CN106971855A - A kind of nickel ferrite based magnetic loaded nanoparticle electrode material and preparation method and purposes - Google Patents
A kind of nickel ferrite based magnetic loaded nanoparticle electrode material and preparation method and purposes Download PDFInfo
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- CN106971855A CN106971855A CN201710229629.7A CN201710229629A CN106971855A CN 106971855 A CN106971855 A CN 106971855A CN 201710229629 A CN201710229629 A CN 201710229629A CN 106971855 A CN106971855 A CN 106971855A
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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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- 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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- 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
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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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- 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 kind of nickel ferrite based magnetic loaded nanoparticle electrode material and preparation method and purposes, preparation method is as follows：Step 1, the powder of nickel salt, molysite, hexa, ammonium fluoride added in distilled water, ultrasound, then it is well mixed with magnetic stirrer, obtain precursor solution, it is stand-by；Step 2, the precursor solution of step 1 poured into the reactor of polytetrafluoroethylsubstrate substrate, seal, be placed in baking oven, the temperature of baking oven is controlled to carry out hydro-thermal reaction between 140~200 DEG C, room temperature is cooled to, washing, vacuum drying produce nickel ferrite based magnetic loaded nanoparticle electrode material.The present invention proposes one kind and uses abundance, and cheap raw material prepares the straightforward procedure of ferrous acid nickel electrode material, and can be further used as electrode material for super capacitor.
Description
Technical field
The invention belongs to nano composite material technical field, and in particular to a kind of new nickel ferrite based magnetic loaded nanoparticle electrode material
Material and preparation method and purposes.
Background technology
With developing rapidly for economic society, the height of environmental degradation that fossil energy is triggered, lack of energy by various countries
Degree concern, and new energy storage equipment such as ultracapacitor (ECs) is had extended cycle life due to charge-discharge velocity height, is worked
Temperature range is wide, the advantages of environmentally safe, be known as by scientist be most potential alleviating energy crisis energy storage device.
Electrode material is the important component of ultracapacitor, is to influence the pass of ultracapacitor production cost and performance
Key factor.Electrode material for super capacitor mainly has carbon material, metal oxide materials and conducting polymer materials.Carbon material has
Have extended cycle life, cost it is low, but its specific capacitance is relatively low 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
It is low.Metal oxide materials are due to that can occur the redox reaction of Rapid reversible, so that with higher Faraday pseudo-capacitance
But still it is expensive to there is noble metal, the problems such as transition metal oxide specific capacitance is relatively low.Therefore, the task of top priority is to visit
Rigging has high-performance and the environment-friendly electrode material less expensive for practical application.
The nickel ferrite based magnetic loaded nanoparticle electrode material of the present invention, in the case where current density is 4A/g, fills by the constant current of 1500 times
Electric discharge, capacitance still keeps 80.3%, with good electrochemical stability.In addition the material has higher specific capacitance
Value, has broad application prospects in the field of electrochemical appliance.
The content of the invention
The purpose of the present invention aims to provide a kind of simple reliable preparation side based on nickel ferrite based magnetic loaded nanoparticle electrode material
Method.
To achieve the above object, the technical solution adopted by the present invention is by a certain amount of nickel chloride, ferric nitrate, hexa-methylene
Tetramine, the powder of ammonium fluoride add distilled water, are well mixed, are transferred in the reactor of polytetrafluoroethylsubstrate substrate, through high-temperature water
After thermal response, product is washed, nickel ferrite based magnetic loaded nano material is dried to obtain, then electrode of super capacitor is made in resulting materials.
Concrete technical scheme is as follows：
In a kind of nickel ferrite based magnetic loaded nanoparticle electrode material, the nickel ferrite based magnetic loaded nanoparticle electrode material, nickel ferrite based magnetic loaded nanometer
The pattern of grain is irregular spheric granules, and average grain diameter is 47nm；The ferrous acid nano nickel particles are used for super capacitor electrode
Pole material, after 1500 cycle charge-discharges, capacitance still keeps more than 80.3%.
A kind of preparation method of nickel ferrite based magnetic loaded nanoparticle electrode material, step is as follows：
The preparation of step 1, precursor solution：
The powder of a certain amount of nickel salt, molysite, hexa, ammonium fluoride is added in distilled water, 100ml burnings are placed in
In cup, ultrasound a period of time in Ultrasound Instrument is put into, then is well mixed 30 minutes it with magnetic stirrer, presoma is obtained
Solution, it is stand-by；
The preparation of step 2, nickel ferrite based magnetic loaded nanoparticle electrode material：
In the reactor that the precursor solution of step 1 is poured into 100ml polytetrafluoroethylsubstrate substrates, sealing is placed in baking oven,
Control the temperature of baking oven to carry out hydro-thermal reaction between 140~200 DEG C, react 6~20 hours, be cooled to room temperature, repeatedly wash,
Vacuum drying, produces nickel ferrite based magnetic loaded nanoparticle electrode material.
