CN107610943A - A kind of preparation method of iron molybdate graphene composite structure electrode material for super capacitor - Google Patents
A kind of preparation method of iron molybdate graphene composite structure electrode material for super capacitor Download PDFInfo
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- CN107610943A CN107610943A CN201710676759.5A CN201710676759A CN107610943A CN 107610943 A CN107610943 A CN 107610943A CN 201710676759 A CN201710676759 A CN 201710676759A CN 107610943 A CN107610943 A CN 107610943A
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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 discloses a kind of preparation method of iron molybdate graphene composite structure electrode material for super capacitor, this method comprises the following steps：（1）Using native graphite as raw material, graphite oxide is obtained with Hummers legal systems are improved；（2）By step（1）Obtained graphite oxide ultrasonic dissolution forms uniform graphite oxide dispersion in distilled water；Sodium molybdate and anhydrous ferric chloride are then added, dissolving is sufficiently stirred, obtains dispersion liquid；（3）By step（2）Resulting dispersion liquid is transferred in reactor, heating response 12 hours, then natural cooling；（4）By step（3）Obtained product is repeatedly washed with distilled water and absolute ethyl alcohol, is then dried, that is, obtains iron molybdate graphene composite structure electrode material for super capacitor.Preparation method of the present invention preferably resolves nano material agglomeration traits in ordinary graphite alkene preparation process, and obtains the sandwich of the graphene parcel iron molybdate of excellent performance.
Description
Technical field
The present invention relates to nano composite material preparation field, especially a kind of iron molybdate graphene composite structure super capacitor
The preparation method of device electrode material.
Background technology
Because global energy in the near future can be inevitably exhausted and will exhaust, in current energy resource consumption speed
Under, one of key challenge of new century is undoubtedly energy storage and conversion.From traditional fossil fuel such as solar energy, wind energy, water power
The replacement of regenerative resource is waited until with bio-fuel.However, these traditional intermittent energy sources are influenceed by natural conditions very much, such as
Weather and geographical position etc. etc., therefore, solve future source of energy crisis active demand promoted high performance energy conversion and
The development of storage device.Super capacitor, also known as electrochemical capacitor, it, which has filled up traditional sucrose capacitor, (has high power close
Degree) gap battery (there is high-energy-density) between, due to their high power density, fast charging and discharging process and grow all
In life-span phase, just causing the extensive concern of people at present.
Traditional super capacitance electrode material is carbon material, and the main energy storage mode of carbon material is electric double layer energy storage, due to
The particle diameter of carbon material is uneven, causes its capacitance relatively low.Traditional fake capacitance material is mainly transition group metallic oxide, together
When, because iron molybdate has multivalent state, there can be more preferable fake capacitance performance than single transition group metallic oxide.Meanwhile
Because graphene has abundant functional group and many excellent chemical properties.
Therefore, it is necessary to design a kind of preparation method of iron molybdate graphene composite structure electrode material for super capacitor.
The content of the invention
For the defects of existing technology, there is provided a kind of iron molybdate graphene composite structure electrode material for super capacitor
Preparation method.
The present invention is realized by following proposal：
A kind of preparation method of iron molybdate graphene composite structure electrode material for super capacitor, this method comprise the following steps：
（1）Using native graphite as raw material, graphite oxide is obtained with Hummers legal systems are improved；
（2）By step（1）Obtained graphite oxide ultrasonic dissolution forms uniform graphite oxide dispersion in distilled water；With
Sodium molybdate and anhydrous ferric chloride are added afterwards, are sufficiently stirred dissolving, are obtained dispersion liquid；
（3）By step（2）Resulting dispersion liquid is transferred in reactor, heating response 12 hours, then natural cooling；
（4）By step（3）Obtained product is repeatedly washed with distilled water and absolute ethyl alcohol, is then dried, that is, obtains molybdic acid
Iron graphene composite structure electrode material for super capacitor.
The mass ratio of the graphite oxide and distilled water is 1:500-700.
The mass ratio of the graphite oxide and sodium molybdate is 1:20-30, the quality of the graphite oxide and anhydrous ferric chloride
Than for 1:10-20.
The reactor is ptfe autoclave.
In step（3）In be heated to 120-160 DEG C.
