O KTVIXTQDYHMGHF-UHFFFAOYSA-L 0.000 claims description 2
- ZOTKGJBKKKVBJZ-UHFFFAOYSA-L cobalt(2+);carbonate Chemical compound [Co+2].[O-]C([O-])=O ZOTKGJBKKKVBJZ-UHFFFAOYSA-L 0.000 claims description 2
- 239000007788 liquid Substances 0.000 claims description 2
- 239000007773 negative electrode material Substances 0.000 claims description 2
- 229910000008 nickel(II) carbonate Inorganic materials 0.000 claims description 2
- ZULUUIKRFGGGTL-UHFFFAOYSA-L nickel(ii) carbonate Chemical compound [Ni+2].[O-]C([O-])=O ZULUUIKRFGGGTL-UHFFFAOYSA-L 0.000 claims description 2
- 229910000030 sodium bicarbonate Inorganic materials 0.000 claims description 2
- 235000017557 sodium bicarbonate Nutrition 0.000 claims description 2
- 229910000029 sodium carbonate Inorganic materials 0.000 claims description 2
- 235000017550 sodium carbonate Nutrition 0.000 claims description 2
- 229910052938 sodium sulfate Inorganic materials 0.000 claims description 2
- 235000011152 sodium sulphate Nutrition 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
- 239000003990 capacitor Substances 0.000 abstract description 20
- 239000007772 electrode material Substances 0.000 abstract description 10
- 230000005611 electricity Effects 0.000 abstract description 3
- 239000007783 nanoporous material Substances 0.000 abstract 3
- 239000000463 material Substances 0.000 description 19
- 239000000243 solution Substances 0.000 description 12
- 238000012360 testing method Methods 0.000 description 11
- 229910052799 carbon Inorganic materials 0.000 description 8
- 238000000227 grinding Methods 0.000 description 8
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 description 7
- 238000002484 cyclic voltammetry Methods 0.000 description 7
- 239000004744 fabric Substances 0.000 description 7
- 238000004519 manufacturing process Methods 0.000 description 7
- 229910005949 NiCo2O4 Inorganic materials 0.000 description 6
- 238000002604 ultrasonography Methods 0.000 description 6
- 238000006243 chemical reaction Methods 0.000 description 5
- UBEWDCMIDFGDOO-UHFFFAOYSA-N cobalt(II,III) oxide Inorganic materials [O-2].[O-2].[O-2].[O-2].[Co+2].[Co+3].[Co+3] UBEWDCMIDFGDOO-UHFFFAOYSA-N 0.000 description 5
- OQUOOEBLAKQCOP-UHFFFAOYSA-N nitric acid;hexahydrate Chemical compound O.O.O.O.O.O.O[N+]([O-])=O OQUOOEBLAKQCOP-UHFFFAOYSA-N 0.000 description 5
- 239000007787 solid Substances 0.000 description 5
- 238000004146 energy storage Methods 0.000 description 4
- 239000011521 glass Substances 0.000 description 4
- 239000003292 glue Substances 0.000 description 4
- 239000000843 powder Substances 0.000 description 4
- 238000011160 research Methods 0.000 description 4
- 238000007664 blowing Methods 0.000 description 3
- 238000001035 drying Methods 0.000 description 3
- 238000005485 electric heating Methods 0.000 description 3
- 238000002474 experimental method Methods 0.000 description 3
- 238000012545 processing Methods 0.000 description 3
- 238000006479 redox reaction Methods 0.000 description 3
- 238000004506 ultrasonic cleaning Methods 0.000 description 3
- RYGMFSIKBFXOCR-UHFFFAOYSA-N Copper Chemical compound [Cu] RYGMFSIKBFXOCR-UHFFFAOYSA-N 0.000 description 2
- 229910003266 NiCo Inorganic materials 0.000 description 2
- 238000013019 agitation Methods 0.000 description 2
- 239000012752 auxiliary agent Substances 0.000 description 2
- 238000004140 cleaning Methods 0.000 description 2
- 239000011889 copper foil Substances 0.000 description 2
- 238000007599 discharging Methods 0.000 description 2
- 238000009826 distribution Methods 0.000 description 2
- 230000000694 effects Effects 0.000 description 2
- 238000001027 hydrothermal synthesis Methods 0.000 description 2
- 150000002500 ions Chemical class 0.000 description 2
- 238000003756 stirring Methods 0.000 description 2
- 238000010408 sweeping Methods 0.000 description 2
- 230000032258 transport Effects 0.000 description 2
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 description 1
- WHXSMMKQMYFTQS-UHFFFAOYSA-N Lithium Chemical compound [Li] WHXSMMKQMYFTQS-UHFFFAOYSA-N 0.000 description 1
