CN106971855B - 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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- CN106971855B CN106971855B CN201710229629.7A CN201710229629A CN106971855B CN 106971855 B CN106971855 B CN 106971855B CN 201710229629 A CN201710229629 A CN 201710229629A CN 106971855 B CN106971855 B CN 106971855B
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- 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 provides a kind of nickel ferrite based magnetic loaded nanoparticle electrode material and preparation methods and purposes, the preparation method is as follows: step 1, will nickel salt, molysite, hexa, ammonium fluoride powder be added distilled water in, ultrasound, it is uniformly mixed it with magnetic stirrer again, precursor solution is obtained, for use；Step 2 pours into the precursor solution of step 1 in the reaction kettle of polytetrafluoroethylsubstrate substrate, and sealing is placed in baking oven, the temperature of control baking oven is to carry out hydro-thermal reaction between 140~200 DEG C, it is cooled to room temperature, washs, is dried in vacuo to get nickel ferrite based magnetic loaded nanoparticle electrode material.Abundance is used the invention proposes a kind of, 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 nanocomposite technical fields, and in particular to a kind of novel nickel ferrite based magnetic loaded nanoparticle electrode material
Material and preparation method and purposes.
Background technique
With the rapid development of economic society, height of the environmental degradation, lack of energy that fossil energy is caused by various countries
Degree concern, and novel energy storage equipment such as supercapacitor (ECs) is had extended cycle life due to charge-discharge velocity height, is worked
The advantages that temperature range is wide, no pollution to the environment, be known as by scientist be most potential alleviating energy crisis energy storage device.
Electrode material is the important component of supercapacitor, is the pass for influencing supercapacitor production cost and performance
Key factor.Electrode material for super capacitor mainly has carbon material, metal oxide materials and conducting polymer materials.Carbon material tool
Many advantages, such as having extended cycle life, be at low cost, 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 thermal stability is poor, oxidizable, safety
It is low.Redox reaction of the metal oxide materials since Rapid reversible can occur, thus Faraday pseudo-capacitance with higher
But still the problems such as that there are noble metals is expensive, and transition metal oxide specific capacitance is relatively low.Therefore, the task of top priority is to visit
Rigging has high-performance and the environmental-friendly electrode material cheaper for practical application.
Nickel ferrite based magnetic loaded nanoparticle electrode material of the invention is filled in the case where current density is 4A/g by 1500 constant currents
Electric discharge, capacitance still keep 80.3%, have good electrochemical stability.In addition to this material specific capacitance with higher
Value, has broad application prospects in the field of electrochemical appliance.
Summary of the invention
The purpose of the present invention is intended to provide a kind of simple preparation side reliably 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 that by a certain amount of nickel chloride, ferric nitrate, hexa-methylene
The powder addition distilled water of tetramine, ammonium fluoride, is uniformly mixed, is transferred in the reaction kettle of polytetrafluoroethylsubstrate substrate, through high-temperature water
After thermal response, by product washing, it is dried to obtain nickel ferrite based magnetic loaded nano material, then electrode of super capacitor is made in resulting materials.
Specific technical solution is as follows:
A kind of nickel ferrite based magnetic loaded nanoparticle electrode material, in the nickel ferrite based magnetic loaded nanoparticle electrode material, nickel ferrite based magnetic loaded nanometer
The pattern of grain is irregular spheric granules, average grain diameter 47nm；The ferrous acid nano nickel particles are used for super capacitor electrode
Pole material, after 1500 cycle charge-discharges, capacitance still keeps 80.3% or more.
A kind of preparation method of nickel ferrite based magnetic loaded nanoparticle electrode material, steps are 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 burning is placed in
In cup, it is put into ultrasound a period of time in Ultrasound Instrument, then be uniformly mixed it with magnetic stirrer 30 minutes, obtains presoma
Solution, for use；
The preparation of step 2, nickel ferrite based magnetic loaded nanoparticle electrode material:
The precursor solution of step 1 is poured into the reaction kettle of 100ml polytetrafluoroethylsubstrate substrate, seals, be placed in baking oven,
The temperature of control baking oven is that hydro-thermal reaction is carried out between 140~200 DEG C, reacts 6~20 hours, is cooled to room temperature, repeatedly wash,
Vacuum drying is to get nickel ferrite based magnetic loaded nanoparticle electrode material.
