CN106006763A - Method for preparing nickel cobaltate nanocrystalline assembly - Google Patents
Method for preparing nickel cobaltate nanocrystalline assembly Download PDFInfo
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- CN106006763A CN106006763A CN201610335153.0A CN201610335153A CN106006763A CN 106006763 A CN106006763 A CN 106006763A CN 201610335153 A CN201610335153 A CN 201610335153A CN 106006763 A CN106006763 A CN 106006763A
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01G—COMPOUNDS CONTAINING METALS NOT COVERED BY SUBCLASSES C01D OR C01F
- C01G53/00—Compounds of nickel
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- 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
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- 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
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- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01G—CAPACITORS; CAPACITORS, RECTIFIERS, DETECTORS, SWITCHING DEVICES OR LIGHT-SENSITIVE DEVICES, OF THE ELECTROLYTIC TYPE
- H01G11/00—Hybrid capacitors, i.e. capacitors having different positive and negative electrodes; Electric double-layer [EDL] capacitors; Processes for the manufacture thereof or of parts thereof
- H01G11/22—Electrodes
- H01G11/30—Electrodes characterised by their material
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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
- C01P2004/01—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
- C01P2004/01—Particle morphology depicted by an image
- C01P2004/04—Particle morphology depicted by an image obtained by TEM, STEM, STM or AFM
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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
- C01P2004/30—Particle morphology extending in three dimensions
- C01P2004/32—Spheres
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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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- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
- Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
- Y02E—REDUCTION OF GREENHOUSE GAS [GHG] EMISSIONS, RELATED TO ENERGY GENERATION, TRANSMISSION OR DISTRIBUTION
- Y02E60/00—Enabling technologies; Technologies with a potential or indirect contribution to GHG emissions mitigation
- Y02E60/13—Energy storage using capacitors
Abstract
The invention belongs to the technical field of metal oxide preparation and relates to a method for preparing a nickel cobaltate nanocrystalline assembly. Nickel cobaltate nanocrystalline assemblies of different morphologies are synthesized by changing varieties of solvents in the solvothermal reaction process to be used for preparing an electrode material in the field of supercapacitors, and the problems that in the prior art, when a metal oxide serves as the electrode material, the manufacturing cost is too high and the environmental pollution is caused are solved. The concrete process is that nickel nitrate hexahydrate and cobalt nitrate hexahydrate serve as metal sources, ammonium acetate and urea serve as a pH modifier and a precipitator respectively, ethanol or isopropanol and water are mixed to serve as a solvent, a precursor of a nanocrystalline assembly is prepared through a solvothermal method, and then high temperature annealing is performed to obtain the nickel cobaltate nanocrystalline assembly. The method is simple in preparation process, reliable in principle, low in cost, good in electrochemical performance, wide in application and friendly in use environment and has good economic benefits and development and application prospects.
Description
Technical field:
The invention belongs to metal oxide materials preparing technical field, relate to the acid of a kind of cobalt utilizing solvent-thermal method to prepare different-shape
The method of nickel nanometer crystal assembly, obtained cobalt acid nickel nanometer crystal assembly has preferable electric conductivity, is applied to super capacitor
Device field, has good development prospect and using value.
Background technology:
Cobalt acid nickel is a kind of typical spinelle mixed valence composite oxide of metal, active height, the feature of good stability.
In its crystal structure, nickel ion occupies octahedral site, and cobalt ion had both occupied octahedral site, occupied again whole tetrahedrons
, there is Co in the structure in space2+/Co3+And Ni2+/Ni3+Oxidation-reduction pair, therefore, its electro-chemical activity is the most single
Nickel oxide and Cobalto-cobaltic oxide, cobalt acid nickel has preferable electric conductivity and low cost, environmentally friendly, ultracapacitor lead
Territory has good development prospect and using value.In the prior art, the primary synthetic methods of cobalt acid nickel has: high temperature solid-state method,
Mechanochemical synthesis, sol-gel process, liquid chemical precipitation method etc..Wherein high temperature solid-state chemical reaction method is cobalt acid nickel tradition
Synthetic method, although technique is simple, but response time length, energy consumption are high, product granularity is big；Introduce during Mechano-chemical Synthesizing
A large amount of strains and defect, products therefrom bad dispersibility；Sol-gal process is by adding the product grain particle diameter that surfactant obtains
Less and be evenly distributed, but it is easily introduced impurity；And the product structure of liquid chemical precipitation method synthesis is imperfect, can generating portion Asia
Steady phase.Chinese patent (CN10033497.3,2011) utilizes sol-gal process to synthesize, and pattern is uniform, specific surface area big, knot
Crystalline substance degree is high, the porous cobalt acid nickel material of even aperture distribution.Chinese patent (CN10195864.X, 2011) provides a kind of cobalt acid
The coprecipitation method of nano nickel particles, obtained cobalt acid nickel nanometer crystal assembly is spinel structure, and particle size is 10
Ran, and it is applied to electrode material for super capacitor.Chinese patent (CN201210222916.2,2012) provides
A kind of method of water heat transfer mesoporous nickel cobalt nano wire and application thereof, gained cobalt acid nickel nano wire be spinel-type Emission in Cubic,
Purity height, porous, there is higher specific surface area, can be used as electrode material for super capacitor.