- 239000011149 active material Substances 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 239000010406 cathode material Substances 0.000 description 1
- 239000003795 chemical substances by application Substances 0.000 description 1
- 229910000428 cobalt oxide Inorganic materials 0.000 description 1
- 238000004891 communication Methods 0.000 description 1
- 239000013078 crystal Substances 0.000 description 1
- 125000004122 cyclic group Chemical group 0.000 description 1
- 238000000840 electrochemical analysis Methods 0.000 description 1
- 230000005518 electrochemistry Effects 0.000 description 1
- 230000007613 environmental effect Effects 0.000 description 1
- 239000012535 impurity Substances 0.000 description 1
- 238000011835 investigation Methods 0.000 description 1
- 229910052744 lithium Inorganic materials 0.000 description 1
- LGQLOGILCSXPEA-UHFFFAOYSA-L nickel sulfate Chemical compound [Ni+2].[O-]S([O-])(=O)=O LGQLOGILCSXPEA-UHFFFAOYSA-L 0.000 description 1
- GNRSAWUEBMWBQH-UHFFFAOYSA-N nickel(II) oxide Inorganic materials [Ni]=O GNRSAWUEBMWBQH-UHFFFAOYSA-N 0.000 description 1
- 229910000363 nickel(II) sulfate Inorganic materials 0.000 description 1
- 230000003647 oxidation Effects 0.000 description 1
- 238000007254 oxidation reaction Methods 0.000 description 1
- 238000003825 pressing Methods 0.000 description 1
- 239000002994 raw material Substances 0.000 description 1
- 230000002441 reversible effect Effects 0.000 description 1
- 239000011029 spinel Substances 0.000 description 1
- 230000006641 stabilisation Effects 0.000 description 1
- 238000011105 stabilization Methods 0.000 description 1
- 238000003860 storage Methods 0.000 description 1
- 231100000331 toxic Toxicity 0.000 description 1
- 230000002588 toxic effect Effects 0.000 description 1
- 229910052723 transition metal Inorganic materials 0.000 description 1
- 229910000314 transition metal oxide Inorganic materials 0.000 description 1
- 150000003624 transition metals Chemical class 0.000 description 1
Classifications
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B82—NANOTECHNOLOGY
- B82Y—SPECIFIC USES OR APPLICATIONS OF NANOSTRUCTURES; MEASUREMENT OR ANALYSIS OF NANOSTRUCTURES; MANUFACTURE OR TREATMENT OF NANOSTRUCTURES
- B82Y30/00—Nanotechnology for materials or surface science, e.g. nanocomposites
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B82—NANOTECHNOLOGY
- B82Y—SPECIFIC USES OR APPLICATIONS OF NANOSTRUCTURES; MEASUREMENT OR ANALYSIS OF NANOSTRUCTURES; MANUFACTURE OR TREATMENT OF NANOSTRUCTURES
- B82Y40/00—Manufacture or treatment of nanostructures
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01G—COMPOUNDS CONTAINING METALS NOT COVERED BY SUBCLASSES C01D OR C01F
- C01G53/00—Compounds of nickel
-
- 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
- H01G11/46—Metal oxides
-
- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01M—PROCESSES OR MEANS, e.g. BATTERIES, FOR THE DIRECT CONVERSION OF CHEMICAL ENERGY INTO ELECTRICAL ENERGY
- H01M10/00—Secondary cells; Manufacture thereof
- H01M10/05—Accumulators with non-aqueous electrolyte
- H01M10/052—Li-accumulators
- H01M10/0525—Rocking-chair batteries, i.e. batteries with lithium insertion or intercalation in both electrodes; Lithium-ion batteries
-
- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01M—PROCESSES OR MEANS, e.g. BATTERIES, FOR THE DIRECT CONVERSION OF CHEMICAL ENERGY INTO ELECTRICAL ENERGY
- H01M4/00—Electrodes
- H01M4/02—Electrodes composed of, or comprising, active material
- H01M4/36—Selection of substances as active materials, active masses, active liquids
- H01M4/48—Selection of substances as active materials, active masses, active liquids of inorganic oxides or hydroxides
- H01M4/52—Selection of substances as active materials, active masses, active liquids of inorganic oxides or hydroxides of nickel, cobalt or iron
- H01M4/525—Selection of substances as active materials, active masses, active liquids of inorganic oxides or hydroxides of nickel, cobalt or iron of mixed oxides or hydroxides containing iron, cobalt or nickel for inserting or intercalating light metals, e.g. LiNiO2, LiCoO2 or LiCoOxFy
