CN106206082B - The preparation method and application of nickel oxide/graphene combination electrode with electrochemical capacitance energy storage characteristic - Google Patents
The preparation method and application of nickel oxide/graphene combination electrode with electrochemical capacitance energy storage characteristic Download PDFInfo
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Abstract
The invention discloses the preparation method and applications of nickel oxide/graphene combination electrode with electrochemical capacitance energy storage characteristic, nickel oxide and graphene composite material modified electrode are prepared for by substrate substep electrodeposition process of nickel foam, morphology characterization is carried out to nickel oxide/graphene composite material by scanning electron microscope, as a result show that graphene film is tightly attached to foam nickel surface, nickel oxide nano piece uniform load is on graphene film.The capacitive property of the combination electrode is tested by electrochemical method, the result shows that the chemical property of nickel oxide/graphene combination electrode is greatly improved compared with graphene modified electrode, charge-discharge test shows nickel oxide/graphene combination electrode in 1 mA/cm2Specific capacitance under current density is 381 mF/cm2, it is a kind of good super capacitor material to illustrate nickel oxide/graphene composite material.
Description
Technical field
The present invention relates to a kind of preparation of ultracapacitor combination electrode and its tests of capacitive property.
Background technology
With the exhaustion of traditional energy and the appearance of environmental degradation problem, about cleaning, efficient, novel, regenerative resource
The research of material and device is constantly subjected to the extensive attention of researcher with application.It is easily transmitted and utilizes since electric energy has
The characteristics of, far superior to other various forms of energy, so electric energy how to be made full use of just to become extremely important.In this background
Under all kinds of electrochmical power sources come into being, such as fuel cell, lithium ion battery and ultracapacitor.Compared with ordinary capacitor
The energy density higher of ultracapacitor, compared with lithium battery, the power density higher of ultracapacitor, ultracapacitor in addition
Also have many advantages, such as that good cycling stability, charge/discharge rates are fast, specific capacitance is big, environmental pollution is small, therefore ultracapacitor
Have wide practical use in multiple fields such as new-energy automobile, solar power system, military equipments.
Ultracapacitor can be divided into according to the difference of energy storage mechnism by double electric layers supercapacitor and the super electricity of fake capacitance
Container.Double layer capacitor is grown up based on the double electrode layer theory of Helmholtz, is had compared with ordinary capacitor
Even closer charge layer can provide higher capacitance.The electrode material of fake capacitance ultracapacitor is usually to have greatly
The redox reaction of Rapid reversible occurs in the electrolytic solution for the electroactive material of specific surface area, these materials, so as in electrode
Complete the storage of a large amount of charges and release process in surface.
Electrode material be influence ultracapacitor capacitive character can principal element, develop the electrode material of high-capacitance for
Key effect can be had by improving ultracapacitor capacitive character.Transition metal oxide is a kind of energy storage material being concerned,
Energy density is higher than the energy density of double layer capacitor.That studies earliest has metal oxide containing precious metals such as ruthenium-oxide, yttrium oxide etc.,
Splendid fake capacitance performance is shown, but its is expensive, limits practical application.Base metal oxide also has preferable electricity
Capacitive energy common are manganese oxide, nickel oxide, cobalt oxide etc..Wherein nickel have derive from a wealth of sources, be cheap, it is easy preparation and
The advantages that theoretical specific capacitance is high, is a kind of ideal fake capacitance material.
Graphene has the characteristics that high conductivity, good mechanical property and bigger serface, can not only surpass as electric double layer
The grade ideal electrode material of capacitor and the preferable base material of fake capacitance ultracapacitor.Graphene is super in fake capacitance
The reason of composite material capacitive property can be improved in capacitor application, has:（1）Graphene makees load matrix in the composite
When, the fake capacitance active material of nanoscale can be distributed in graphene surface with stable and uniform, substantially increase active matter
The electro-chemical activity and utilization rate of matter;（2）Graphene can play the role of electron channel, pass through graphene and fake capacitance activity
Good contact between substance, can occur quick electron-transport in the composite；（3）Unique planar structure of graphene
Help to limit STRUCTURE DECOMPOSITION of the fake capacitance active material during ion insertion/disengaging, so as to improve composite material
Stability.