Summary of the invention:
It is an object of the invention to the shortcoming overcoming prior art to exist, it is nanocrystalline that proposition one utilizes solvent-thermal method to prepare cobalt acid nickel
The method of assembly, by the cobalt acid nickel nanometer crystal assembly of the kind synthesis different-shape of solvent during change solvent thermal reaction,
For preparing the electrode material of ultracapacitor, it is possible to overcome in prior art metal-oxide as manufacturing cost during electrode material
Problem that is too high and that cause environmental pollution.
To achieve these goals, the present invention is by Nickelous nitrate hexahydrate (Ni (NO3)2·6H2And cabaltous nitrate hexahydrate O)
(Co(NO3)2·6H2O) as source metal, ammonium acetate (CH3COO (NH4)2) and carbamide (CO (NH2)2) it is respectively pH adjusting agent
And precipitant, with ethanol or isopropanol and water mixed liquid as solvent, prepared the precursor of nanometer crystal assembly by solvent-thermal method,
Obtaining cobalt acid nickel nanometer crystal assembly through high annealing again, its specific embodiment comprises the following steps:
First by the Co (NO of 2mmol3)2·6H2Ni (the NO of O and 1mmol3)2·6H2O is dissolved in ethanol or the isopropyl of 30mL
Alcohol, with the mixed solvent of water, after magnetic agitation is uniform mixed liquor, adds the CH3COO (NH of 9mmol4)2With 15mmol's
CO(NH2)2Continuing to be stirred until homogeneous, in the Teflon inner bag of the pyroreaction still that then mixed liquor moves into 40mL, good seal is anti-
Answering still, put in baking oven, arranging heating-up temperature is 120 DEG C, and the response time is 10 hours, has reacted and after natural cooling
Collect solid product centrifugation, then with after deionized water and washing with alcohol 3-10 time, under the conditions of 60 DEG C dry 12 hours
After, obtain the presoma of the cobalt acid nickel nanometer crystal assembly of lilac, more above-mentioned presoma is placed in Muffle furnace, in air atmosphere
Arranging temperature in enclosing is 350 DEG C, and annealing time is 2 hours, and thermograde is 2min DEG C-1Anneal.Wherein, arrange mixed
When in bonding solvent, the volume ratio of ethanol and water is 1:1, the cobalt acid named CNA1 of nickel nanometer crystal assembly prepared；Arrange mixed
When in bonding solvent, the volume ratio of isopropanol and water is 1:1, the cobalt acid named CNA2 of nickel nanometer crystal assembly prepared, it is achieved
The preparation of cobalt acid nickel nanometer crystal assembly.
Cobalt acid nickel nanometer crystal assembly prepared by the present invention as the packaging technology of the ultracapacitor of electrode material is: first by 4.25
Cobalt acid nickel nanometer crystal assembly, 0.5mg acetylene black and 0.25mg politef prepared by mg is according to the mass ratio of 17:2:1
After mixing, it is dissolved in the isopropanol of 3mL, is stirred until homogeneous under ultrasound condition, when mixture is become sticky shape from solution,
By its flakiness, pressure is taped against on foamed nickel substrate, controls temperature under vacuum and is 110 DEG C and is dried 12 hours, is dried
After completing, thin slice is taken out, the pressure of tablet machine is set to 1.0 × 107Pa, flattens thin slice, then is cut into a diameter of 1cm
Circular electric pole piece, keep on each electrode slice for the active material of 5mg, the thickness of each electrode slice is 1mm, in room temperature
Under the conditions of with potassium hydroxide aqueous solution as electrolyte, make two electrode separation with perforated membrane, be assembled into symmetric form two electrode super electricity
Container.
