CN107591255A - A kind of ultracapacitor graphene/CuFe2O4Composite nano materials and preparation method thereof - Google Patents

A kind of ultracapacitor graphene/CuFe2O4Composite nano materials and preparation method thereof Download PDF

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Publication number
CN107591255A
CN107591255A CN201710807096.6A CN201710807096A CN107591255A CN 107591255 A CN107591255 A CN 107591255A CN 201710807096 A CN201710807096 A CN 201710807096A CN 107591255 A CN107591255 A CN 107591255A
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cufe
graphene
nano materials
composite nano
10min
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刘海燕
吕乐福
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NANLING COUNTY PRODUCTION FORCE PROMOTION CENTER
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NANLING COUNTY PRODUCTION FORCE PROMOTION CENTER
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    • YGENERAL 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
    • Y02TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
    • Y02EREDUCTION OF GREENHOUSE GAS [GHG] EMISSIONS, RELATED TO ENERGY GENERATION, TRANSMISSION OR DISTRIBUTION
    • Y02E60/00Enabling technologies; Technologies with a potential or indirect contribution to GHG emissions mitigation
    • Y02E60/13Energy storage using capacitors

Abstract

The invention discloses a kind of ultracapacitor graphene/CuFe2O4Composite nano materials and preparation method thereof, the CuFe2O4For nanometer chip architecture, size about 100nm, size uniformity, and it is evenly distributed on flake graphite alkene.The invention also discloses above-mentioned graphene/CuFe2O4Composite nano materials and preparation method thereof, comprise the following steps:1)By Cu (CH3COO)2、Fe(CH3COO)2In molar ratio 1:2 proportionings, are dissolved in deionized water, form 1.5 mol/L mixed solution.2)By above-mentioned mixed solution and redox graphene(rGO)Suspension mixes, and forms new mixing suspension.3)LiOH solution is added in above-mentioned mixing suspension, adjusts to PH, is placed in afterwards in reactor, react 21h at 100 DEG C;Last thing is annealed at ambient pressure.Graphene/CuFe prepared by the present invention2O4Composite nano materials electrochemical performance, it is a kind of preferable electrode material for super capacitor.