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2004/00—Particle morphology
- C01P2004/01—Particle morphology depicted by an image
- C01P2004/03—Particle morphology depicted by an image obtained by SEM
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2004/00—Particle morphology
- C01P2004/60—Particles characterised by their size
- C01P2004/64—Nanometer sized, i.e. from 1-100 nanometer
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2006/00—Physical properties of inorganic compounds
- C01P2006/40—Electric properties
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- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
- Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
- Y02E—REDUCTION OF GREENHOUSE GAS [GHG] EMISSIONS, RELATED TO ENERGY GENERATION, TRANSMISSION OR DISTRIBUTION
- Y02E60/00—Enabling technologies; Technologies with a potential or indirect contribution to GHG emissions mitigation
- Y02E60/10—Energy storage using batteries
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- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
- Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
- Y02E—REDUCTION OF GREENHOUSE GAS [GHG] EMISSIONS, RELATED TO ENERGY GENERATION, TRANSMISSION OR DISTRIBUTION
- Y02E60/00—Enabling technologies; Technologies with a potential or indirect contribution to GHG emissions mitigation
- Y02E60/13—Energy storage using capacitors
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- Manufacturing & Machinery (AREA)
- General Chemical & Material Sciences (AREA)
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- Electric Double-Layer Capacitors Or The Like (AREA)
Abstract
The present invention relates to a kind of preparation methods of high-performance cobalt acid nickel nano-porous materials, belong to electrode material and electrochemical field, to prepare the electrode material of supercapacitor.The present invention provides a kind of preparation method of cobalt acid nickel nano-porous materials, the preparation method comprises the following steps: the compound containing cobalt ions, the compound containing nickel ion, the compound containing sodium ion are added in organic solvent, precipitating reagent is added, obtains mixed solution；Obtained mixed solution is ultrasonically treated, is then heated；Mixed solution after heating is cooling, it is then roasted, generates uniform cobalt acid nickel nano-porous materials, effectively increase the reserve of electricity of supercapacitor as the electrode material of super capacitor.
Description
Technical field
The invention belongs to electrode materials and electrochemical field, are related to a kind of cathode material of lithium ion battery, specifically one
The preparation method and application of kind cobalt acid nickel porous material.
Background technique
China develops super capacitor since the last century 80's, and is included in national brainstorm subject.Super electricity
Holding not only has the advantages that power density is big and that energy density is high is two big, also have charging rate fastly, have extended cycle life, electrode material
Material enriches and the advantages such as environmental protection.Supercapacitor as a kind of novel energy-storing element, supercapacitor means of transport (especially
There are also special means of transports for electronic or hybrid vehicle), electric power, computer, communication, military affairs etc. have surprising production
Product value and huge market potential.Although world forefront has not been reached yet in current China super capacitor level of industry, super
The research in grade capacitor field has reached world lead level.The core element of supercapacitor is electrode, and electrode material is to determine to surpass
The key factor of grade capacitor performance, therefore the super capacitance electrode material for having chemical property high is researched and developed, become in research
Most popular project.