Beneficial effects of the present invention are：
1. a kind of preparation method of iron molybdate graphene composite structure electrode material for super capacitor of the present invention is in ordinary graphite alkene
Nano material agglomeration traits are preferably resolved in preparation process, and obtain the compound of the graphene parcel iron molybdate of excellent performance
Structural material.
2. a kind of preparation method of iron molybdate graphene composite structure electrode material for super capacitor of the present invention solves biography
The deficiency for technique of uniting, its manufacture craft is simple, easy to operate, and energy consumption is low, has good application prospect.
Brief description of the drawings
Fig. 1 is a kind of scanning electron microscopic picture of iron molybdate graphene composite structure electrode material for super capacitor of the present invention
（SEM）；
Fig. 2 is a kind of X diffraction spectrograms of iron molybdate graphene composite structure electrode material for super capacitor of the present invention（XRD）；
Fig. 3 is a kind of constant current charge-discharge curve map of iron molybdate graphene composite structure electrode material for super capacitor of the present invention；
Fig. 4 is a kind of cyclic voltammetric charging and discharging curve of iron molybdate graphene composite structure electrode material for super capacitor of the present invention
Figure；
Fig. 5 is a kind of iron molybdate graphene composite structure electrode material for super capacitor following in 1M KOH electrolyte of the present invention
Ring stability diagram.
Embodiment
The preferred embodiment of the invention is further illustrated below in conjunction with the accompanying drawings：
Embodiment 1
A kind of preparation method of iron molybdate graphene composite structure electrode material for super capacitor, this method comprise the following steps：
（1）Using native graphite as raw material, graphite oxide is obtained with Hummers legal systems are improved；
（2）By step（1）Obtained 0.1g graphite oxides ultrasonic dissolution forms uniform graphite oxide in 60ml distilled water
Dispersion liquid；2.42g sodium molybdates and 1.62g anhydrous ferric chlorides are then added, dissolving is sufficiently stirred, obtains dispersion liquid；
（3）By step（2）Resulting dispersion liquid is transferred in reactor, is heated to 120 DEG C and is reacted 12 hours, then naturally cold
But；Reactor is ptfe autoclave.
（4）By step（3）Obtained product is repeatedly washed with distilled water and absolute ethyl alcohol, is then dried, that is, is obtained
Iron molybdate graphene composite structure electrode material for super capacitor.
Embodiment 2
A kind of preparation method of iron molybdate graphene composite structure electrode material for super capacitor, this method comprise the following steps：
（1）Using native graphite as raw material, graphite oxide is obtained with Hummers legal systems are improved；
（2）By step（1）Obtained 0.1g graphite oxides ultrasonic dissolution forms uniform graphite oxide in 70ml distilled water
Dispersion liquid；2g sodium molybdates and 2g anhydrous ferric chlorides are then added, dissolving is sufficiently stirred, obtains dispersion liquid；
（3）By step（2）Resulting dispersion liquid is transferred in reactor, is heated to 140 DEG C and is reacted 12 hours, then naturally cold
But；Reactor is ptfe autoclave.
（4）By step（3）Obtained product is repeatedly washed with distilled water and absolute ethyl alcohol, is then dried, that is, is obtained
Iron molybdate graphene composite structure electrode material for super capacitor.
Embodiment 3
A kind of preparation method of iron molybdate graphene composite structure electrode material for super capacitor, this method comprise the following steps：
（1）Using native graphite as raw material, graphite oxide is obtained with Hummers legal systems are improved；
（2）By step（1）Obtained 0.1g graphite oxides ultrasonic dissolution forms uniform graphite oxide in 50ml distilled water
Dispersion liquid；3g sodium molybdates and 1g anhydrous ferric chlorides are then added, dissolving is sufficiently stirred, obtains dispersion liquid；
（3）By step（2）Resulting dispersion liquid is transferred in reactor, is heated to 160 DEG C and is reacted 12 hours, then naturally cold
But；Reactor is ptfe autoclave.
（4）By step（3）Obtained product is repeatedly washed with distilled water and absolute ethyl alcohol, is then dried, that is, is obtained
Iron molybdate graphene composite structure electrode material for super capacitor.
