CN106340403A - Preparation method and purpose of zinc cobaltate nano wire or nanometer band electrode material - Google Patents
Preparation method and purpose of zinc cobaltate nano wire or nanometer band electrode material Download PDFInfo
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- CN106340403A CN106340403A CN201610878534.3A CN201610878534A CN106340403A CN 106340403 A CN106340403 A CN 106340403A CN 201610878534 A CN201610878534 A CN 201610878534A CN 106340403 A CN106340403 A CN 106340403A
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- acid zinc
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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
- H01G11/84—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
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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
- H01G11/24—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 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
-
- 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 provides a preparation method and purpose of a zinc cobaltate nano wire or nanometer band electrode material. The method comprises the following steps: step 1, preparation of a zinc cobaltate precursor solution, i.e., adding powder of soluble cobalt salt, soluble zinc salt, hexamethylenetetramine and ammonium fluoride into distilled water, performing ultrasonic processing, performing uniform stirring by use of a magnetic stirrer, waiting for application; step 2, preparation of zinc cobaltate precursor powder, i.e., transferring the zinc cobaltate precursor solution in the first step to a reaction vessel of a polytetrafluoroethylene substrate, sealing, performing constant-temperature thermal reaction, after the reaction is completed, cooling to a room temperature, washing a solid product and performing vacuum drying so as to obtain the zinc cobaltate precursor powder; and step 3, preparation of a zinc cobaltate nano wire or nanometer band, i.e., putting the zinc cobaltate precursor powder obtained in the second step into a tubular furnace protected by inert gas for calcining so as to obtain the zinc cobaltate nano wire or nanometer band. The process is simple, the reappearance is good, the price is low, the requirement for environmental friendliness is met, and batch production is facilitated.
Description
Technical field
The invention belongs to nano composite material technical field is and in particular to a kind of cobalt acid zinc nano wire or nanometer band electrode material
The preparation method and its usage of material.
Background technology
Developing rapidly with economic society, environmental degradation that fossil energy is caused, lack of energy are subject to the height of various countries
Degree concern, and new energy storage equipment such as ultracapacitor (ecs) is high due to charge-discharge velocity, has extended cycle life, work
Temperature range width, the advantages of environmentally safe, is known as by scientist being the energy storage device of the most potential alleviating energy crisis.
Electrode material is the important component part of ultracapacitor, is the pass of impact ultracapacitor production cost and performance
Key factor.Electrode material for super capacitor mainly has material with carbon element, metal oxide materials and conducting polymer materials.Material with carbon element has
Have extended cycle life, low cost many advantages, such as, but it is more low than electric capacity and oxidation resistance is poor.Conductive polymer electrodes material
Material has good electric conductivity, but conductive polymer electrodes material stability is poor, and heat endurance is poor, oxidizable, security
Low.Due to can there is the redox reaction of Rapid reversible in metal oxide materials, thus having higher Faraday pseudo-capacitance
But still there is the problems such as noble metal is expensive, and transition metal oxide is more relatively low than electric capacity.Therefore, the task of top priority is to visit
It is the less expensive electrode material of practical application that rigging has high-performance and environmental friendliness.
The porous cobalt acid zinc nano structure electrode material of the present invention, under current density is for 3a/g, through the perseverance of 1500 times
Stream discharge and recharge, capacitance still keeps 81.3%, has good electrochemical stability.In addition this material has higher ratio
Capacitance, has broad application prospects in the field of electrochemical appliance.
Content of the invention
The purpose of the present invention aims to provide the preparation of a kind of simply reliable cobalt acid zinc nano wire or nanometer band electrode material
Method, and explore its application in super capacitor material.
The present invention is achieved through the following technical solutions:
A kind of cobalt acid zinc nano wire or the preparation method of nanometer band electrode material, comprise the steps:
Step 1, the preparation of cobalt acid zinc precursor solution:
The powder of soluble cobalt, soluble zinc salt, hexa, ammonium fluoride is added in distilled water, ultrasonic
Process, magnetic stirrer is uniformly, stand-by;
Step 2, the preparation of cobalt acid zinc precursor powder:
The cobalt acid zinc precursor solution of step 1 is transferred in the reactor of polytetrafluoroethylsubstrate substrate, sealing, carries out constant temperature
Thermal response, after completion of the reaction, is cooled to room temperature, solid product is washed, is vacuum dried, and obtains final product cobalt acid zinc precursor powder;
The preparation of step 3, cobalt acid zinc nano wire or nanobelt:
Calcined in tube furnace step 2 gained cobalt acid zinc precursor powder being put into inert gas shielding, that is, obtained
Cobalt acid zinc nano wire or nanobelt.
