CN105489398A - Preparation method of Fe2O3/graphene composite material - Google Patents
Preparation method of Fe2O3/graphene composite material Download PDFInfo
- Publication number
- CN105489398A CN105489398A CN201610024861.2A CN201610024861A CN105489398A CN 105489398 A CN105489398 A CN 105489398A CN 201610024861 A CN201610024861 A CN 201610024861A CN 105489398 A CN105489398 A CN 105489398A
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- China
- Prior art keywords
- composite material
- preparation
- graphene oxide
- graphene
- fe2o3
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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
-
- 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
-
- 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
- H01G11/32—Carbon-based
- H01G11/36—Nanostructures, e.g. nanofibres, nanotubes or fullerenes
-
- 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
- H01G11/46—Metal oxides
-
- 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 belongs to the technical field of a supercapacitor nanometer composite material, and particularly to a preparation method of an Fe2O3/graphene composite material. The preparation method of the Fe2O3/graphene composite material comprises the steps of (1), preparing a graphene oxide colloidal solution; (2) mixing the graphene oxide colloidal solution and a ferric hydroxide colloid or a saturated ferric chloride solution, and performing ultrasonic treatment; and (3) placing the mixed solution after ultrasonic treatment into a hydrothermal reactor for reaction, and after reaction finishement, performing natural cooling, washing and drying for obtaining the Fe2O3/graphene composite material. The preparation method has advantages of simple operation and environment-friendly process. Not only can size of Fe2O3 particle diameter be effectively controlled for obtaining Fe2O3 crystals with different particle diameters, but also the Fe2O3 is dispersed in the graphene in a more uniform manner. The Fe2O3/graphene composite material represents an excellent electrochemical performance when used as a supercapacitor nanometer composite material. Furthermore the preparation method is a novel way for preparing a controllable metal oxide in a supercapacitor electrode material.
Description
Technical field
The invention belongs to a kind of preparing technical field of ultracapacitor electric conducting material, be specifically related to a kind of Fe
2o
3the preparation method of/graphene composite material.
Background technology
Along with people are to the continuous increase of energy demand, exploitation high-efficiency energy-storage equipment becomes an important task.Ultracapacitor, is a kind of novel energy-storing device reacting generation electrochemical capacitor by faraday, has increasing application gradually in recent years in portable electric appts, hybrid vehicle and Electric power car.The electrode material performance of ultracapacitor affects its chemical property to a great extent.By Fe
2o
3uniform crystal dispersion among Graphene, thus obtains taking Graphene as the composite material of matrix, is the effective means preparing high performance electrode material.But in preparation process, due to Fe
2o
3the formation speed of crystal, often occurs piling up or growing into larger crystal, can not get homodisperse composite material, had a strong impact on the chemical property of material, therefore, prepare the Graphene/Fe of size tunable
2o
3composite material has important meaning to the high performance electrode material for super capacitor of preparation.
Summary of the invention
In order to overcome the deficiencies in the prior art, the object of the present invention is to provide a kind of Fe
2o
3the preparation method of/graphene composite material, this preparation method is simple, the Fe obtained
2o
3in/graphene composite material, Fe
2o
3uniform crystal dispersion among Graphene, simultaneously Fe
2o
3size tunable.
Saturated ferric chloride solution is made colloid or is directly mixed with graphene oxide under low temperature or normal temperature by saturated ferric chloride solution by the present invention, and is aided with ultrasonic process, prepares the Fe of different-grain diameter
2o
3be dispersed in the composite material in Graphene.
The invention provides a kind of Fe
2o
3the preparation method of/graphene composite material, concrete steps are as follows:
(1) graphene oxide is dispersed in water, afterwards ultrasonic process, obtains the graphene oxide colloidal solution of transparent and homogeneous;
(2) graphene oxide colloidal solution step (1) obtained and ferric hydroxide colloid or the mixing of saturated ferric chloride solution, after mixing, ultrasonic process 20min ~ 2h;
(3) by the mixed solution that step (2) obtains, in water heating kettle, 170-190 DEG C is reacted 10 ~ 13 hours; After reaction terminates, naturally cool, washing, oven dry obtain Fe
2o
3/ graphene composite material.
In above-mentioned steps (1), in graphene oxide colloidal solution, the mass volume ratio concentration of graphene oxide is between 0.3-0.6mg/mL.
In above-mentioned steps (2), by graphene oxide colloidal solution and ferric hydroxide colloid mixing, be realize by graphene oxide colloidal solution is slowly added drop-wise in ferric hydroxide colloid while stirring.