In step 1, described nickel salt, molysite, hexa, the mol ratio of ammonium fluoride are 0.2~2：0.2~2：3
~10：2~10, concentration of the nickel salt in distilled water is 5~25mmol/L.
Described nickel salt is any in nickel chloride, nickel nitrate and nickel acetate.
Described molysite is any in iron chloride, ferric nitrate and ferric acetate.
In step 2, the hydrothermal temperature is 140~200 DEG C, and the time is 6~20 hours.
Nickel ferrite based magnetic loaded nanoparticle electrode material as electrode material for super capacitor preparation：
Be respectively 1 centimetre * 5 centimetres of fritter with scissor cut Cheng Kuanchang by the foam nickel sheet bought, then by its according to
It is secondary to be respectively placed in acetone soln, dilute hydrochloric acid solution (20%), the aqueous solution, and ultrasonically treated each 5 minutes.It is placed in after handling well true
Dried in empty drying box, it is stand-by.
It is 7~8 in mass ratio by nickel ferrite based magnetic loaded nanoparticle electrode material and acetylene black, polytetrafluoroethylene (PTFE)：1~2:1 is uniform
Mixing, obtains sticky slurry, then whole slurry are applied in ready foam nickel sheet, finally dries 3 at 60~150 DEG C
It is cooled to room temperature within~6 hours, obtains electrode material for super capacitor.
Described nickel ferrite based magnetic loaded, acetylene black, polytetrafluoroethylene (PTFE) mass ratio are 7~8：1~2:1, described drying temperature is
60~150 degree, drying time is 3~6 hours.
Beneficial effect：
The present invention proposes one kind and uses abundance, and cheap raw material prepares the simple side of ferrous acid nickel electrode material
Method, and electrode material for super capacitor can be further used as.First, the pattern of the material be nano particle, its specific surface area compared with
Greatly, fully contacting for electrolyte and electrode material is conducive to.Secondly, the good conductivity of the material, electric charge is in electrode/electrolyte
Migration resistance is small, and its space structure is conducive to insertion/abjection of active ion.In addition, the material is used as super electricity
The active material of capacitor positive electrode material, is repeated after charge and discharge cycles, and its physics and chemical property are stablized relatively.Work of the present invention in a word
Skill is simple, and favorable reproducibility is cheap, meets environment-friendly requirement, is easy to batch production.
Brief description of the drawings
Fig. 1 is the X-ray powder diffraction analysis chart (XRD) of the gained ferrous acid nano nickel particles of the embodiment of the present invention 1；
Fig. 2 is the scanning electron microscope (SEM) photograph (SEM) of the gained ferrous acid nano nickel particles of the embodiment of the present invention 1；
Fig. 3 is the grain size distribution of the gained ferrous acid nano nickel particles of the embodiment of the present invention 1；
Fig. 4 is the cycle life test chart of the gained ferrous acid nano nickel particles of the embodiment of the present invention 1.
Embodiment
The present invention is expanded on further below by example, but protection scope of the present invention is not limited to these examples.This
Raw material in invention example is purchased from Shanghai Chinese medicines group, is that analysis is pure.
Embodiment 1
The powder of 2mmol nickel chloride, 1mmol ferric nitrates, 6mmol hexas, 5mmol ammonium fluorides is added
80ml distilled water, is placed in 100ml beakers, is put into ultrasound 5 minutes in Ultrasound Instrument, mixes 30 minutes it with magnetic stirrer
Close uniform.In the reactor that above-mentioned solution is poured into 100ml polytetrafluoroethylsubstrate substrates, sealing is placed in baking oven, control baking oven
Temperature is 200 DEG C, reacts 10 hours, is cooled to room temperature, and repeatedly washing, vacuum drying, produce ferrous acid nano nickel particles.Gained iron
Sour nano nickel particles and acetylene black, polytetrafluoroethylene (PTFE) are in certain mass ratio 8:1:1 uniform mixing, obtains a kind of sticky silt
Slurry, then whole slurry are applied in foam nickel sheet, finally it is cooled to room temperature within 3 hours in 150 degree of dryings, obtains nickel ferrite based magnetic loaded nanometer
Mosaic electrode material.Each diffraction maximum position and relative intensity match with the JPCDS cards (10-0325) of nickel ferrite based magnetic loaded in Fig. 1,
It is face-centered cubic spinel-type ferrous acid nickel to show product.Ferrous acid nano nickel particles have successfully been prepared as can be seen from Figure 2.From it
Grain size distribution (Fig. 3) understands that the average grain diameter of the ferrous acid nano nickel particles prepared is 47 nanometers.Fig. 4 shows nickel ferrite based magnetic loaded nanometer
Grain is as electrode material for super capacitor, and after 1500 cycle charge-discharges, capacitance still keeps more than 80.3%.