Description

A kind of ultracapacitor graphene/CuFe2O4Composite nano materials and its preparation Method
Technical field
The present invention relates to electrode material for super capacitor field, especially graphene combination electrode material field.
Background technology
Ultracapacitor, it is a kind of novel energy-storing element between common electrostatic capacitor and secondary cell.Due to It has that specific power is high, specific capacity is big, cost is low, have extended cycle life, be memoryless, efficiency for charge-discharge is high, it is not necessary to safeguards and protects The advantages that supporting, therefore in mobile communication, information technology, electric automobile, Aero-Space and science and techniques of defence etc. with wide Application prospect.Countries in the world all give great attention, and are researched and developed as focus development project and strategic research.
Graphene is a kind of two-dimentional carbon nanomaterial, has excellent physical characteristic.Graphene can be applied and super electricity Container has been primarily due to following characteristics:Compared with traditional porous carbon materials, graphene(1)With very high electrical conductivity (104-106S/m)(2)Very big specific surface area(-2675m2/g).But also there is its shortcoming, apply on ultracapacitor, stone Black alkene interlayer is easily accumulated, and reduces specific surface area, while also counteracts that electrolyte enters electrode surface.
The composite of graphene and nano-oxide has some reports, the electrode material for ultracapacitor.Such as Graphene and CuO, Fe2O3、V2O5、NiO、Co3O4、Mn2O5Deng the composite of formation.But graphene is formed with multivariant oxide The also less report of composite nano materials.This patent proposes a kind of graphene and CuFe2O4The composite nano materials of formation, it is one The good electrode material for super capacitor of kind.
The content of the invention
It is contemplated that graphene and binary oxide are organically combined, a kind of new composite nano materials are formed, to Acquisition prepares the combination electrode material of premium properties ultracapacitor.
The present invention provides a kind of ultracapacitor graphene/CuFe2O4Composite nano materials and preparation method thereof, it is described CuFe2O4For nanometer chip architecture, size about 100nm, size uniformity, and it is evenly distributed on flake graphite alkene.
Present invention also offers a kind of above-mentioned ultracapacitor graphene/CuFe2O4Composite nano materials and its preparation side Method, comprise the following steps:
1)By Cu (CH3COO)2、Fe(CH3COO)2In molar ratio 1:2 proportionings, are dissolved in deionized water, form 1.5 mol/L's Mixed solution;
2)By above-mentioned mixed solution and redox graphene(rGO)Suspension mixes, volume ratio 1:3-1:6, wherein rGO hangs Supernatant liquid concentration is 1.5 mol/L, forms new mixing suspension;
3)2 mol/L LiOH solution is added in above-mentioned mixing suspension, it is 10.5 to adjust to PH, and ultrasonic vibration makes its uniform Afterwards, it is placed in reactor, reacts 21h at 100 DEG C, obtained sediment is cleaned repeatedly with deionized water and ethanol, is obtained just Walk product;
4)Above-mentioned primary product is carried out to alternating, step annealing at ambient pressure, annealing process is:Ar gas, 600 DEG C, 10min, N2 Gas, 800 DEG C, 10min, Ar gas, 1000 DEG C, 10min, N2Gas, 1200 DEG C, 10min, after annealing, obtain final product.
The useful achievement of the present invention is:
1)Graphene/CuFe prepared by the present invention2O4Composite nano materials, CuFe2O4For nanometer chip architecture, without other oxides Nano material occurs, and size is very uniform.
2)Graphene/CuFe prepared by the present invention2O4Composite nano materials pattern is homogeneous, is evenly distributed, and with graphene knot Close firmly, suitable for mass industrialized production.
3)Graphene/CuFe prepared by the present invention2O4Composite nano materials electrochemical performance, it is a kind of preferably super Level capacitor electrode material.
Brief description of the drawings
Fig. 1 is embodiment 1)Obtained graphene/CuFe2O4The transmission electron microscope of composite nano materials(TEM)Figure.
Fig. 2 is embodiment 1)Obtained graphene/CuFe2O4Cyclical stability when composite nano materials are as electrode is bent Line, test current density 3 A/g.
Embodiment
To further illustrate the present invention, illustrated in more detail with reference to specific embodiment and accompanying drawing.
Embodiment 1
1)By Cu (CH3COO)2、Fe(CH3COO)2In molar ratio 1:2 proportionings, are dissolved in deionized water, form 1.5 mol/L's Mixed solution;
2)By above-mentioned mixed solution and redox graphene(rGO)Suspension mixes, volume ratio 1:3, wherein rGO suspension Concentration is 1.5 mol/L, forms new mixing suspension;
3)2 mol/L LiOH solution is added in above-mentioned mixed solution, it is 10.5 to adjust to PH, and ultrasonic vibration makes its uniform Afterwards, it is placed in reactor, reacts 21h at 100 DEG C, obtained sediment is cleaned repeatedly with deionized water and ethanol, is obtained just Walk product;