Cobalt acid nickel nanometer crystal assembly prepared by the present invention has ferrimagnetism, has relatively in the application of bipolar electrode ultracapacitor
Good ultracapacitor performance, by ethanol with water with the mixed solution of volume 1:1 for solvent time, nanocrystalline group of the cobalt acid nickel of preparation
The ultracapacitor performance of dress body is more preferable.
Compared with prior art, its preparation technology is simple for the present invention, and principle is reliable, and low cost is widely used, and uses environment friend
Good, there is good economic benefit and development prospect.
Accompanying drawing illustrates:
Fig. 1 is the scanning electron microscope diagram of cobalt acid nickel nanometer crystal assembly prepared by the present invention, and wherein, (a) is CNA1's
Presoma, (b) is the presoma of CNA2, and (c) is CNA1, and (d) is CNA2.
Fig. 2 be the cobalt acid nickel nanometer crystal assembly prepared of the present invention ultrasonic after transmission electron microscope figure, wherein, (a) is
The presoma of CNA1, (b) is the presoma of CNA2, and (c) is CNA1, and (d) is CNA2.
Fig. 3 is that cobalt acid nickel nanometer crystal assembly CNA1 and CNA2 prepared by the present invention is water-soluble at the KOH that electrolyte is 2mol/L
The performance schematic diagram of ultracapacitor during liquid, wherein, (a) is cyclic voltammetry curve；B () is constant current charge-discharge curve；(c)
For the specific capacity under different electric current densities；D () is electric current density when being 1A/g, specific capacity is with the change curve of cycle-index.
Fig. 4 is the electrochemical impedance collection of illustrative plates of cobalt acid nickel nanometer crystal assembly CNA1 and CNA2 prepared by the present invention.
Fig. 5 is the property of the cobalt acid nickel nanometer crystal assembly CNA1 for preparing of present invention ultracapacitor under different electrolytes concentration
Energy schematic diagram, wherein, (a) is cyclic voltammetry curve；B () is constant current charge-discharge curve；C () is under different electric current density
Specific capacity；D () is electrochemical impedance collection of illustrative plates.
Detailed description of the invention:
Below by embodiment and combine accompanying drawing the present invention will be further described.
Embodiment 1:
The preparation technology of the cobalt acid nickel nanometer crystal assembly that the present embodiment relates to is: first by the Co (NO of 2mmol3)2·6H2O and 1
Ni (the NO of mmol3)2·6H2O is dissolved in the ethanol of 30mL or the mixed solvent of isopropanol and water, and magnetic agitation is uniform
After mixed liquor, add the CH3COO (NH of 9mmol4)2CO (NH with 15mmol2)2Continue to be stirred until homogeneous, then will be mixed
Close in the Teflon inner bag of the pyroreaction still that liquid moves into 40mL, good seal reactor, put in baking oven, heating-up temperature is set
Being 120 DEG C, the response time is 10 hours, reacted and natural cooling after collect solid product centrifugation, then spend from
After sub-water and washing with alcohol 3-10 time, after being dried 12 hours under the conditions of 60 DEG C, obtain nanocrystalline group of the cobalt acid nickel of lilac
The presoma of dress body, more above-mentioned presoma is placed in Muffle furnace, arranging temperature in air atmosphere is 350 DEG C, annealing time
Being 2 hours, thermograde is 2min DEG C-1Anneal.Wherein, arranging the volume ratio of ethanol and water in mixed solvent is 1:1
Time, the cobalt acid named CNA1 of nickel nanometer crystal assembly prepared；Arranging the volume ratio of isopropanol and water in mixed solvent is 1:1
Time, the cobalt acid named CNA2 of nickel nanometer crystal assembly prepared, it is achieved that the preparation of cobalt acid nickel nanometer crystal assembly.
The present embodiment is the scanning electron microscope diagram of the cobalt acid nickel nanometer crystal assembly of preparation, as it is shown in figure 1, wherein, (a)
For the presoma of CNA1, (b) is the presoma of CNA2, and (c) is CNA1, and (d) is CNA2；A () and (c) is in Hemicentrotus seu Strongylocentrotus
Shape spherical, surface is made up of threadiness, and (b) and (d) presents spherical, and surface is made up of squame；By (a) and (c)
Or (b) carries out contrast with (d) and understand, pattern does not the most change；As shown in Figure 1, sized by (c) and (d) is equal not
Deng micron ball, the crystallite dimension calculated is respectively 13.9nm and 14.4nm, show micron ball by nanocrystalline in order
Composition.