In step 1, the nickel salt, molysite, hexa, ammonium fluoride molar ratio be 0.2~2:0.2~2:3
~10:2~10, concentration of the nickel salt in distilled water are 5~25mmol/L.
The nickel salt is any in nickel chloride, nickel nitrate and nickel acetate.
The 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.
Preparation of the nickel ferrite based magnetic loaded nanoparticle electrode material as electrode material for super capacitor:
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%), in aqueous solution, and be ultrasonically treated each 5 minutes.It handles well and is placed on very
It is dry in empty drying box, for use.
It with acetylene black, polytetrafluoroethylene (PTFE) is in mass ratio that 7~8:1~2:1 is uniform by nickel ferrite based magnetic loaded nanoparticle electrode material
Mixing, obtains sticky slurry, then whole slurry are applied to ready nickel foam on piece, finally at 60~150 DEG C dry 3
It is cooled to room temperature within~6 hours, obtains electrode material for super capacitor.
The nickel ferrite based magnetic loaded, acetylene black, polytetrafluoroethylene (PTFE) mass ratio are 7~8:1~2:1, and the drying temperature is
60~150 degree, drying time is 3~6 hours.
The utility model has the advantages that
Abundance is used the invention proposes a kind of, 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.Firstly, the pattern of the material be nano particle, specific surface area compared with
Greatly, be conducive to coming into full contact with for electrolyte and electrode material.Secondly, the good conductivity of the material, charge is in electrode/electrolyte
Migration resistance is small, and its space structure is conducive to insertion/abjection of active ion.In addition to this, the material is as super electricity
The active material of capacitor positive electrode material, after repeating charge and discharge cycles, physics and chemical property are relatively stable.Work of the present invention in a word
Skill is simple, favorable reproducibility, cheap, meets environmental-friendly requirement, convenient for batch production.
Detailed description of the invention
Fig. 1 is the X-ray powder diffraction analysis chart (XRD) of 1 gained ferrous acid nano nickel particles of the embodiment of the present invention；
Fig. 2 is the scanning electron microscope (SEM) photograph (SEM) of 1 gained ferrous acid nano nickel particles of the embodiment of the present invention；
Fig. 3 is the grain size distribution of 1 gained ferrous acid nano nickel particles of the embodiment of the present invention；
Fig. 4 is the cycle life test chart of 1 gained ferrous acid nano nickel particles of the embodiment of the present invention.
Specific embodiment
Below by example, the present invention is further explained, 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 the nickel chloride of 2mmol, 1mmol ferric nitrate, 6mmol hexa, 5mmol ammonium fluoride is added
80ml distilled water is placed in 100ml beaker, is put into ultrasound 5 minutes in Ultrasound Instrument, keeps it mixed with magnetic stirrer 30 minutes
It closes uniform.Above-mentioned solution is poured into the reaction kettle of 100ml polytetrafluoroethylsubstrate substrate, seals, be 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 are to get ferrous acid nano nickel particles.Gained iron
Sour nano nickel particles and acetylene black, polytetrafluoroethylene (PTFE) are uniformly mixed in certain mass ratio 8:1:1, obtain a kind of sticky silt
Slurry, then whole slurry are applied to nickel foam on piece, it is finally cooled to room temperature within dry 3 hours at 150 degree, obtains nickel ferrite based magnetic loaded nanometer
Mosaic electrode material.Each diffraction maximum position and relative intensity match with the JPCDS card (10-0325) of nickel ferrite based magnetic loaded in Fig. 1,
Show that product is face-centered cubic spinel-type ferrous acid nickel.Ferrous acid nano nickel particles have successfully been prepared as can be seen from Figure 2.From it
The average grain diameter of the ferrous acid nano nickel particles prepared known to grain size distribution (Fig. 3) is 47 nanometers.Fig. 4 shows nickel ferrite based magnetic loaded nanometer
Grain is used as electrode material for super capacitor, and after 1500 cycle charge-discharges, capacitance still keeps 80.3% or more.