In above-mentioned steps (2), the volume ratio of described graphene oxide colloidal solution and ferric hydroxide colloid is 14:1 ~ 16:1.
In above-mentioned steps (2), by graphene oxide colloidal solution and the mixing of saturated ferric chloride solution, be by under condition of ice bath or room temperature condition, saturated ferric chloride solution be added drop-wise in graphene oxide colloidal solution realize while stirring.
In above-mentioned steps (2), the volume ratio of described graphene oxide colloidal solution and saturated ferric chloride solution is 20:1 ~ 30:1.
In above-mentioned steps (2), ultrasonic power is 300W.
The Fe that the present invention obtains by saturated ferric chloride solution being made colloid
2o
3in/graphene composite material, Fe
2o
3particle diameter between 600 ~ 800nm.
The Fe that saturated ferric chloride solution obtains is adopted under condition of ice bath of the present invention
2o
3in/graphene composite material, Fe
2o
3particle diameter between 300 ~ 500nm; The Fe that saturated ferric chloride solution obtains is adopted under normal temperature condition
2o
3in/graphene composite material, Fe
2o
3particle diameter between 0.9 ~ 1.2 μm.
Beneficial effect of the present invention is:
1) preparation method of the present invention is simple and easy to do, size controlling successful.
2) Fe
2o
3be dispersed among Graphene, and Graphene is without obvious agglomeration.
3) by control Fe
2o
3particle diameter, the chemical property of composite material is is also significantly regulated and controled simultaneously, and all demonstrates good chemical property.
4) preparing overall process does not have noxious substance to produce, and environmental friendliness meets Green Chemistry concept.
Accompanying drawing explanation
Fig. 1 is Fe prepared by embodiment 1
2o
3particle diameter is at composite material SEM (ESEM) figure of about 500nm.
Fig. 2 is Fe prepared by embodiment 2
2o
3particle diameter is schemed at the composite material SEM of about 800nm.
Fig. 3 is Fe prepared by embodiment 3
2o
3particle diameter is schemed at the composite material SEM of about 1.2 μm.
Fig. 4 is embodiment 1,2, three kinds of different-grain diameter Fe in 3
2o
3with the cyclic voltammetry curve of composite material under sweep speed is 20mV/s of Graphene.
Fig. 5 is embodiment 1,2, three kinds of different-grain diameter Fe in 3
2o
3with the charging and discharging curve of composite material under 2A/g of Graphene.
Embodiment
Further illustrate technical scheme of the present invention below by several preferred example, but the explanation of described embodiment is only a part of embodiment of the present invention, should not be interpreted as limitation of the present invention in any degree.
Embodiment 1
1) preparing 30mL concentration is the graphene oxide solution of 0.5g/mL, and ultrasonic process, obtains the colloidal solution of transparent and homogeneous.
2) get the deionized water of 30mL, be heated to boiling, drip the saturated ferric chloride solution of 2mL to it, keep boiling 3min, obtained ferric hydroxide colloid, then cools naturally.
3) get 2mL ferric hydroxide colloid, slowly add 1 while stirring) middle solution, ultrasonic 30min.
4) above-mentioned solution is proceeded to 100mL polytetrafluoroethylene as in the stainless steel water heating kettle of liner, keep 12 hours at 180 DEG C of constant temperature.
5) after water heating kettle cools naturally, spend deionized water gained respectively and precipitate three times, and dry at 80 DEG C.In the composite material obtained, Fe
2o
3particle diameter is at about 500nm.Its scanning electron microscope (SEM) photograph as shown in Figure 1.
The chemical property of the electrochemical workstation test CHI760 test material adopting Shanghai Chen Hua Instrument Ltd. to produce, active material, conductive black and polytetrafluoroethylene mix according to 8:1:1, are then coated in nickel foam and make electrode.Cv curve is as shown in a in Fig. 4, and obvious redox peak, illustrates that composite material demonstrates good electrochemical behavior in cyclic process.Charging and discharging curve is as shown in a in Fig. 5, and under the current density of 2A/g, capacitance reaches 375F/g.
Embodiment 2
1) preparing 30mL concentration is the graphene oxide solution of 0.5g/mL, and ultrasonic process, obtains the colloidal solution of transparent and homogeneous.
2) by 1) in solution proceed among ice bath, treat that its temperature is down to 0-5 DEG C.
3) to 1) the saturated ferric chloride solution of middle solution dropping 1mL, limit edged stirs, ultrasonic 30min after completing.
4) above-mentioned solution is proceeded to 100mL polytetrafluoroethylene as in the stainless steel water heating kettle of liner, keep 12 hours at 180 DEG C of constant temperature.