The present embodiment be preparation cobalt acid nickel nanometer crystal assembly ultrasonic after transmission electron microscope figure, as in figure 2 it is shown, its
In, (a) is the presoma of CNA1, and (b) is the presoma of CNA2, and (c) is CNA1, and (d) is CNA2, by (a) with
C () or (b) and (d) carry out contrast and understand, cobalt acid nickel nanometer crystal assembly is to be obtained after high annealing by presoma.
Embodiment 2:
The present embodiment relates to:
First by cobalt acid nickel nanometer crystal assembly, 0.5mg acetylene black and the 0.25mg politef prepared by 4.25mg according to 17:2:1
Mass ratio mixing after, be dissolved in the isopropanol of 3mL, under ultrasound condition, stirring is for homogeneous mixture, when mixture is by solution
When becoming sticky shape, by its flakiness, pressure is taped against on foamed nickel substrate, controls temperature under vacuum and is 110 DEG C and is dried
12 hours, after being dried, thin slice is taken out, the pressure of tablet machine is set to 1.0 × 107Pa, flattens thin slice, then cuts
Becoming the circular electric pole piece of a diameter of 1cm, keep the active material for 5mg on each electrode slice, the thickness of each electrode slice is
1mm, at ambient temperature with potassium hydroxide aqueous solution as electrolyte, makes two electrode separation with perforated membrane, is assembled into symmetric form
Two electrode super capacitors.
The present embodiment relates to prepared cobalt acid nickel nanometer crystal assembly CNA1 and CNA2 at the KOH aqueous solution of 2mol/L
Characterizing for ultracapacitor performance during electrolyte, its result is as it is shown on figure 3, (a) is for being 40mV/s at scanning speed
Under the conditions of cyclic voltammetry curve, curve, close to rectangle, shows that CNA1 and CNA2 is respectively provided with preferable capacitive property；(b) be
It is 0.1A g in electric current density-1Time constant current charge-discharge curve and be presented on the specific capacity under different electric current density；CNA1 in (c)
Present the specific capacity bigger relative to CNA2, reach 244.31F g-1；D () shows that in electric current density be 1A g-1Condition
Lower discharge and recharge 2000 times, CNA1 and CNA2 specific capacity is kept at 90.75% and 91.58%, and CNA1 has relative to CNA2
There is preferable cyclical stability.
The present embodiment relates to prepared cobalt acid nickel nanometer crystal assembly CNA1 and CNA2 at the KOH aqueous solution of 2mol/L
For the impedance of the ultracapacitor of assembling during electrolyte as shown in Figure 4, its test frequency range is 0.01Hz to 1,000,00Hz；
Wherein, bold portion is the impedance spectrogram simulating corresponding equivalent circuit according to Zview software, the initial data recorded and simulation
Data match；Spectrogram presents the semicircle of a high frequency region and the oblique line of low frequency range and slope is relatively big, illustrate that energy storage device is close
Preferably ultracapacitor, and the resistance value that CNA1 is relative to CNA2 is less, bent with cyclic voltammetry curve and constant current charge-discharge
The conclusion that line obtains is consistent；Impedance diagram shows, CNA1 has preferable super capacitor in the application of bipolar electrode ultracapacitor
Device behavior.
The present embodiment relates to prepared cobalt acid nickel nanometer crystal assembly CNA1 ultracapacitor under different electrolytes concentration
Performance test as it is shown in figure 5, wherein, (a) is the cyclic voltammetry curve that electrolyte measures, and (b) is that constant current charge-discharge is bent
Line, (c) is specific capacity and electric current density relation curve, and (d) is impedance spectrum；Fig. 3 and Fig. 5 carries out contrast understand, when
When the concentration of KOH aqueous solution is gradually increased, from 1mol L-1、2mol L-1To 6mol L-1Time, the specific capacity of ultracapacitor
First increases and then decreases；Showing the excessive concentration of electrolyte or the too low accumulation being all unfavorable for electric charge, the concentration of electrolyte is 2mol L-1
Time capacitor performance best.