In step 1, the soluble cobalt that used, soluble zinc salt, hexa, ammonium fluoride are in distilled water
Substance withdrawl syndrome is than for 0.2~2:0.2~2:3~10:2~10;The described ultrasonically treated time is 5min.
In step 1, described soluble cobalt is any one in cobalt chloride, cobalt nitrate and cobalt acetate.
In step 1, described soluble zinc salt is any one in zinc chloride, zinc nitrate and zinc acetate.
In step 2, the temperature of described constant temperature thermal response is 100~160 DEG C, and the reaction time is 6~20 hours.
In step 3, described inert gas is argon gas;Described calcining heat be 200~500 DEG C, heating rate be 1~5 DEG C/
min.
Prepared cobalt acid zinc nano wire or nanobelt are used for making electrode of super capacitor, and preparation process is as follows:
Step a, by foam nickel sheet with cutting into a length of 1 centimetre * 5 centimetres of wide *, be then sequentially placed into acetone, volume
Fraction is 20% dilute hydrochloric acid solution, in water, each ultrasonically treated 5 minutes;After being disposed, vacuum drying, stand-by;
Step b, to mass fraction be 30% polytetrafluoroethylene aqueous dispersion in add cobalt acid zinc nano wire or nanobelt
With acetylene black, make cobalt acid zinc nano wire or nanobelt be 7~8:1~2:1 with the mass ratio of acetylene black, polytetrafluoroethylene (PTFE), mix,
Obtain a kind of sticky slurry, then slurry is applied in the foam nickel sheet handled well, finally in 60~150 DEG C of drying 3~6h
It is cooled to room temperature, standby.
Beneficial effect:
The present invention proposes one kind aboundresources, cheap raw material prepare cobalt acid zinc electrode material straightforward procedure with
And it is self-assembled into ultracapacitor.First, the pattern of this material is nano wire or nano-band array, and its specific surface area is larger, has
Sufficiently contact with electrode material beneficial to electrolyte.Secondly, the good conductivity of this material, electric charge migrates in electrode/electrolyte
Resistance is little, and its space structure is conducive to the insertion/abjection of work ion.In addition, this material is super as being assembled into
Level capacitor anode electroactive material, after repetitive cycling, its physics is relative with chemical property stable, especially stable electrochemical property.
Present invention process is simple in a word, and favorable reproducibility is cheap, meets eco-friendly requirement, is easy to produce in batches.
Through research, the cobalt acid zinc nano wire prepared by the present invention or nanobelt and acetylene black, the mass ratio of polytetrafluoroethylene (PTFE)
During for 7~8:1~2:1, the electrode of super capacitor obtaining has optimum performance.
Brief description
Fig. 1 divides for the x-ray powder diffraction of Example 1 and Example 2 of the present invention gained cobalt acid zinc nano wire and nanobelt
Analysis figure (xrd);
Fig. 2 is the scanning electron microscope (SEM) photograph (sem) of the embodiment of the present invention 1 gained cobalt acid zinc nano wire;
Fig. 3 is the scanning electron microscope (SEM) photograph (sem) of the embodiment of the present invention 2 gained cobalt acid zinc nanobelt;
Fig. 4 is the stable circulation life test figure of the embodiment of the present invention 1 gained cobalt acid zinc nano wire.
Specific embodiment
Below by specific embodiment, the invention will be further described.
Embodiment 1
The powder of the cobalt chloride of 2mmol, 1mmol zinc chloride, 6mmol hexa, 5mmol ammonium fluoride is added
80ml distilled water, is placed in 100ml beaker, puts into ultrasonic 5 minutes in Ultrasound Instrument, so that it is mixed with magnetic stirrer
Close uniformly.Above-mentioned solution is poured in the reactor of 100ml polytetrafluoroethylsubstrate substrate, sealing, be placed in baking oven, control baking oven
Temperature is 140 DEG C, reacts 10 hours, is cooled to room temperature, repeatedly washing, vacuum drying, obtains final product cobalt acid zinc precursor;Will be above-mentioned
Cobalt acid zinc precursor is put in tube furnace and is calcined at 400 DEG C, and calcinating speed is 1 DEG C/min, is incubated 2 hours, obtains cobalt acid
Zinc nano wire.In Fig. 1, each diffraction maximum position and relative intensity are all matched with jpcds card (75-0576), show that product is face
Heart cubic spinel type znco2o4.The length of the cobalt acid zinc nano wire prepared as can be seen from Figure 2 is 1.7~2.6 microns, width
For 185~305 nanometers.Fig. 4 shows cobalt acid zinc nano wire as electrode material for super capacitor, in 1500 cycle charge-discharges
Afterwards, capacitance keeps 81.3%.