Theoretically, Co3O4Possess highest specific capacitance in transition metal oxide, is the pole for preparing super capacitor electrode
Good material, and preparation method and uncomplicated, but Co price for other transition metal it is more expensive but also
It is toxic.Therefore, by cobalt/cobalt oxide investigation of materials, developing and Co3O4Structure is similar, function difference less and cost more
Just become a research direction for cheap and environmentally friendly material.NiCo2O4It is a kind of AB of Spinel2O4Type combined oxidation
Object, nickel ion occupy octahedral site, and cobalt ions had not only occupied octahedral site but also occupied tetrahedral site, in its physical structure
On, NiCo2O4Material and Co3O4It is quite similar, NiCo2O4Inherently there is Ni2+And Ni3+、Co2+And Co3+Two pairs of redox couples
Ion, so compared to NiO and Co3O4, NiCo2O4Itself has preferable electric conductivity.In addition to this, NiCo2O4The electricity of material
Chemical property is compared with Co3O4More have excellent, production cost is low, and raw material is sufficient.Therefore, research prepares high performance cobalt acid nickel material tool
There is important meaning.
Summary of the invention
For above-mentioned technical problem in the prior art, the present invention provides a kind of preparation of high-performance cobalt acid nickel porous material
Method, to improve the electrode performance of lithium battery.
The present invention provides a kind of preparation method of cobalt acid nickel porous material, including following steps:
Compound containing cobalt ions, the compound containing nickel ion, the compound containing sodium ion are added organic molten
In agent, precipitating reagent is added, obtains mixed solution；
Obtained mixed solution is ultrasonically treated, is then heated；
Mixed solution after heating is cooling, it is then roasted, obtains cobalt acid nickel porous material.
Preferably, the compound containing cobalt ions is one or more of cobalt nitrate, cobalt carbonate and cobaltous sulfate；Contain nickel
The compound of ion is one or more of nickel nitrate, nickelous carbonate and nickel sulfate；Compound containing sodium ion be sodium nitrate,
One or more of sodium carbonate, sodium bicarbonate and sodium sulphate.
It is highly preferred that cobalt nitrate is cabaltous nitrate hexahydrate；Nickel nitrate is Nickelous nitrate hexahydrate.
Preferably, organic solvent is polyethylene glycol；Precipitating reagent is urea.
It is highly preferred that polyethylene glycol is polyethylene glycol 400.
Preferably, polyethylene glycol 400, cabaltous nitrate hexahydrate, Nickelous nitrate hexahydrate, sodium nitrate, urea quality proportioning be
(300-500): (40-60): (20-40): 1:(100-200).It is highly preferred that polyethylene glycol 400, cabaltous nitrate hexahydrate, six water
Close nickel nitrate, sodium nitrate, urea quality proportioning be (400-500): (50-60): (25-35): 1:(100-150).
Preferably, obtained mixed solution is ultrasonically treated, ultrasonic time is 20-120 minutes.It is highly preferred that super
The sound time is 30-90 minutes.
Preferably, the mixed solution after ultrasound is heated, heating temperature is 80-100 DEG C, and heating time is that 1-4 is small
When.It is highly preferred that heating temperature is 90-100 DEG C, heating time is 2-3 hours.
Preferably, it will be roasted after the mixed solution cooling after heating, maturing temperature is 300-600 DEG C, calcining time
It is 4-8 hours.It is highly preferred that heating rate is 2-3 DEG C per minute.
Specifically, the preparation method of cobalt acid nickel porous material, using hydro-thermal method, comprising the following steps:
Measure 30-50mL polyethylene glycol 400 in beaker, weigh 4-6g cabaltous nitrate hexahydrate, 2-4g Nickelous nitrate hexahydrate,
Beaker is added in 0.08-0.1g sodium nitrate, and being slowly stirred is scattered in it in polyethylene glycol, then weighs 10-20g urea and is added and burns
Cup；
Acquired solution is carried out ultrasound 20-120 minutes, acquired solution is then heated to 80-100 DEG C, in constant temperature
Lower stirring 1-4 hours；
After reaction, solution taking-up is cooled to room temperature, under conditions of contacting with air, is heated to 300-600 DEG C,
Heating rate is 2-3 DEG C per minute, is roasted 4-8 hours；
Black solid is obtained to its cooling, grinding obtains cobalt acid nickel porous material.