4)Above-mentioned primary product is carried out to alternating, step annealing at ambient pressure, annealing process is:Ar gas, 600 DEG C, 10min, N2 Gas, 800 DEG C, 10min, Ar gas, 1000 DEG C, 10min, N2Gas, 1200 DEG C, 10min, after annealing, obtain final product stone Black alkene/CuFe2O4Composite nano materials.
Embodiment 2
1)By Cu (CH3COO)2、Fe(CH3COO)2In molar ratio 1:2 proportionings, are dissolved in deionized water, form 1.5 mol/L's Mixed solution;
2)By above-mentioned mixed solution and redox graphene(rGO)Suspension mixes, volume ratio 1:4, wherein rGO suspension Concentration is 1.5 mol/L, forms new mixing suspension;
3)2 mol/L LiOH solution is added in above-mentioned mixing suspension, it is 10.5 to adjust to PH, and ultrasonic vibration makes its uniform Afterwards, it is placed in reactor, reacts 21h at 100 DEG C, obtained sediment is cleaned repeatedly with deionized water and ethanol, is obtained just Walk product;
4)Above-mentioned primary product is carried out to alternating, step annealing at ambient pressure, annealing process is:Ar gas, 600 DEG C, 10min, N2 Gas, 800 DEG C, 10min, Ar gas, 1000 DEG C, 10min, N2Gas, 1200 DEG C, 10min, after annealing, obtain final product stone Black alkene/CuFe2O4Composite nano materials.
Embodiment 3
1)By Cu (CH3COO)2、Fe(CH3COO)2In molar ratio 1:2 proportionings, are dissolved in deionized water, form 1.5 mol/L's Mixed solution;
2)By above-mentioned mixed solution and redox graphene(rGO)Suspension mixes, volume ratio 1:6, wherein rGO suspension Concentration is 1.5 mol/L, forms new mixing suspension;
3)2 mol/L LiOH solution is added in above-mentioned mixing suspension, it is 10.5 to adjust to PH, and ultrasonic vibration makes its uniform Afterwards, it is placed in reactor, reacts 21h at 100 DEG C, obtained sediment is cleaned repeatedly with deionized water and ethanol, is obtained just Walk product;
4)Above-mentioned primary product is carried out to alternating, step annealing at ambient pressure, annealing process is:Ar gas, 600 DEG C, 10min, N2 Gas, 800 DEG C, 10min, Ar gas, 1000 DEG C, 10min, N2Gas, 1200 DEG C, 10min, after annealing, obtain final product stone Black alkene/CuFe2O4Composite nano materials.
Pass through transmission electron microscope(TEM)To graphene/CuFe made from each embodiment2O4Composite nano materials are carried out Morphology observation, if Fig. 1 is graphene/CuFe that embodiment 1 obtains2O4The transmission electron microscope of composite nano materials(TEM) Scheme, CuFe is shown in figure2O4For nanometer chip architecture, size about 100nm, size uniformity, and it is evenly distributed in flake graphite alkene On.
Using nano composite material made from each embodiment as electrode, electrical performance testing is carried out.Test result is shown, real Apply graphene/CuFe that example 1 obtains2O4During electrode of the composite nano materials as ultracapacitor, have electric double layer capacitance special Property, under 1 A/g current density, the F/g of specific capacitance 579;When current density increases to 10 A/g, specific capacitance is 465 F/ G, conservation rate 80.3%;After loop test 5000 times, specific capacitance conservation rate is 88.2%;Performance is extremely excellent, far above having reported Other electric double layer capacitance electrodes in road, such as the 50-150 F/g of activated carbon.Fig. 2 is graphene/CuFe that embodiment 1 obtains2O4It is multiple Stable circulation linearity curve when closing nano material as electrode, the test A/g of current density 3, after loop test 5000 times, than electricity It is 88.2% to hold conservation rate.Graphene/CuFe is made in embodiment 2 and embodiment 32O4Composite nano materials are as super capacitor electrode During pole, it is as follows to test its electrical performance index:
Graphene/CuFe is made in embodiment 22O4Composite nano materials, there is electric double layer capacitance characteristic;It is close in 1 A/g electric current Under degree, the F/g of specific capacitance 561;When current density increases to 10 A/g, specific capacitance is 443 F/g, conservation rate 79%;Circulation After test 5000 times, specific capacitance conservation rate is 90.1%.
Graphene/CuFe is made in embodiment 32O4Composite nano materials, there is electric double layer capacitance characteristic;In 1 A/g electric current Under density, the F/g of specific capacitance 602;When current density increases to 10 A/g, specific capacitance is 487 F/g, conservation rate 80.9%; After loop test 5000 times, specific capacitance conservation rate is 87.5%.
Obviously, although present disclosure has been made complete and clearly described with regard to its disclosed embodiment, It is not limited only to this, and embodiments described above is only part of the embodiment of the present invention, rather than whole embodiments.It is right For the personnel of art, obtained institute is made improvements and substitutes to the present invention by the guidance of these statements There is other embodiment, among the present invention.