Embodiment 2
The powder of the cobalt nitrate of 2mmol, 1mmol zinc acetate, 10mmol hexa, 5mmol ammonium fluoride is added
80ml distilled water, is placed in 100ml beaker, puts into ultrasonic 5 minutes in Ultrasound Instrument, so that it is mixed with magnetic stirrer
Close uniformly.Above-mentioned solution is poured in the reactor of 100 milliliters of polytetrafluoroethylsubstrate substrate, sealing, be placed in baking oven, control baking oven
Temperature be 160 DEG C, react 12 hours, be cooled to room temperature, repeatedly washing, vacuum drying, obtain final product cobalt acid zinc precursor;Will be above-mentioned
Cobalt acid zinc precursor is put in tube furnace and is calcined at 400 DEG C, and calcinating speed is 2 DEG C/min, is incubated 2 hours, obtains cobalt acid
Zinc hierarchy nanobelt.In Fig. 1, each diffraction maximum position and relative intensity are also all matched with jpcds card (75-0576),
Show that product is face-centered cubic spinel-type znco2o4.Prepare as can be seen from Figure 3 cobalt acid zinc nanobelt length be 2.5~
5.6 microns, width is 0.15~0.27 micron.
Embodiment 3
The powder of the cobalt chloride of 2mmol, 2mmol zinc chloride, 3mmol hexa, 10mmol ammonium fluoride is added
80ml distilled water, is placed in 100ml beaker, puts into ultrasonic 5 minutes in Ultrasound Instrument, so that it is mixed with magnetic stirrer
Close uniformly.Above-mentioned solution is poured in the reactor of 100ml polytetrafluoroethylsubstrate substrate, sealing, be placed in baking oven, control baking oven
Temperature is 120 DEG C, reacts 6 hours, is cooled to room temperature, repeatedly washing, vacuum drying, obtains final product cobalt acid zinc precursor;By above-mentioned cobalt
Sour zinc precursor is put in tube furnace and is calcined at 500 DEG C, and calcinating speed is 5 DEG C/min, is incubated 5 hours, obtains cobalt acid zinc
Hierarchy nano wire.
Prepared cobalt acid zinc nano wire or nanobelt are used as electrode of super capacitor, and preparation process is as follows:
Step a, by foam nickel sheet with cutting into a length of 1 centimetre * 5 centimetres of wide *, be then sequentially placed into acetone, volume
Fraction is 20% dilute hydrochloric acid solution, in water, each ultrasonically treated 5 minutes;After being disposed, vacuum drying, stand-by;
Step b, to mass fraction be 30% polytetrafluoroethylene aqueous dispersion in add cobalt acid zinc and acetylene black, make cobalt acid
Zinc nano wire or nanobelt are 7:2:1 with the mass ratio of acetylene black, polytetrafluoroethylene (PTFE), and wherein, the quality of cobalt acid zinc is 7mg, mixes
After even, obtain a kind of sticky slurry, then slurry is applied in the foam nickel sheet handled well, finally in 60 DEG C of drying 3~6h
It is cooled to room temperature, standby.
Embodiment 4
By the cobalt acetate of 0.2mmol, 0.2mmol zinc nitrate, 10mmol hexa, 2mmol ammonium fluoride powder
Add 80ml distilled water, be placed in 100ml beaker, put into ultrasonic 5 minutes in Ultrasound Instrument, made within 30 minutes with magnetic stirrer
It mixes.Above-mentioned solution is poured in the reactor of 100ml polytetrafluoroethylsubstrate substrate, sealing, be placed in baking oven, control and dry
The temperature of case is 100 DEG C, reacts 20 hours, is cooled to room temperature, repeatedly washing, vacuum drying, obtains final product cobalt acid zinc precursor;Will be upper
State cobalt acid zinc precursor to put in tube furnace and calcined at 200 DEG C, calcinating speed is 5 DEG C/min, is incubated 2 hours, obtains cobalt
Sour zinc hierarchy nano wire.
Prepared cobalt acid zinc nano wire or nanobelt are used as electrode of super capacitor, and preparation process is as follows:
Step a, by foam nickel sheet with cutting into a length of 1 centimetre * 5 centimetres of wide *, be then sequentially placed into acetone, volume
Fraction is 20% dilute hydrochloric acid solution, in water, each ultrasonically treated 5 minutes;After being disposed, vacuum drying, stand-by;
Step b, to mass fraction be 30% polytetrafluoroethylene aqueous dispersion in add cobalt acid zinc and acetylene black, make cobalt acid
Zinc nano wire or nanobelt are 8:1:1 with the mass ratio of acetylene black, polytetrafluoroethylene (PTFE), and wherein, the quality of cobalt acid zinc is 8mg, mixes
After even, obtain a kind of sticky slurry, then slurry is applied in the foam nickel sheet handled well, finally in 150 DEG C of drying 3~6h
It is cooled to room temperature, standby.