Embodiment 2
The powder of 2mmol ferric nitrate, 1mmol nickel acetates, 10mmol hexas, 5mmol ammonium fluorides is added
80ml distilled water, is placed in 100ml beakers, is put into ultrasound 5 minutes in Ultrasound Instrument, mixes 30 minutes it with magnetic stirrer
Close uniform.In the reactor that above-mentioned solution is poured into 100 milliliters of polytetrafluoroethylsubstrate substrates, sealing is placed in baking oven, controls baking oven
Temperature be 180 DEG C, react 12 hours, be cooled to room temperature, repeatedly washing, vacuum drying, produce ferrous acid nano nickel particles.Gained
Ferrous acid nano nickel particles and acetylene black, polytetrafluoroethylene (PTFE) are in certain mass ratio 7:2:1 uniform mixing, obtains a kind of sticky silt
Slurry, then whole slurry are applied in foam nickel sheet, finally it is cooled to room temperature within 5 hours in 130 degree of dryings, obtains nickel ferrite based magnetic loaded nanometer
Mosaic electrode material.
Embodiment 3
The powder of 2mmol nickel chloride, 2mmol ferric nitrates, 3mmol hexas, 10mmol ammonium fluorides is added
80ml distilled water, is placed in 100ml beakers, is put into ultrasound 5 minutes in Ultrasound Instrument, mixes 30 minutes it with magnetic stirrer
Close uniform.In the reactor that above-mentioned solution is poured into 100ml polytetrafluoroethylsubstrate substrates, sealing is placed in baking oven, control baking oven
Temperature is 160 DEG C, reacts 6 hours, is cooled to room temperature, and repeatedly washing, vacuum drying, that is, obtain nickel ferrite based magnetic loaded nano particle.Gained
Ferrous acid nano nickel particles and acetylene black, polytetrafluoroethylene (PTFE) are in certain mass ratio 8:1:1 uniform mixing, obtains a kind of sticky silt
Slurry, then whole slurry are applied in foam nickel sheet, finally it is cooled to room temperature within 6 hours in 100 degree of dryings, obtains nickel ferrite based magnetic loaded nanometer
Mosaic electrode material.
Embodiment 4
By 0.2mmol ferric acetate, 0.2mmol nickel nitrates, 10mmol hexas, 2mmol ammonium fluorides powder
40ml distilled water is added, is placed in 50ml beakers, ultrasound 5 minutes in Ultrasound Instrument is put into, is made within 30 minutes with magnetic stirrer
It is well mixed.In the reactor that above-mentioned solution is poured into 50ml polytetrafluoroethylsubstrate substrates, sealing is placed in baking oven, and control is dried
The temperature of case is 140 DEG C, reacts 20 hours, is cooled to room temperature, and repeatedly washing, vacuum drying, produce nickel ferrite based magnetic loaded；By above-mentioned ferrous acid
Nickel is put into tube furnace to be calcined at 200 DEG C, and calcinating speed is 5 degree per minute, is incubated 2 hours, obtains nickel ferrite based magnetic loaded classification knot
Structure nano particle.By gained nickel ferrite based magnetic loaded and acetylene black, polytetrafluoroethylene (PTFE) in certain mass ratio 8:1:1 uniform mixing, obtains one
Sticky slurry is planted, then whole slurry are smeared in above-mentioned ready foam nickel sheet, finally dries 6 hours and cools down at 150 degree
To room temperature, nickel ferrite based magnetic loaded nanoparticle electrode material is obtained.
Description to examples detailed above is understood that for ease of those skilled in the art and using the present invention.It is ripe
Know the personnel of art technology obviously can easily make various modifications to these examples, and General Principle described herein
It is applied in other examples without passing through performing creative labour.Therefore, the invention is not restricted to example here, art technology
Personnel are according to the announcement of the present invention, and the improvement made for the present invention and modification all should be within protection scope of the present invention.
