CN109599271A - A kind of electrode material Ni3V2O8And its synthetic method - Google Patents
A kind of electrode material Ni3V2O8And its synthetic method Download PDFInfo
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- CN109599271A CN109599271A CN201811414465.6A CN201811414465A CN109599271A CN 109599271 A CN109599271 A CN 109599271A CN 201811414465 A CN201811414465 A CN 201811414465A CN 109599271 A CN109599271 A CN 109599271A
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- electrode material
- deionized water
- nicl
- microballoon
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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
- H01G11/46—Metal oxides
-
- 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
-
- 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 present invention relates to a kind of electrode material Ni3V2O8And its synthetic method.Herein with NiCl2•6H2O、NH3•H2O and NH4VO3For raw material, Ni is synthesized with microwave assisting method3V2O8Microballoon.Nickel has the advantages that theoretical capacity is high, and vanadium then has a variety of valence states, in nature rich reserves.Using them as raw material, their intrinsic structural properties are effectively combined, the Ni prepared with microwave assisting method3V2O8Microballoon shows excellent chemical property.This result shows that, Ni3V2O8There is preferable development prospect in following electrochemical energy storage field as electrode material for super capacitor, in addition, this energy-efficient microwave assisting method also provides reference foundation for the energy storage in other fields.
Description
Technical field
The invention belongs to supercapacitor fields, and in particular to one kind is with NiCl2•6H2O, NH3•H2O and NH4VO3For original
Material synthesizes electrode material for super capacitor Ni with microwave assisting method3V2O8Technology.
Background technique
With the rapid development of economy, to energy demand be continuously increased and the lasting consumption of fossil fuel, environmental pollution
Problem is increasingly prominent, is alleviating energy crisis and improvement environment, and more and more researchers are dedicated to studying clean energy resource.And surpass
Grade capacitor causes the extensive concern of researcher as a kind of energy storage device, this is because supercapacitor function with higher
Rate density, excellent cyclical stability, it is environmentally friendly and at low cost the advantages that.The capacitive property of supercapacitor mainly depends on
In the electrode material of supercapacitor, so the research of preparation and performance to electrode material for super capacitor is this field
Research emphasis.In recent years, people constantly look for being suitble to electrode material for super capacitor, achieve certain research achievement.Recently,
Transition metal vanadate has carried out research by some researchers and has been considered as preferable electrode of super capacitor material
Material.The Ni that many researchers prepare3V2O8And compound all shows more excellent chemical property, but its
Synthetic method takes a long time.This just causes us to explore a kind of more efficient method, while the sample prepared is gathered around again
There is preferably chemical property.
Microwave assisting method is a kind of novel method, and this method has that easy to operate, reaction speed is fast, safety and energy conservation
The advantages that.Nickel has the advantages that theoretical capacity is high, and vanadium then has a variety of valence states, in nature rich reserves.It is with them
Raw material, the Ni prepared with microwave assisting method3V2O8Microballoon shows excellent chemical property, this is because Ni3V2O8Microballoon
When carrying out charge and discharge in KOH electrolyte as electrode material, there is biggish specific surface area, be conducive to electrode material and electrolysis
Liquid comes into full contact with, and accelerates electron transmission, to improve the redox reaction degree of active material.This result shows that,
Ni3V2O8Microballoon has preferable development prospect in following electrochemical energy storage field as electrode material for super capacitor, this
Outside, this energy-efficient microwave assisting method also provides reference foundation for the energy storage in other fields.
Summary of the invention
For current Ni3V2O8The disadvantages such as the preparation method of electrode material is complicated, poor circulation, and energy density is low, this hair
It is bright to provide a kind of low in cost, high-performance, no pollution to the environment Ni3V2O8Microballoon electrode material and its efficient energy-saving safe
Preparation method.
Ni proposed by the present invention3V2O8Microballoon electrode material is made with microwave assisting method.The method can be by nickel and vanadium
Intrinsic property is effectively combined, and microwave method is directly radiated energy on reactant with microwave, generates molecule
High speed rotation and collision, to synthesize Ni3V2O8Microballoon.Products therefrom specific capacitance with higher and good stable circulation
Property, method have many advantages, such as easy to operate, low in cost, safety non-pollution, high-efficient.
Ni proposed by the present invention3V2O8Microballoon the preparation method is as follows:
1, with NiCl2•6H2O, NH3•H2O and NH4VO3For raw material, by 7.5-8mmol NiCl2•6H2O and 1-5 mL NH3•H2O
It is dissolved in 15-25 mL deionized waters, obtains NiCl2And NH3•H2The mixed solution of O.
2, by 4-5 mmol NH4VO3It is dissolved in 75-85 DEG C of the deionized water of 15-25 mL of other portion, obtains
NH4VO3Solution.
3, by NiCl2And NH3•H2The instillation NH of the mixed solution of O at the uniform velocity4VO3In solution, under 75-85 DEG C of water bath conditions
Uniform suspension is formed after 5-10 min of stirring.
4, suspension obtained by previous step is transferred in the round-bottomed flask of 100 mL, using microwave reaction instrument 100-300
W is stirred at reflux 15-60 min under the conditions of 40-100 DEG C, obtains yellow mercury oxide Ni3V2O8。
5, the obtained yellow mercury oxide of previous step is filtered, and is washed 3-5 times with deionized water and dehydrated alcohol respectively,
55-65 DEG C of dry 6-12 h in air dry oven are then placed in, Ni is finally obtained3V2O8Electrode material.