More specifically, the preparation method of cobalt acid nickel porous material, using hydro-thermal method, comprising the following steps:
40-50mL polyethylene glycol 400 is measured in beaker, weighs 5-6g cabaltous nitrate hexahydrate, 2.5-3.5g six is hydrated nitre
Beaker is added in sour nickel, 0.08-0.1g sodium nitrate, and being slowly stirred is scattered in it in polyethylene glycol, then weighs 10-15g urea
Beaker is added；
Acquired solution is carried out ultrasound 30-90 minutes, acquired solution is then heated to 90-100 DEG C, under constant temperature conditions
Stirring 2-3 hours；
After reaction, solution taking-up is cooled to room temperature, under conditions of contacting with air, is heated to 400 DEG C, heating
Rate is 2-3 DEG C per minute, is roasted 6 hours；
Black solid is obtained to its cooling, grinding obtains cobalt acid nickel porous material.
The present invention also provides the application of prepared cobalt acid nickel porous material, the cobalt acid nickel using the method for the present invention preparation is suitble to
The negative electrode material for serving as lithium ion battery, super capacitor effectively improves the performances such as the storage of super capacitor.
Gained cobalt acid nickel porous material of the invention, studies its structure using scanning electron microscope (SEM), and
Test can be carried out to its electrochemistry.The results show that the invention has the following beneficial effects:
(1) preparation method obtains production die and can achieve ten rans through the invention, illustrates preparation of the present invention
Nanometre grade cobalt acid nickel material can be prepared in method, and the material prepared is highly uniform.During the experiment, we
Using urea as precipitating reagent, addition sodium nitrate is auxiliary agent, increases cobalt acid nickel product specific surface area, is come from sem test photo
It sees, material is that point is crystalline, and rough surface increases the specific surface area of material by many.Super capacitance electrode material possesses
Redox reaction can preferably occur for the advantages of large specific surface area, so that super capacitor provides higher energy storage.
(2) the super capacitor device of the cobalt acid nickel material production obtained using preparation method of the present invention has certain energy storage
With stable and quick charging/discharging function, specific capacitance nearly 30F/g.
Detailed description of the invention
Attached drawing is used to provide further understanding of the present invention, and constitutes part of specification, with reality of the invention
It applies example to be used to explain the present invention together, not be construed as limiting the invention.
Fig. 1 is the sem test photo according to the cobalt acid nickel porous material of the preparation of embodiment 2 under 10000 times.
Fig. 2 is the sem test photo according to the cobalt acid nickel porous material of the preparation of embodiment 3 under 10000 times.
Fig. 3 is the cyclic voltammetry curve of the super capacitor device of the cobalt acid nickel porous material production obtained using embodiment 2
Figure.
Specific embodiment
Now in conjunction with specific embodiment, the invention will be further described, following embodiment be intended to illustrate invention rather than it is right
Of the invention further limits.
Embodiment 1
A kind of preparation method of cobalt acid nickel porous material measures 50mL polyethylene glycol 400 in beaker, weighs six hydration nitre
Beaker is added in sour cobalt 5.8g, Nickelous nitrate hexahydrate 2.9g, sodium nitrate 0.09g, and being slowly stirred makes it be scattered in polyethylene glycol 400
In, it then weighs 10g urea and beaker is added, carry out ultrasound 1 hour using ultrasonic cleaning instrument, acquired solution is then put into oil bath
Pot, is heated to 100 DEG C, constant temperature is stirred to react 2 hours, mixing speed 300r/min；After reaction, solution is taken out and is cooled down
It to room temperature, is transferred in rectangular crucible, is placed in Muffle furnace under conditions of being contacted with air, it is permanent to be first heated to 300 DEG C of holdings
Temperature processing 2 hours is heated to 400 DEG C of constant temperature and handles 6 hours, and heating rate is 2-3 DEG C per minute, cooling that black is solid to its
Body finally obtains cobalt acid nickel porous material with grinding alms bowl grinding.
Embodiment 2
A kind of preparation method of cobalt acid nickel porous material measures 45mL polyethylene glycol 400 in beaker, weighs six hydration nitre
Beaker is added in sour cobalt 5.8g, Nickelous nitrate hexahydrate 2.9g, sodium nitrate 0.1g, and being slowly stirred is scattered in it in polyethylene glycol 400,
Then it weighs 15g urea and beaker is added, carry out ultrasound 1 hour using ultrasonic cleaning instrument, acquired solution is then put into oil bath pan
100 DEG C are heated to, magnetic agitation is reacted 2 hours, mixing speed 300r/min: after reaction, solution taking-up being cooled to
Room temperature is transferred in rectangular crucible, is placed in Muffle furnace under conditions of contacting with air, and 300 DEG C of holding constant temperature are first heated to
Processing 2 hours is heated to 400 DEG C of constant temperature and handles 6 hours, and heating rate is 2-3 DEG C per minute, cooling that black is solid to its
Body finally obtains cobalt acid nickel porous material with grinding alms bowl grinding.