Embodiment 2
The powder of the ferric nitrate of 2mmol, 1mmol nickel acetate, 10mmol hexa, 5mmol ammonium fluoride is added
80ml distilled water is placed in 100ml beaker, is put into ultrasound 5 minutes in Ultrasound Instrument, keeps it mixed with magnetic stirrer 30 minutes
It closes uniform.Above-mentioned solution is poured into the reaction kettle of 100 milliliters of polytetrafluoroethylsubstrate substrates, seal, be placed in baking oven, controls baking oven
Temperature be 180 DEG C, react 12 hours, be cooled to room temperature, repeatedly washing, be dried in vacuo to get ferrous acid nano nickel particles.Gained
Ferrous acid nano nickel particles and acetylene black, polytetrafluoroethylene (PTFE) are uniformly mixed in certain mass ratio 7:2:1, obtain a kind of sticky silt
Slurry, then whole slurry are applied to nickel foam on piece, it is finally cooled to room temperature within dry 5 hours at 130 degree, obtains nickel ferrite based magnetic loaded nanometer
Mosaic electrode material.
Embodiment 3
The powder of the nickel chloride of 2mmol, 2mmol ferric nitrate, 3mmol hexa, 10mmol ammonium fluoride is added
80ml distilled water is placed in 100ml beaker, is put into ultrasound 5 minutes in Ultrasound Instrument, keeps it mixed with magnetic stirrer 30 minutes
It closes uniform.Above-mentioned solution is poured into the reaction kettle of 100ml polytetrafluoroethylsubstrate substrate, seals, be placed in baking oven, control baking oven
Temperature is 160 DEG C, reacts 6 hours, is cooled to room temperature, and repeatedly washs, is dried in vacuo to get ferrous acid nano nickel particles are arrived.Gained
Ferrous acid nano nickel particles and acetylene black, polytetrafluoroethylene (PTFE) are uniformly mixed in certain mass ratio 8:1:1, obtain a kind of sticky silt
Slurry, then whole slurry are applied to nickel foam on piece, it is finally cooled to room temperature within dry 6 hours at 100 degree, obtains nickel ferrite based magnetic loaded nanometer
Mosaic electrode material.
Embodiment 4
By the ferric acetate of 0.2mmol, 0.2mmol nickel nitrate, 10mmol hexa, 2mmol ammonium fluoride powder
40ml distilled water is added, is placed in 50ml beaker, is put into ultrasound 5 minutes in Ultrasound Instrument, was made with magnetic stirrer 30 minutes
It is uniformly mixed.Above-mentioned solution is poured into the reaction kettle of 50ml polytetrafluoroethylsubstrate substrate, seal, be placed in baking oven, control is dried
The temperature of case is 140 DEG C, reacts 20 hours, is cooled to room temperature, and repeatedly washing, vacuum drying are to get 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, keeps the temperature 2 hours, obtains nickel ferrite based magnetic loaded classification knot
Structure nano particle.Gained nickel ferrite based magnetic loaded and acetylene black, polytetrafluoroethylene (PTFE) are uniformly mixed in certain mass ratio 8:1:1, obtain one
The sticky slurry of kind, then whole slurry are smeared into above-mentioned ready nickel foam on piece, finally in 150 degree of dry coolings in 6 hours
To room temperature, nickel ferrite based magnetic loaded nanoparticle electrode material is obtained.