By X-ray powder diffraction (XRD) and scanning electron microscope respectively to obtained Ni3V2O8Electrode material object phase and
Pattern is characterized, and by electro-chemical test, is evaluated its specific capacitance.
Detailed description of the invention
Fig. 1 is the XRD curve of obtained sample.
Fig. 2 is the stereoscan photograph of obtained sample.
Fig. 3 is the charging and discharging curve of made sample.
Specific embodiment
Embodiment
By 7.6 mmol NiCl2•6H2O and 3 mL NH3•H2O is dissolved in 20 mL deionized waters, obtains NiCl2And NH3•
H2The mixed solution of O is added dropwise to the NH of 0.5 mol/L of 80 DEG C of 20 mL4VO3In solution, 10 are stirred under 80 DEG C of water-baths
After min, suspension is transferred in the round-bottomed flask of 100 mL, is stirred at reflux at 200 W, 40 DEG C using microwave reaction instrument
30 min.Obtained precipitating is washed three times with deionized water and dehydrated alcohol respectively, is then placed in air dry oven 60 DEG C
Dry 6 h.Finally obtain Ni3V2O8Electrode material.By X-ray powder diffraction (XRD) and scanning electron microscope respectively to made
The electrode material object phase and pattern obtained is characterized, the results showed that prepared sample and Ni3V2O8Standard card PDF#74-
1484 is consistent, and pattern is in microballoon, and size is in 200 nm or so；And electro-chemical test is carried out to it, the results showed that obtain
Ni3V2O8Electrode material has higher specific capacitance, and when current density is 1A/g, specific capacitance value is up to 1230 F/g.
Claims (6)
1. a kind of Ni3V2O8Microballoon electrode material, it is characterised in that the preparation method is as follows: (1) is with NiCl2•6H2O, NH3•H2O and
NH4VO3For raw material, by NiCl2•6H2O and NH3•H2O is dissolved in deionized water, obtains NiCl2And NH3•H2The mixed solution of O；
(2) by NH4VO3It is dissolved in in addition a deionized water, obtains NH4VO3Solution；(3) by NiCl2And NH3•H2The mixed solution of O
Instillation NH at the uniform velocity4VO3In solution, uniform suspension is formed after heating water bath and stirring；(4) it will suspend obtained by previous step
Liquid is transferred in the round-bottomed flask of 100 mL, is reacted, is obtained using microwave reaction instrument regulation power, temperature and reaction time
Yellow mercury oxide Ni3V2O8；(5) the obtained yellow mercury oxide of previous step is filtered, and is washed respectively with deionized water and dehydrated alcohol
It washs, is then placed in drying in air dry oven, finally obtains Ni3V2O8Electrode material.
2. Ni as described in claim 13V2O8Microballoon electrode material, it is characterised in that step (1) described NiCl2•6H2O dosage
For 7.5-8mmol, NH3•H2O dosage is 1-5 mL, and deionized water dosage is 15-25 mL.
3. Ni as described in claim 13V2O8Microballoon electrode material, it is characterised in that step (2) described NH4VO3Dosage is 4-5
Mmol, deionized water dosage are 15-25 mL, and deionized water temperature is 75-85 DEG C.
4. Ni as described in claim 13V2O8Microballoon electrode material, it is characterised in that step (3) described water bath heating temperature is
75-85 DEG C, mixing time is 5-10 min.
5. Ni as described in claim 13V2O8Microballoon electrode material, it is characterised in that step (4) microwave power is 100-
300 W, heating temperature are 40-100 DEG C, and return time is 15-60 min.
6. Ni as described in claim 13V2O8Microballoon electrode material, it is characterised in that step (5) deionized water and anhydrous
Ethanol washing number is respectively 3-5 times, and drying temperature is 55-65 DEG C, and drying time is 6-12 h.
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| Application Number | Priority Date | Filing Date | Title |
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| CN201811414465.6A CN109599271A (en) | 2018-11-26 | 2018-11-26 | A kind of electrode material Ni3V2O8And its synthetic method |
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| CN201811414465.6A CN109599271A (en) | 2018-11-26 | 2018-11-26 | A kind of electrode material Ni3V2O8And its synthetic method |
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Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN110364372A (en) * | 2019-08-02 | 2019-10-22 | 浙江工业大学 | A kind of supercapacitor vanadic acid nickel material, preparation method and application |
| CN111816454A (en) * | 2020-07-02 | 2020-10-23 | 西安交通大学 | Foamed nickel loaded NiCo2V2O8Method for assembling flexible supercapacitor |
| CN113171746A (en) * | 2021-04-26 | 2021-07-27 | 内江师范学院 | Flaky nickel vanadate nano material for adsorbing VB and preparation method thereof |
-
2018
- 2018-11-26 CN CN201811414465.6A patent/CN109599271A/en active Pending
Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN110364372A (en) * | 2019-08-02 | 2019-10-22 | 浙江工业大学 | A kind of supercapacitor vanadic acid nickel material, preparation method and application |
| CN111816454A (en) * | 2020-07-02 | 2020-10-23 | 西安交通大学 | Foamed nickel loaded NiCo2V2O8Method for assembling flexible supercapacitor |
| CN113171746A (en) * | 2021-04-26 | 2021-07-27 | 内江师范学院 | Flaky nickel vanadate nano material for adsorbing VB and preparation method thereof |
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