The advantages of present invention can improve electrode specific surface area using nickel foam porous structure, using it as combination electrode
Collector obtains grapheme material on its surface, then be modified with graphene material by electrochemical process by potentiostatic electrodeposition method
The collection liquid surface electro-deposition of material obtains nickel oxide nano piece, successfully prepares nickel oxide/graphene combination electrode, passes through scanning
Electronic Speculum characterizes its microscopic appearance, and electrochemically its capacitive property is tested.
Invention content
The purpose of the present invention is announce the preparation method of nickel oxide/graphene combination electrode with electrochemical capacitance energy storage characteristic
And application process, specific method are：Have using potentiostatic method in the synthesis of foamed nickel current collector granule surface contral and live compared with high electrochemical
The graphene film of property, further electrochemical deposition prepare the excellent nickel oxide/graphene combination electrode of capacitive property.By sweeping
The shape characteristic of the prepared combination electrode of Electronic Speculum evaluation is retouched, a layer graphene has uniformly been coated in foamed nickel current collector and has been in
Reveal the NiO nanometer sheets being evenly distributed.Three-electrode system is built by working electrode of the combination electrode, passes through cyclic voltammetric
Method, AC impedence method and constant current charge-discharge method test the capacitive property of the combination electrode.The result shows that the combination electrode
Under high current density there is very high energy density and excellent high rate performance, equally shown in cycle charge discharge electrical testing
Splendid cyclical stability illustrates that nickel oxide/graphene combination electrode has potential application value in ultracapacitor field.
Nickel oxide/graphene combination electrode is by foamed nickel current collector（Basal layer）, graphene（Middle layer）With NiO nanometer sheets
（Outer layer）It forms.
The graphene forms ultra-thin close clad on foamed nickel current collector surface.
The NiO nanometer sheets homoepitaxial can effectively improve the specific surface area of combination electrode in graphene surface.
A kind of method for preparing nickel oxide/graphene combination electrode, using foamed nickel current collector as basal layer, utilizes constant potential
Sedimentation obtains graphene interlayers, then powered in graphene interlayers with two step cyclic voltammetries in substrate surface electro-deposition
Deposition obtains NiO nanometer sheet outer layers, and specific preparation process is as follows：
1) nickel foam is cut into the square of certain size, it is clear with acetone, certain density hydrochloric acid solution ultrasound successively
It washes certain time and number, is cleaned later with distilled water, then with ethanol rinse, finally dried up with nitrogen spare；
2) a certain amount of graphene oxide of ultrasonic disperse obtains uniform suspension in the PBS buffer solution of certain pH, removes
Using above-mentioned suspension as electrolyte after oxygen, foamed nickel current collector（NF）For working electrode, three-electrode system is built, in nickel foam collection
Flow surface deposits to obtain graphene using potentiostatic method, and taking-up obtains GR/NF after being cleaned with distilled water, be dried in vacuo standby
With；
3) certain density nickel nitrate solution is configured with the acetate buffer solution of certain pH dissolving nickel nitrate, with above-mentioned nitric acid
Nickel solution is electrolyte, is worked electrode with GR/NF electrodes, builds three-electrode system.Using two step cyclic voltammetries in GR/NF
The NiO nanometer sheets that electrode surface electro-deposition is evenly distributed with distilled water clean to obtain nickel oxide/graphene compound after taking-up
Electrode is denoted as NiO/GR/NF, spare after vacuum drying；
4) using KOH as electrolyte, NF, GR/NF, the NiO/GR/NF prepared respectively using step 1, step 2 and step 3 is work
Make electrode, build three-electrode system, the capacitance of above-mentioned working electrode is tested by cyclic voltammetry and constant current charge-discharge method
Performance.