Embodiment 3
A kind of preparation method of cobalt acid nickel porous material measures 40mL polyethylene glycol 400 in beaker, weighs six hydration nitre
Beaker is added in sour cobalt 5.8g, Nickelous nitrate hexahydrate 2.9g, sodium nitrate 0.1g, and being slowly stirred is scattered in it in polyethylene glycol 400,
Then it weighs 15g urea and beaker is added, carry out ultrasound 1 hour using ultrasonic cleaning instrument, acquired solution is then put into oil bath pan
100 DEG C are heated to, magnetic agitation is reacted 2 hours, mixing speed 330r/min: after reaction, solution taking-up being cooled to
Room temperature is transferred in rectangular crucible, is placed in Muffle furnace under conditions of contacting with air, is directly heated at 400 DEG C of constant temperature
Reason 6 hours, heating rate be 2-3 DEG C per minute, to its cooling black solid, it is more to finally obtain cobalt acid nickel with grinding alms bowl grinding
Porous materials.
Referring to Fig. 1 and Fig. 2, by scanning electron microscope it can be seen that the cobalt acid nickel material crystal grain thus made can achieve
Ten rans illustrate that the preparation method of experiment is available nanometre grade cobalt acid nickel material, and the material prepared
Expect highly uniform.During the experiment, for the present invention using urea as precipitating reagent, being added to sodium nitrate is auxiliary agent, makes its specific surface area
Increase, from the point of view of sem test photo, material is that point is crystalline, and rough surface increases the specific surface area of material
Many.In addition, can be seen that from the comparison of Fig. 1 and Fig. 2, the temperature of calcining is to have centainly for the partial size and surface area of material
It influences.Test also demonstrates NiCo2O4It the advantages of possessing large specific surface area as super capacitance electrode material, can be more preferable
Generation redox reaction, so that the super capacitor for preparing it is capable of providing higher energy storage.
Embodiment 4
The NiCo that this example prepares embodiment 22O4Powder carries out electro-chemical test
The preparation of super capacitor test device
Then the carbon cloth of clip 1cm × 2cm is placed on beaker soaked in absolute ethyl alcohol, beaker is placed in supersonic cleaning machine
It carries out being cleaned by ultrasonic 1h using water level appropriate, removes the impurity being attached on carbon cloth.After cleaning into carbon cloth is put to dry glass
Glass culture dish is put into electric heating constant-temperature blowing drying box with taking out after 80 DEG C of dry 30min, is cooled to room temperature to it, uses liquid glue
One layer is painted in the one side of carbon cloth, the clip oiliness paper more slightly larger than carbon cloth is attached on glue, and surrounding is cut.With another
A glass culture dish is pressing against the carbon cloth close to oiliness paper and is being put into electric heating constant-temperature blowing drying box with taking out after 80 DEG C of dry 30min,
One layer of thin glue is painted on oiliness paper later, the 0.02g NiCo that will be prepared2O4Powder is uniformly dispersed on glue, and uses glass
Stick is flat-pushing to keep powder distribution uniform, places into electric heating constant-temperature blowing drying box with taking out after 80 DEG C of dry 1h, is cooled to room temperature, cuts
The copper foil of two pieces of 1cm × 1cm is taken, distribution is attached on carbon cloth and powder bed, then burn-ons conducting wire on copper foil to test.
Cyclic voltammetry
Cyclic voltammetry method is the onset potential by control load on the working electrode (s, and with certain scanning speed
Rate carries out, and one cycle is formed by just sweeping with anti-two parts of sweeping, and completes a charge and discharge process.Different potentials be electrolysed
Material in matter on working electrode can generate different degrees of redox reaction, and be recorded with electric current-potential curve,
That is cyclic voltammetry curve.Curve can reflect the chemical properties such as redox reversible and the capacitance of electrode material.It follows
The scanning speed of ring volt-ampere test is surveyed the C-V curve changing rule under different scanning rates, is filled between 10-100mV/s
The voltage window of discharge test is in -0.6-0.4V.