Claims (8)
1. the preparation method of a kind of cobalt acid zinc nano wire or nanometer band electrode material is it is characterised in that comprise the steps:
Step 1, the preparation of cobalt acid zinc precursor solution:
The powder of soluble cobalt, soluble zinc salt, hexa, ammonium fluoride is added in distilled water, ultrasonically treated,
Magnetic stirrer is uniformly, stand-by;
Step 2, the preparation of cobalt acid zinc precursor powder:
The cobalt acid zinc precursor solution of step 1 is transferred in the reactor of polytetrafluoroethylsubstrate substrate, sealing, carries out constant temp. heating anti-
Should, after completion of the reaction, it is cooled to room temperature, solid product is washed, is vacuum dried, obtain final product cobalt acid zinc precursor powder;
The preparation of step 3, cobalt acid zinc nano wire or nanobelt:
Calcined in tube furnace step 2 gained cobalt acid zinc precursor powder being put into inert gas shielding, that is, obtained cobalt acid
Zinc nano wire or nanobelt.
2. the preparation method of a kind of cobalt acid zinc nano wire according to claim 1 or nanometer band electrode material, its feature exists
In, in step 1, the soluble cobalt that used, soluble zinc salt, hexa, material in distilled water for the ammonium fluoride
Amount concentration ratio be 0.2~2:0.2~2:3~10:2~10;The described ultrasonically treated time is 5min.
3. the preparation method of a kind of cobalt acid zinc nano wire according to claim 1 or nanometer band electrode material, its feature exists
In, in step 1, described soluble cobalt is any one in cobalt chloride, cobalt nitrate and cobalt acetate.
4. the preparation method of a kind of cobalt acid zinc nano wire according to claim 1 or nanometer band electrode material, its feature exists
In, in step 1, described soluble zinc salt is any one in zinc chloride, zinc nitrate and zinc acetate.
5. the preparation method of a kind of cobalt acid zinc nano wire according to claim 1 or nanometer band electrode material, its feature exists
In in step 2, the temperature of described constant temperature thermal response is 100~160 DEG C, and the reaction time is 6~20 hours.
6. the preparation method of a kind of cobalt acid zinc nano wire according to claim 1 or nanometer band electrode material, its feature exists
In, in step 3, described inert gas is argon gas;Described calcining heat is 200~500 DEG C, and heating rate is 1~5 DEG C/min.
7. the purposes of the prepared cobalt acid zinc nano wire prepared by claim 1~6 any one or nanometer band electrode material,
It is characterized in that, described cobalt acid zinc nano wire or nanobelt are used for making electrode of super capacitor.
8. the purposes of cobalt acid zinc nano wire according to claim 7 or nanometer band electrode material is it is characterised in that described surpass
The preparation process of level electrode for capacitors is as follows:
Step a, by foam nickel sheet with cutting into a length of 1 centimetre * 5 centimetres of wide *, be then sequentially placed into acetone, volume fraction
In dilute hydrochloric acid solution for 20%, water, each ultrasonically treated 5 minutes;After being disposed, vacuum drying, stand-by;
Step b, to mass fraction be 30% polytetrafluoroethylene aqueous dispersion in add cobalt acid zinc nano wire or nanobelt and second
Acetylene black, makes cobalt acid zinc nano wire or nanobelt be 7~8:1~2:1 with the mass ratio of acetylene black, polytetrafluoroethylene (PTFE), mixes, obtain
A kind of sticky slurry, then slurry is applied in the foam nickel sheet handled well, finally cool down in 60~150 DEG C of drying 3~6h
To room temperature, standby.
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Cited By (3)
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CN107032414A (en) * | 2017-03-13 | 2017-08-11 | 中山大学 | A kind of preparation method of the sour zinc nano-material of flexible cobalt |
CN108962614A (en) * | 2018-06-15 | 2018-12-07 | 五邑大学 | A kind of preparation method of the porous structure cobalt acid zinc containing carbon composite electrode material |
CN112537798A (en) * | 2020-12-07 | 2021-03-23 | 中国民用航空飞行学院 | Preparation method of zinc cobaltate nanowire |
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CN108962614A (en) * | 2018-06-15 | 2018-12-07 | 五邑大学 | A kind of preparation method of the porous structure cobalt acid zinc containing carbon composite electrode material |
CN112537798A (en) * | 2020-12-07 | 2021-03-23 | 中国民用航空飞行学院 | Preparation method of zinc cobaltate nanowire |
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