The size of square nickel foam stated in step 1 is the cm of 1 cm × 1；The nickel foam hole stated in step 1
Gap rate is more than 90%；The nickel foam pore diameter range stated in step 1 is the mm of 1 mm ~ 10；The hydrochloric acid solution stated in step 1
A concentration of 3.0 mol/L；It is 3 times that each solution stated in step 1, which is cleaned by ultrasonic number, the time being cleaned by ultrasonic every time
For 10 min.
The pH of PBS buffer solutions stated in step 2 is 8.0；The graphene oxide stated in step 2 it is a concentration of
1.0 mg/mL；The deoxidation method stated in step 2 is to be passed through a certain amount of nitrogen；Three electricity of the structure stated in step 2
Electrode systems include：Working electrode（Foamed nickel current collector）, reference electrode（Saturated calomel electrode）, auxiliary electrode（Platinum plate electrode）；
The condition that the potentiostatic electrodeposition method stated in step 2 prepares graphene is：Sedimentation potential be -1.2 V, sedimentation time 600
s；The distilled water stated in step 2 is redistilled water.
The pH for the acetate buffer solution stated in step 3 is 4.0；The nickel nitrate solution stated in step 3 it is a concentration of
1.0 mmol/L；The three-electrode system stated in step 3 is working electrode（GR/NF）, reference electrode（Saturated calomel electrode）、
Auxiliary electrode（Platinum plate electrode）；The first step cyclic voltammetry sedimentary condition stated in step 3：Using above-mentioned nickelous nitrate solution as
Electrolyte, potential window are the V of -1.0 V~0.5, and sweep speed is 70 mV/s, and the scanning number of turns is 30 circles；It is stated in step 3
Second step cyclic voltammetry sedimentary condition：To complete the electrode of first step cyclic voltammetry deposition reaction as working electrode, with
The PBS solution of pH 7 is electrolyte, and potential window is the V of -1 V~1.5, and sweep speed is 100 mV/s, and the scanning number of turns is 30
Circle.
A concentration of 1.0 mol/L for the KOH solution stated in step 4；Reference in the three-electrode system that step 4 is stated
Electrode is mercury/mercuric oxide electrode, auxiliary electrode is platinum plate electrode；The potential range for the cyclic voltammetry stated in step 4
For 0~0.8 V, 5,10,20,30,50,80,100,150 mV/s of sweep speed；The perseverance electricity stated in step 4
The potential range for flowing charge-discharge test is 0~0.5 V, 1,2,3,5,10,20,40 mA/cm of current density2。
The beneficial effects of the invention are as follows：The present invention proposes one kind and simply prepares nickel oxide/graphene combination electrode and survey
The method for trying the combination electrode capacitive property.Using potentiostatic electrodeposition method in the synthesis of foamed nickel current collector granule surface contral with higher
The graphene film of electro-chemical activity, further electrochemistry formated have the NiO nanometer sheets of outstanding capacitive property, structure oxidation
Nickel/graphene combination electrode.Electrochemical method prepares the method for graphene and NiO nanometer sheets with simple and convenient, quick and green
The free of contamination feature of color.Nickel oxide/graphene combination electrode prepared by the present invention can give full play to reticulated foam nickel specific surface
The characteristics of big is accumulated, express passway can be provided for electron-transport after the close coated graphite alkene of collection liquid surface, be conducive to electronics
Absorption and desorption process.The shortcomings that combination electrode can effectively overcome NiO internal resistances larger, gives full play to NiO nanometer sheets
Fake capacitance amount enhances the capacitive property of combination electrode.Result of the test shows that nickel oxide/graphene combination electrode has good follow
Ring stability and higher energy density can have potential application value as the working electrode of ultracapacitor.