Claims (2)
1. the preparation method of a cobalt acid nickel nanometer crystal assembly, it is characterised in that: by Nickelous nitrate hexahydrate and cabaltous nitrate hexahydrate
As source metal, with ammonium acetate and carbamide respectively as pH adjusting agent and precipitant, then make with ethanol or isopropanol and water mixed liquid
For solvent, prepared the precursor of nanometer crystal assembly by solvent-thermal method, then obtain the cobalt nanocrystalline assembling of acid nickel through high annealing
Body, its specific embodiment comprises the following steps:
First the cabaltous nitrate hexahydrate of 2mmol and the Nickelous nitrate hexahydrate of 1mmol are dissolved in the ethanol of 30mL or isopropanol with
In the mixed solvent of water, after magnetic agitation is uniform mixed liquor, the carbamide of the ammonium acetate and 15mmol that add 9mmol continues to stir
Mix to uniformly, in the Teflon inner bag of the pyroreaction still that then mixed liquor is moved into 40mL, good seal reactor, put into baking
In case, arranging heating-up temperature is 120 DEG C, and the response time is 10 hours, has reacted and has collected solid product after natural cooling
Centrifugation, then with after deionized water and washing with alcohol 3-10 time, after being dried 12 hours under the conditions of 60 DEG C, obtain grey violet
The presoma of the cobalt acid nickel nanometer crystal assembly of color, more above-mentioned presoma is placed in Muffle furnace, air atmosphere arranges temperature
Being 350 DEG C, annealing time is 2 hours, and thermograde is 2min DEG C-1Anneal, wherein, ethanol in mixed solvent is set
When being 1:1 with the volume ratio of water, the cobalt acid named CNA1 of nickel nanometer crystal assembly prepared；Isopropyl in mixed solvent is set
When the volume ratio of alcohol and water is 1:1, the cobalt acid named CNA2 of nickel nanometer crystal assembly prepared, it is achieved that cobalt acid nickel nanometer
The preparation of brilliant assembly.
2. according to the preparation method of the cobalt acid nickel nanometer crystal assembly described in claim 1, it is characterised in that: the cobalt acid nickel of preparation
Nanometer crystal assembly has ferrimagnetism, has ultracapacitor performance in the application of bipolar electrode ultracapacitor, by ethanol with
The ultracapacitor better performances of the cobalt acid nickel nanometer crystal assembly prepared when water is with the mixed solution of volume 1:1 for solvent.
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| CN108980622A (en) * | 2018-08-20 | 2018-12-11 | 中国石油大学(北京) | A kind of nano combined pour-point depressant and its preparation method and application |
| CN109243850A (en) * | 2018-11-05 | 2019-01-18 | 南京晓庄学院 | Ni-Co oxide nanocrystalline and its controllable synthesis method and application |
| CN110560679A (en) * | 2019-08-08 | 2019-12-13 | 安徽师范大学 | Ni-Co alloy material with three-dimensional polyhedral structure and preparation method and application thereof |
| CN114604906A (en) * | 2022-03-02 | 2022-06-10 | 常州大学 | Molybdenum-doped R-Mo-NiCo for sodium borohydride reduction constructed by double-defect process2O4And preparation method and application thereof |
| CN114853092A (en) * | 2022-03-30 | 2022-08-05 | 武汉工程大学 | Preparation method of nano-scale double transition metal oxide with large specific surface area |
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Cited By (8)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN108980622A (en) * | 2018-08-20 | 2018-12-11 | 中国石油大学(北京) | A kind of nano combined pour-point depressant and its preparation method and application |
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| CN109243850A (en) * | 2018-11-05 | 2019-01-18 | 南京晓庄学院 | Ni-Co oxide nanocrystalline and its controllable synthesis method and application |
| CN110560679A (en) * | 2019-08-08 | 2019-12-13 | 安徽师范大学 | Ni-Co alloy material with three-dimensional polyhedral structure and preparation method and application thereof |
| CN110560679B (en) * | 2019-08-08 | 2021-10-29 | 安徽师范大学 | Ni-Co alloy material with three-dimensional polyhedral structure and preparation method and application thereof |
| CN114604906A (en) * | 2022-03-02 | 2022-06-10 | 常州大学 | Molybdenum-doped R-Mo-NiCo for sodium borohydride reduction constructed by double-defect process2O4And preparation method and application thereof |
| CN114604906B (en) * | 2022-03-02 | 2024-03-22 | 常州大学 | Double-defect technology for constructing sodium borohydride reduced molybdenum doped R-Mo-NiCo 2 O 4 Preparation method and application |
| CN114853092A (en) * | 2022-03-30 | 2022-08-05 | 武汉工程大学 | Preparation method of nano-scale double transition metal oxide with large specific surface area |
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