If sweep speed is k, then it is respectively discharge curve and charging curve in horizontal axis that discharge scanning speed, which is-k, S1 and S2,
On projected area, it is assumed that charging capacitor and discharge capacity are equal.
For discharge curve
- mkC=I (U)
(U2-U1) mkC=S1
Similarly charging curve
(U2-U1) mkC=S2
Two formulas are subtracted each other
S is the figure that cyclic voltammetry curve surrounds
One complete CV curve is equivalent to a charge and discharge process, therefore cyclic integral area should be only electric discharge divided by 2
Part, if active material quality be two electrodes on gross mass, capacitor capacitance=integral area/(2 × scanning speed ×
Potential difference × gross activity substance), substance single electrode is 4 times of capacitor, i.e. single electrode capacitor=2 × integral area/(scanning speed
Degree × potential difference × gross activity substance).
It is the circulation volt of the super capacitor device of the cobalt acid nickel porous material production obtained using embodiment 2 referring to Fig. 3
Pacify curve graph.As can be seen from the figure cyclic voltammetry curve has a pair of obvious redox peaks, and the shape of curve shows that this is tested
The capacitance characteristic of device is clearly distinguishable from electric double layer capacitance, the shape of the cyclic voltammetry curve of electric double layer capacitance generally all close to
Ideal rectangle.It is 69.2240 by the area integral that Origin software data processing obtains the curve, the tester is calculated
The capacitor of part is 0.5769F, specific capacitance 28.84F/g.By electrochemical property test, demonstrates and obtained using the present invention
The super capacitor device of cobalt acid nickel porous material production has certain energy storage and stabilization and quick charging/discharging function.
Claims (8)
1. a kind of preparation method of cobalt acid nickel porous material, which comprises the following steps:
Compound containing cobalt ions, the compound containing nickel ion, the compound containing sodium ion are added in organic solvent,
Precipitating reagent is added, obtains mixed solution；
Obtained mixed solution is ultrasonically treated, is then heated；
Mixed solution after heating is cooling, it is then roasted, obtains cobalt acid nickel porous material.
2. the preparation method of cobalt acid nickel porous material according to claim 1, which is characterized in that the chemical combination containing cobalt ions
Object is one or more of cobalt nitrate, cobalt carbonate and cobaltous sulfate；Compound containing nickel ion is nickel nitrate, nickelous carbonate and sulphur
One or more of sour nickel；Compound containing sodium ion is one of sodium nitrate, sodium carbonate, sodium bicarbonate and sodium sulphate
Or it is several；Organic solvent is polyethylene glycol；Precipitating reagent is urea.
3. the preparation method of cobalt acid nickel porous material according to claim 2, which is characterized in that cobalt nitrate is six hydration nitre
Sour cobalt；Nickel nitrate is Nickelous nitrate hexahydrate；Polyethylene glycol is polyethylene glycol 400.
4. the preparation method of cobalt acid nickel porous material according to claim 3, which is characterized in that polyethylene glycol 400, six water
Close cobalt nitrate, Nickelous nitrate hexahydrate, sodium nitrate, urea quality proportioning be (300-500): (40-60): (20-40): 1:
(100-200)。
5. the preparation method of cobalt acid nickel porous material according to claim 1, which is characterized in that the mixed solution that will be obtained
It is ultrasonically treated, ultrasonic time is 20-120 minutes；Then heated at constant temperature is carried out, heating temperature is 80-100 DEG C, when heating
Between be 1-4 hours.
6. the preparation method of cobalt acid nickel porous material according to claim 1, which is characterized in that the mixing after heating is molten
Liquid cooling is but roasted afterwards, and maturing temperature is 300-600 DEG C, and calcining time is 4-8 hours, and heating rate is 2-3 DEG C per minute.
7. the cobalt acid nickel porous material of any one of claim 1-6 the method preparation.
8. application of the cobalt acid nickel porous material as claimed in claim 7 in the negative electrode material of rechargeable lithium ion batteries.
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