Description of the drawings
Fig. 1：(A) nickel foam（NF）, (B) graphene/nickel foam（GR/NF）, (C) nickel oxide/graphene/nickel foam
（NiO/GR/NF）The scanning electron microscope (SEM) photograph of combination electrode（Illustration is partial enlarged view）.
Fig. 2：Different operating electrode（a→c：NF, GR/NF, NiO/GR/NF）Cyclic voltammetry curve, illustration is that NF is followed
Ring volt-ampere curve enlarged drawing, electrolyte are 1.0 mol/L KOH, and 100 mV/s of sweep speed, potential window is 0~0.8V.
Fig. 3：The not synsedimentary number of turns（a→e：5,10,40,20,30）Under obtained nickel oxide/graphene/nickel foam it is compound
Electrode, in 1.0 mol/L KOH solutions, sweep speed is the cyclic voltammetry curve (A) of 100 mV/s；10 mA/cm2Electricity
Charging and discharging curve (B) under current density and not the specific capacitance change curve (C) under the synsedimentary number of turns.
Fig. 4：Nickel oxide/graphene/nickel foam combination electrode in 1.0 mol/L KOH solutions different scanning speed (a →
h:5,10,20,30,50,80,100,150 mV/s) under cyclic voltammetry curve.
Fig. 5：Nickel oxide/graphene/nickel foam combination electrode is in different current density (a → g：1,2,3,5,10,20,40
mA/cm2) under discharge curve (A) and specific capacitance change curve (B).
Fig. 6：Nickel oxide/graphene/nickel foam combination electrode is 10 mA/cm in current density2Under conditions of follow for 1000 times
Ring charge and discharge specific capacitance change curve, illustration are part cycle charge-discharge curve.
Specific embodiment
Below in conjunction with Figure of description and specific preferred embodiment, the invention will be further described, but not therefore and
It limits the scope of the invention.
Material and instrument employed in following embodiment are commercially available.
Embodiment 1
Foamed nickel current collector pre-processes：Nickel foam is cut into the square of the cm of 1 cm × 1, is then sequentially placed into acetone
With ultrasound 3 times respectively in the hydrochloric acid of 3.0 mol/L, 10 min, is drenched after thoroughly being washed with redistilled water with absolute ethyl alcohol every time
It washes, is finally saved backup with nitrogen drying vacuum, the morphology characterization of foamed nickel current collector is shown in Fig. 1 (A).
Embodiment 2
25 mL of PBS buffer solution of pH 8.0 is configured, then adds in 25.0 mg graphene oxides, after ultrasonic disperse is uniform
To 1.0 stable mg/mL graphene oxide suspensions, using it as electrolyte, foamed nickel current collector is working electrode, and saturation is sweet
Mercury electrode is reference electrode, and platinum plate electrode builds three-electrode system for auxiliary electrode, in -1.2 V of sedimentation potential and sedimentation time
Under conditions of 600 s, obtain on foamed nickel current collector surface coating close graphene film by potentiostatic electrodeposition method, prepare
Graphene modified electrode be denoted as GR/NF, morphology characterization is shown in Fig. 1 (B).
Embodiment 3
The nickel nitrate solution of 1.0 mmol/L is configured with the acetate buffer solution of pH 4.0, using it as electrolyte, is with GR/NF
Working electrode, saturated calomel electrode are reference electrode, and platinum plate electrode builds three-electrode system for auxiliary electrode.Pass through cyclic voltammetric
Method completes first step electrodeposition process, sedimentary condition：The V of potential window ranging from -1.0 V~0.5, sweep speed are 70 mV/
S, the scanning number of turns are 30 circles.Second step process is completed by cyclic voltammetry, experiment condition is：To complete first step cyclic voltammetric
The electrode of method is working electrode, and saturated calomel electrode does reference electrode, and platinum plate electrode does auxiliary electrode structure three-electrode system, with
The PBS solution of pH 7.0 is electrolyte, and potential window is the V of -1.0 V~1.5, and sweep speed is 100 mV/s and the scanning number of turns
For 30 circles.The NiO nanometer sheets being evenly distributed by two step cyclic voltammetries in the electro-deposition of GR/NF surfaces, with steaming after taking-up
Distilled water cleans to obtain nickel oxide/graphene/nickel foam combination electrode, and morphology characterization is shown in Fig. 1 (C), is denoted as NiO/GR/NF, very
It is spare after sky is dry.