Claims (9)
1. a kind of nickel ferrite based magnetic loaded nanoparticle electrode material, it is characterised in that in the nickel ferrite based magnetic loaded nanoparticle electrode material, ferrous acid
The pattern of nano nickel particles is irregular spheric granules, and average grain diameter is 47nm；The ferrous acid nano nickel particles are used for super
Capacitor electrode material, after 1500 cycle charge-discharges, capacitance still keeps more than 80.3%.
2. a kind of preparation method of nickel ferrite based magnetic loaded nanoparticle electrode material as claimed in claim 1, it is characterised in that step is such as
Under：
The preparation of step 1, precursor solution：
The powder of nickel salt, molysite, hexa, ammonium fluoride is added in distilled water, ultrasound, then use magnetic stirrer
It is well mixed, precursor solution is obtained, it is stand-by；
The preparation of step 2, nickel ferrite based magnetic loaded nanoparticle electrode material：
In the reactor that the precursor solution of step 1 is poured into polytetrafluoroethylsubstrate substrate, sealing is placed in baking oven, controls baking oven
Temperature be to carry out hydro-thermal reaction between 140~200 DEG C, be cooled to room temperature, washing, vacuum drying produce nickel ferrite based magnetic loaded nanometer
Grain electrode material.
3. a kind of preparation method of nickel ferrite based magnetic loaded nanoparticle electrode material as claimed in claim 2, it is characterised in that step 1
In, described nickel salt, molysite, hexa, the mol ratio of ammonium fluoride are 0.2~2：0.2~2：3~10：2~10, institute
Concentration of the nickel salt in distilled water is stated for 5~25mmol/L.
4. a kind of preparation method of nickel ferrite based magnetic loaded nanoparticle electrode material as claimed in claim 2 or claim 3, it is characterised in that institute
The nickel salt stated is any in nickel chloride, nickel nitrate and nickel acetate.
5. a kind of preparation method of nickel ferrite based magnetic loaded nanoparticle electrode material as claimed in claim 2 or claim 3, it is characterised in that institute
The molysite stated is any in iron chloride, ferric nitrate and ferric acetate.
6. a kind of preparation method of nickel ferrite based magnetic loaded nanoparticle electrode material as claimed in claim 2, it is characterised in that step 1
In, in step 2, the hydrothermal temperature is 140~200 DEG C, and the time is 6~20 hours.
7. a kind of nickel ferrite based magnetic loaded nanoparticle electrode material described in claim 1 is used as the purposes for preparing super capacitor material.
8. a kind of nickel ferrite based magnetic loaded nanoparticle electrode material described in claim 7 is used as the purposes for preparing super capacitor material,
Characterized in that, preparation process is as follows：Nickel ferrite based magnetic loaded nanoparticle electrode material is equal in mass ratio with acetylene black, polytetrafluoroethylene (PTFE)
Even mixing, obtains sticky slurry, then whole slurry are applied in ready foam nickel sheet, finally dries, obtains super
Capacitor electrode material.
9. a kind of nickel ferrite based magnetic loaded nanoparticle electrode material as claimed in claim 8 is used as the use for preparing super capacitor material
On the way, it is characterised in that described nickel ferrite based magnetic loaded, acetylene black, polytetrafluoroethylene (PTFE) mass ratio are 7~8：1~2:1, described drying
Temperature is 60~150 degree, and drying time is 3~6 hours.
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Cited By (6)
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| CN107308922A (en) * | 2017-08-28 | 2017-11-03 | 华南师范大学 | A kind of water process is with Ni-based from growth three-dimensional material and preparation method thereof |
| CN107452952A (en) * | 2017-08-16 | 2017-12-08 | 华南师范大学 | A kind of composite of nickel ferrite based magnetic loaded and silicon and its preparation method and application |
| CN107597124A (en) * | 2017-09-22 | 2018-01-19 | 常州大学 | A kind of preparation method of Nano Carbon nickel ferrite based magnetic loaded |
| CN107761128A (en) * | 2017-11-10 | 2018-03-06 | 上海应用技术大学 | A kind of FeNiNC electrode materials, preparation method and applications |
| CN110040789A (en) * | 2019-04-17 | 2019-07-23 | 天津大学 | A kind of preparation method of nickel ferrite based magnetic loaded microballoon electrode material for super capacitor |
| CN113249743A (en) * | 2021-05-18 | 2021-08-13 | 上海大学 | Catalyst for electrocatalytic oxidation of glycerol and preparation method thereof |
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| CN113249743A (en) * | 2021-05-18 | 2021-08-13 | 上海大学 | Catalyst for electrocatalytic oxidation of glycerol and preparation method thereof |
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