Description to examples detailed above is for that can understand and apply the invention convenient for those skilled in the art.It is ripe
The personnel for knowing art technology obviously easily can make various modifications to these examples, and General Principle described herein
It is applied in other examples without having to go through creative labor.Therefore, the present invention is not limited to example here, art technologies
Personnel's announcement according to the present invention, the improvement made for the present invention and modification all should be within protection scope of the present invention.
Claims (7)
1. a kind of preparation method of nickel ferrite based magnetic loaded nanoparticle electrode material, in the nickel ferrite based magnetic loaded nanoparticle electrode material, ferrous acid
The pattern of nano nickel particles is irregular spheric granules, average grain diameter 47nm；The ferrous acid nano nickel particles are used for super
Capacitor electrode material, after 1500 cycle charge-discharges, capacitance still keeps 80.3% or more；It is characterized 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 uses magnetic stirrer
It is uniformly mixed it, obtains precursor solution, for use；
The preparation of step 2, nickel ferrite based magnetic loaded nanoparticle electrode material:
The precursor solution of step 1 is poured into the reaction kettle of polytetrafluoroethylsubstrate substrate, seals, is placed in baking oven, controls baking oven
Temperature be 140~200 DEG C between carry out hydro-thermal reaction, be cooled to room temperature, wash, be dried in vacuo to get nickel ferrite based magnetic loaded nanometer
Grain electrode material.
2. a kind of preparation method of nickel ferrite based magnetic loaded nanoparticle electrode material as described in claim 1, which is characterized in that step 1
In, the nickel salt, molysite, hexa, ammonium fluoride molar ratio be 0.2~2:0.2~2:3~10:2~10, institute
Stating concentration of the nickel salt in distilled water is 5~25mmol/L.
3. a kind of preparation method of nickel ferrite based magnetic loaded nanoparticle electrode material as claimed in claim 1 or 2, which is characterized in that institute
The nickel salt stated is any in nickel chloride, nickel nitrate and nickel acetate.
4. a kind of preparation method of nickel ferrite based magnetic loaded nanoparticle electrode material as claimed in claim 1 or 2, which is characterized in that institute
The molysite stated is any in iron chloride, ferric nitrate and ferric acetate.
5. a kind of preparation method of nickel ferrite based magnetic loaded nanoparticle electrode material as described in claim 1, which is characterized in that step 2
In, the hydrothermal temperature is 140~200 DEG C, and the time is 6~20 hours.
6. material made from a kind of preparation method of nickel ferrite based magnetic loaded nanoparticle electrode material as described in claim 1 is used as preparation
The purposes of super capacitor material, which is characterized in that preparation step is as follows: by nickel ferrite based magnetic loaded nanoparticle electrode material and acetylene
Black, polytetrafluoroethylene (PTFE) uniformly mixes in mass ratio, obtains sticky slurry, then whole slurry are applied to ready nickel foam
On piece is finally dried, and electrode material for super capacitor is obtained.
7. a kind of nickel ferrite based magnetic loaded nanoparticle electrode material as claimed in claim 6 is used as the use for preparing super capacitor material
On the way, which is characterized in that the nickel ferrite based magnetic loaded, acetylene black, polytetrafluoroethylene (PTFE) mass ratio are 7~8:1~2:1, the drying
Temperature is 60~150 degree, and drying time is 3~6 hours.
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| CN107452952B (en) * | 2017-08-16 | 2019-10-08 | 华南师范大学 | A kind of composite material and preparation method and application of nickel ferrite based magnetic loaded and silicon |
| 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 |
| 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 |
| CN107761128B (en) * | 2017-11-10 | 2019-12-03 | 上海应用技术大学 | A kind of FeNiNC electrode material, preparation method and applications |
| CN110040789B (en) * | 2019-04-17 | 2021-11-02 | 天津大学 | Preparation method of nickel ferrite microsphere supercapacitor electrode material |
| CN113249743B (en) * | 2021-05-18 | 2022-12-16 | 上海大学 | Catalyst for electrocatalytic oxidation of glycerol and preparation method thereof |
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