Embodiment 4
Using 1.0 mol/L KOH as electrolyte, respectively with NF, GR/NF and NiO/GR/NF for working electrode, mercury/mercury oxide
Electrode is reference electrode, and platinized platinum builds three-electrode system for auxiliary electrode, sets potential window as 0~0.8 V, sweep speed is
0.1 V/s, the capacitive property of above-mentioned working electrode is tested by cyclic voltammetry, and result of the test is shown in Fig. 2.
Embodiment 5
The scanning number of turns in first step cyclic voltammetric electrodeposition process is only adjusted to 5,10 on the basis of embodiment 3,
20,30,40 circles, remaining condition is identical to prepare corresponding modified electrode.It is different using 1.0 mol/L KOH as electrolyte
Nickel oxide/graphene/nickel foam the combination electrode prepared under sedimentary condition is working electrode, and mercury/mercuric oxide electrode is reference electricity
Pole, platinized platinum build three-electrode system for auxiliary electrode, and potential window is 0~0.8 V, and sweep speed passes through cycle for 100 mV/s
Voltammetry is tested the capacitive property of above-mentioned working electrode and is compared, and result of the test is shown in Fig. 3 (A)；Potential range 0~0.5
V, current density are 10 mA/cm2Under conditions of pass through compound electric under different sedimentary conditions described in constant current charge-discharge CURVE STUDY
The variation of electrode capacitance performance, result of the test are shown in Fig. 3 (B).
Embodiment 6
Using 1.0 mol/L KOH as electrolyte, NiO/GR/NF is working electrode, and mercury/mercuric oxide electrode is reference electrode,
Platinum plate electrode builds three-electrode system for auxiliary electrode, and potential window is 0~0.8 V, changes sweep speed and is followed successively by 5,10,
20,30,50,80,100,150 mV/s record cyclic voltammetry curve, see Fig. 4, and then study sweep speed to specific capacitance
The influence of variation,.
Embodiment 7
Using 1.0 mol/L KOH as electrolyte, NiO/GR/NF is working electrode, and mercury/mercuric oxide electrode is reference electrode,
Platinum plate electrode builds three-electrode system for auxiliary electrode, and potential window is 0~0.5 V, and current density is respectively 1,2,3,5,
10, 20, 40 mA/cm2Under conditions of by constant current charge-discharge CURVE STUDY difference current density to the combination electrode electricity
The influence of capacitive energy, result of the test are shown in Fig. 5 (A) and (B).
Embodiment 8
Using 1.0 mol/L KOH as electrolyte, NiO/GR/NF is working electrode, and mercury/mercuric oxide electrode is reference electrode,
Platinum plate electrode builds three-electrode system for auxiliary electrode, and potential window is 0~0.5 V, current density 10mA/cm2Under conditions of
1000 cycle charge discharge electrical testings are carried out, test result is shown in Fig. 6.
The present invention foamed nickel current collector is pre-processed first, recycle electrochemical method prepare nickel oxide/graphene/
Nickel foam combination electrode, scanning electron microscope show that graphene is closely coated with nickel foam and forms three-dimensional netted macroscopic body, and surface is equal
Even distribution NiO nanometer sheets.Compare the capacitive property of NF, GR/NF and NiO/GR/NF respectively again, the results showed that the electricity of NiO/GR/NF
Capacitive preferably, and can carry out electro-chemical test to nickel oxide/graphene/nickel foam combination electrode, as a result show nickel oxide/graphite
Alkene/nickel foam combination electrode has good capacitive property as the working electrode of ultracapacitor.