Claims (4)

  1. A kind of 1. ultracapacitor graphene/CuFe2O4Composite nano materials and preparation method thereof, it is characterised in that:It is described CuFe2O4For nanometer chip architecture, size uniformity, and it is evenly distributed on flake graphite alkene.
  2. A kind of 2. ultracapacitor graphene/CuFe according to claim 12O4Composite nano materials and its preparation side Method, it is characterised in that:The CuFe2O4Size about 100nm.
  3. A kind of 3. ultracapacitor graphene/CuFe according to claim 1 or 22O4Composite nano materials and its preparation Method, it is characterised in that comprise the following steps:
    1)By Cu (CH3COO)2、Fe(CH3COO)2In molar ratio 1:2 proportionings, are dissolved in deionized water, form the mixed of 1.5 mol/L Close solution;
    2)By above-mentioned mixed solution and redox graphene(rGO)Suspension mixes, volume ratio 1:3-1:6, wherein rGO hangs Supernatant liquid concentration is 1.5 mol/L, forms new mixing suspension;
    3)2 mol/L LiOH solution is added in above-mentioned mixing suspension, it is 10.5 to adjust to PH, and ultrasonic vibration makes its uniform Afterwards, it is placed in reactor, reacts 21h at 100 DEG C, obtained sediment is cleaned repeatedly with deionized water and ethanol, is obtained just Walk product;
    4)Above-mentioned primary product is annealed at ambient pressure, obtains final product.
  4. A kind of 4. ultracapacitor graphene/CuFe according to claim 32O4Composite nano materials and its preparation side Method, it is characterised in that:Step 4)The technique of annealing is:Ar gas, 600 DEG C, 10min, N2Gas, 800 DEG C, 10min, Ar gas, 1000 DEG C, 10min, N2Gas, 1200 DEG C, 10min.
CN201710807096.6A 2017-09-08 2017-09-08 A kind of ultracapacitor graphene/CuFe2O4Composite nano materials and preparation method thereof Withdrawn CN107591255A (en)

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Citations (8)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN102527387A (en) * 2011-12-26 2012-07-04 南京理工大学 Copper ferrite-graphene nano complex and preparation method thereof
CN102779994A (en) * 2012-07-23 2012-11-14 浙江大学 Iron-based complex oxide/graphene composite and preparation method and application thereof
CN103066249A (en) * 2013-01-25 2013-04-24 浙江大学 Cobalt-based complex oxide/graphene composite material as well as preparation method and application thereof
CN103316635A (en) * 2013-07-03 2013-09-25 重庆交通大学 Graphene/double-metal oxide composite material and preparation method and application thereof
CN104576075A (en) * 2014-12-31 2015-04-29 江苏江大环保科技开发有限公司 Preparation method of 3D coralline graphene/NiCo2O4 composite material and application of same in super capacitor
CN104882298A (en) * 2015-04-30 2015-09-02 江苏大学 Method for preparing NiCo2O4/graphene supercapacitor material with microwave method
CN104944474A (en) * 2015-06-23 2015-09-30 中南大学 Method for preparing nanometer MnFe2O4/graphene composite material
WO2017091815A1 (en) * 2015-11-25 2017-06-01 William Marsh Rice University Formation of three-dimensional materials by combining catalytic and precursor materials

Patent Citations (8)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN102527387A (en) * 2011-12-26 2012-07-04 南京理工大学 Copper ferrite-graphene nano complex and preparation method thereof
CN102779994A (en) * 2012-07-23 2012-11-14 浙江大学 Iron-based complex oxide/graphene composite and preparation method and application thereof
CN103066249A (en) * 2013-01-25 2013-04-24 浙江大学 Cobalt-based complex oxide/graphene composite material as well as preparation method and application thereof
CN103316635A (en) * 2013-07-03 2013-09-25 重庆交通大学 Graphene/double-metal oxide composite material and preparation method and application thereof
CN104576075A (en) * 2014-12-31 2015-04-29 江苏江大环保科技开发有限公司 Preparation method of 3D coralline graphene/NiCo2O4 composite material and application of same in super capacitor
CN104882298A (en) * 2015-04-30 2015-09-02 江苏大学 Method for preparing NiCo2O4/graphene supercapacitor material with microwave method
CN104944474A (en) * 2015-06-23 2015-09-30 中南大学 Method for preparing nanometer MnFe2O4/graphene composite material
WO2017091815A1 (en) * 2015-11-25 2017-06-01 William Marsh Rice University Formation of three-dimensional materials by combining catalytic and precursor materials

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