Graphite oxide is typically aoxidized by graphite and obtained through strong acid.Mainly there are three kinds of methods for preparing graphite oxide at present：
Brodie methods, Staudenmaier methods and Hummers methods.The preparation process of traditional Hummers methods it is ageing relatively preferable
And it is also relatively safer in preparation process, it is one kind the most frequently used at present.It uses the potassium permanganate and graphite powder in the concentrated sulfuric acid
After the oxidized reaction in end, obtain brown has derivative carboxylic acid group at edge and is mainly phenolic hydroxyl group and epoxide group in the plane
Graphite flake, it is graphene oxide that this graphene layers can be stirred vigorously stripping through ultrasound or high shear, and the shape in water
Into stable, sundown single-layer graphene oxide suspension.Because conjugate network is by serious functionalization, graphene oxide
Thin slice has the speciality of insulation.Partial reduction can be carried out through reduction treatment, obtains the graphene platelet of chemical modification.It is although last
Obtained graphite ene product or redox graphene all has the defects of more, causes its electric conductivity to be not so good as original graphite
Alkene, but the processing procedure that reduction is peeled off in this oxidation can effectively allow insoluble powdered graphite to become to process in water, carry
Approach for making redox graphene.And its easy processing procedure and its solution machinability, consider that the industry of volume production is made
Cheng Zhong, above-mentioned technique have turned into the technical process of the very attractive of manufacture graphene associated materials and component.
System and is changed to dense by improvement Hummers methods in the present invention particular by the dosage of increase potassium permanganate
H2SO4 and H3PO4 volume ratio is 7:2, traditional Hummers methods are improved, detailed experimental implementation process and step exist
This is repeated no more.
Below by various Physico-chemical tests results to the iron molybdate graphene composite structure super capacitor prepared by the present invention
Device electrode material is further elaborated.
1st, structural characterization
（1）Scanning electron microscope analysis（SEM）
Fig. 1 is the scanning electron microscopic picture of the material prepared by the present invention, it can be seen that being more successfully prepared in Fig. 1 right sides
The less graphene of the number of plies, while it has been worth the iron molybdate of multilayer chip, graphene is wrapped in the surface of molybdic acid iron layer.
（2）X diffraction spectrograms (XRD)
Fig. 2 is the X ray diffracting spectrum of the material prepared by the present invention, wherein the diffraction except observing iron molybdate and graphene
Outside peak, exist without other diffraction maximums, illustrate that target product has synthesized and no coupling product produces.
2nd, the chemical property of the material prepared by the present invention
Before electro-chemical test, sample preparation and related preparation are carried out to the material prepared by the present invention, seen below：
The preparation of electrode slice.The nickel screen of cutting certain size first, roomy about 1cm, the ultrasonic half an hour in absolute ethyl alcohol, then
Again ultrasonic half an hour in deionized water, dry in an oven, 24 ~ 48 hours, and weigh.Then second is added in agate mortar
Acetylene black, polyvinylidene fluoride, absolute ethyl alcohol, the present invention prepared by material, while the proportioning of its quality be 1：1：8, mill
It is even, a small amount of absolute ethyl alcohol is added dropwise and is conveniently more preferably equably mixed into slurry, smearing is compressed on nickel screen, and smear layer approximately forms
1cm2, dry 24 hours or so, finally weigh and prepare electro-chemical test.
The composition of three electrode test systems includes this experiment to be tested using three-electrode system, research object working electrode
(WE)；Reference electrode (RE)：Determine working electrode potential.Auxiliary electrode is sometimes referred to as to electrode (CE)：Conduct electric current.Three electrodes
System contains two loops, and a loop is made up of working electrode and reference electrode, for the electrochemical reaction of test job electrode
Process, another loop are made up of working electrode and auxiliary electrode, are played transmission and are electronically formed loop, are surveyed in the electrochemistry
Before examination, 1mol/L potassium hydroxide solution is first prepared with volumetric flask, and is soaked electrode slice half an hour with the solution, regulation is different
Parameter carries out cyclic voltammetric charge-discharge test, constant current charge-discharge test and alcohol sensor respectively.