Claims (2)
1. a kind of preparation method of nickel oxide/graphene combination electrode with electrochemical capacitance energy storage characteristic, it is characterised in that including
Following steps：
(1) pretreatment of foamed nickel current collector NF：Nickel foam is cut into the square of certain size, is sequentially placed into acetone and salt
It ultrasonic certain time in acid, is thoroughly dried up after washing with nitrogen；
(2) PBS buffer solution of certain pH is configured, adds in a certain amount of graphene oxide, ultrasonic disperse uniformly obtains stable uniform
Graphene oxide suspension, using the suspension as electrolyte, pretreated foamed nickel current collector be working electrode, structure three
Electrode system obtains reduced graphene on foamed nickel current collector surface by potentiostatic method, builds graphene modified electrode；
(3) certain density Ni (NO are configured in the acetum of pH 4.03)2Solution, using it as electrolyte, graphene modified
Electrode is working electrode, three-electrode system is built, by cyclic voltammetry in graphene modified electrode surface electro-deposition obtains
Then electrolyte is changed to the PBS solution of pH 7 by mesosome, reset cyclic voltammetry sedimentary condition and obtained in electrode surface
Nickel oxide nano piece, taking-up can obtain nickel oxide/graphene combination electrode after drying；
(4) using KOH solution as electrolyte, using nickel oxide/graphene combination electrode as working electrode, three-electrode system is built, is ground
Study carefully the cyclic voltammetry under different scanning speed, constant current charge-discharge test under different current densities and in high current density
Under constant current cycle charge discharge electrical testing；
The square of certain size described in step (1) is 1cm × 1cm；The concentration of hydrochloric acid is 1.0mol/L~6.0mol/
L；The nickel foam, porosity are more than 90%, and pore diameter range is 1mm~10mm；
The pH ranging from 8.0 of PBS buffer solution described in step (2)；The graphene oxide suspension it is a concentration of
1.0mg/mL；The potentiostatic method, sedimentary condition are：The variation range of sedimentation potential is -1.2V, and sedimentation time is
600s；The three-electrode system including working electrode is foamed nickel current collector, reference electrode is saturated calomel electrode and auxiliary
Electrode is platinum plate electrode；
Ni (NO described in step (3)3)2A concentration of 1.0mmol/L of solution；The three-electrode system includes working electrode
For graphene modified electrode, reference electrode be saturated calomel electrode and auxiliary electrode is platinum plate electrode；Obtain the cycle of intermediate
The sedimentary condition of voltammetry is that potential window is -1.0V~0.5V, sweep speed 70mV/s, and the scanning number of turns is 30 circles；It obtains
The sedimentary condition of the cyclic voltammetry of nickel oxide nano piece is potential window for -1.0V~1.5V, sweep speed 100mV/s,
The number of turns is scanned as 30 circles.
2. preparation method described in claim 1, it is characterised in that a concentration of 1.0mol/ of the KOH solution described in step (4)
L；The three-electrode system is：Using nickel oxide/graphene combination electrode as working electrode, mercury/mercuric oxide electrode is reference electricity
Pole, platinum plate electrode are auxiliary electrode；The potential range of the cyclic voltammetry is 0~0.8V；The different scanning speed
It spends for 5,10,20,30,50,80,100,150mV/s；The potential range of the constant current charge-discharge test is 0~0.5V；Institute
The different current densities stated are 1,2,3,5,10,20,40mA/cm2。
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| CN107967997A (en) * | 2017-11-28 | 2018-04-27 | 中国科学院深圳先进技术研究院 | A kind of three-dimensional high heat-conductivity conducting composite material, its preparation method and application |
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| CN111540914B (en) * | 2020-05-11 | 2022-06-14 | 辽宁大学 | Preparation method of functional porous graphene integrated electrode material and application of functional porous graphene integrated electrode material in vanadium battery |
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