Three electrode test systems are selected in the test of this Experimentation An electrochemical, and wherein electro-chemical test selects Shanghai Chen Hua instrument limited
Electrochemical analyser/work station of the CHI660D models of company's production, electrolyte select 1mol/L metabisulfite solution.
The constant current charge-discharge curve map of material prepared by Fig. 3 inventions, be shown in figure sweep speed for 50,
Under 100 mv/s test, with the increase of sweep speed, single electrode capacitance decays successively.With the increase of scanning voltage,
Specific capacitance reduces wherein 6mv/s specific capacitances and is up to 106.2g；
The cyclic voltammetric charging and discharging curve figure of material prepared by Fig. 4 present invention.Understand with the increase of current density, fill in figure
Discharge time accelerates, while its specific capacitance is gradually reduced, and wherein specific capacitance of the cathode/anode electric current in 0.03 A is up to
108 F/g。
Fig. 5 is cyclical stability figure of the material in 1M KOH electrolyte prepared by the present invention.Cycle charge-discharge 1000
After secondary, specific capacitance 100F/g, 7.4% is only lost, illustrate that this kind of composite has excellent cyclical stability.
Although more detailed elaboration is done to technical scheme and has been enumerated, it will be appreciated that for ability
For field technique personnel, modification is made to above-described embodiment or uses equivalent alternative solution, this is to those skilled in the art
It is it is clear that these modifications or improvements without departing from theon the basis of the spirit of the present invention, belong to the present invention for member
Claimed scope.
Claims (5)
- A kind of 1. preparation method of iron molybdate graphene composite structure electrode material for super capacitor, it is characterised in that this method Comprise the following steps：（1）Using native graphite as raw material, graphite oxide is obtained with Hummers legal systems are improved；（2）By step（1）Obtained graphite oxide ultrasonic dissolution forms uniform graphite oxide dispersion in distilled water；With Sodium molybdate and anhydrous ferric chloride are added afterwards, are sufficiently stirred dissolving, are obtained dispersion liquid；（3）By step（2）Resulting dispersion liquid is transferred in reactor, heating response 12 hours, then natural cooling；（4）By step（3）Obtained product is repeatedly washed with distilled water and absolute ethyl alcohol, is then dried, that is, obtains molybdic acid Iron graphene composite structure electrode material for super capacitor.
- A kind of 2. preparation side of iron molybdate graphene composite structure electrode material for super capacitor according to claim 1 Method, it is characterised in that：The mass ratio of the graphite oxide and distilled water is 1:500-700.
- A kind of 3. preparation side of iron molybdate graphene composite structure electrode material for super capacitor according to claim 1 Method, it is characterised in that：The mass ratio of the graphite oxide and sodium molybdate is 1:20-30, the graphite oxide and anhydrous ferric chloride Mass ratio be 1:10-20.
- A kind of 4. preparation side of iron molybdate graphene composite structure electrode material for super capacitor according to claim 1 Method, it is characterised in that：The reactor is ptfe autoclave.
- A kind of 5. preparation side of iron molybdate graphene composite structure electrode material for super capacitor according to claim 1 Method, it is characterised in that：In step（3）In be heated to 120-160 DEG C.
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN112875756A (en) * | 2021-02-19 | 2021-06-01 | 苏州科技大学 | Manganese molybdate nanoflower/graphene three-dimensional structure and high-specific-volume supercapacitor performance improvement method |
| CN115072791A (en) * | 2022-06-24 | 2022-09-20 | 陕西科技大学 | FeMoO 4 Superfine nano particle, preparation method and application |
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Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN112875756A (en) * | 2021-02-19 | 2021-06-01 | 苏州科技大学 | Manganese molybdate nanoflower/graphene three-dimensional structure and high-specific-volume supercapacitor performance improvement method |
| CN112875756B (en) * | 2021-02-19 | 2022-09-06 | 苏州科技大学 | Manganese molybdate nanoflower/graphene three-dimensional structure and high-specific-volume supercapacitor performance improvement method |
| CN115072791A (en) * | 2022-06-24 | 2022-09-20 | 陕西科技大学 | FeMoO 4 Superfine nano particle, preparation method and application |
| CN115072791B (en) * | 2022-06-24 | 2024-03-01 | 南京和知科技有限公司 | FeMoO 4 Superfine nano particle, preparation method and application |
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