5) after water heating kettle cools naturally, spend deionized water gained respectively and precipitate three times, and dry at 80 DEG C, in the composite material obtained, Fe
2o
3particle diameter is at about 500nm, and its scanning electron microscope (SEM) photograph as shown in Figure 2.
Cv curve is as shown in a in Fig. 4, and obvious redox peak, illustrates that composite material demonstrates good electrochemical behavior in cyclic process.Charging and discharging curve is as shown in a in Fig. 5, and under the current density of 2A/g, capacitance reaches 301F/g.
Embodiment 3
According to the method for embodiment 2, just do not add ice bath, directly to adding saturated ferric chloride solution in graphene oxide.The composite material finally obtained, Fe
2o
3particle diameter is at about 1.2 μm, and its scanning electron microscope (SEM) photograph as shown in Figure 3.
Cv curve is as shown in a in Fig. 4, and obvious redox peak, illustrates that composite material demonstrates good electrochemical behavior in cyclic process.Charging and discharging curve is as shown in a in Fig. 5, and under the current density of 2A/g, capacitance reaches 297F/g.
Claims (9)
1. a Fe
2o
3the preparation method of/graphene composite material, is characterized in that, concrete steps are as follows:
(1) graphene oxide is dispersed in water, afterwards ultrasonic process, obtains the graphene oxide colloidal solution of transparent and homogeneous;
(2) graphene oxide colloidal solution step (1) obtained and ferric hydroxide colloid or the mixing of saturated ferric chloride solution, after mixing, ultrasonic process 20min-2h;
(3) by the mixed solution that step (2) obtains, 170-190 DEG C of reaction 10-13 hour in water heating kettle; After reaction terminates, naturally cool, washing, oven dry obtain Fe
2o
3/ graphene composite material.
2. preparation method as claimed in claim 1, it is characterized in that, in step (1), in graphene oxide colloidal solution, the mass volume ratio concentration of graphene oxide is between 0.3-0.6mg/mL.
3. preparation method as claimed in claim 1, it is characterized in that, in step (2), by graphene oxide colloidal solution and ferric hydroxide colloid mixing, be realize by graphene oxide colloidal solution is slowly added drop-wise in ferric hydroxide colloid while stirring.
4. the preparation method as described in claim 1 or 3, is characterized in that, in step (2), the volume ratio of described graphene oxide colloidal solution and ferric hydroxide colloid is 14:1 ~ 16:1.
5. preparation method as claimed in claim 1, it is characterized in that, in step (2), by graphene oxide colloidal solution and the mixing of saturated ferric chloride solution, be by under condition of ice bath or room temperature condition, saturated ferric chloride solution be added drop-wise in graphene oxide colloidal solution realize while stirring.
6. the preparation method as described in claim 1 or 5, is characterized in that, in step (2), the volume ratio of described graphene oxide colloidal solution and saturated ferric chloride solution is 28:1 ~ 30:1.
7. preparation method as claimed in claim 1, it is characterized in that, in step (2), ultrasonic power is 300W.
8. preparation method as claimed in claim 3, is characterized in that, the Fe obtained
2o
3in/graphene composite material, Fe
2o
3particle diameter between 600 ~ 800nm.
9. preparation method as claimed in claim 5, is characterized in that, the Fe obtained under condition of ice bath
2o
3in/graphene composite material, Fe
2o
3particle diameter between 300 ~ 500nm; The Fe obtained under normal temperature condition
2o
3in/graphene composite material, Fe
2o
3particle diameter between 0.9 ~ 1.2 μm.
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Cited By (11)
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CN105924963A (en) * | 2016-06-06 | 2016-09-07 | 上海应用技术学院 | Preparation method of graphene/ ferric oxide/ polyaniline composite material |
CN106328937A (en) * | 2016-09-13 | 2017-01-11 | 武汉理工大学 | Method molecular self-assembly and preparation of Fe2O3-graphene negative electrode material |
CN106449157A (en) * | 2016-11-29 | 2017-02-22 | 中国科学院山西煤炭化学研究所 | Method for preparing iron-oxide/graphene-film super-capacitor electrode material |
CN106854389A (en) * | 2017-01-11 | 2017-06-16 | 山东欧铂新材料有限公司 | A kind of micaceous iron oxide/graphene oxide composite material and preparation method thereof |
CN107093520A (en) * | 2017-03-03 | 2017-08-25 | 清华大学深圳研究生院 | A kind of three layers of integrated flexible film ultracapacitor and preparation method thereof |
CN107256810A (en) * | 2017-06-12 | 2017-10-17 | 中科合成油技术有限公司 | A kind of iron oxide/stannic oxide/graphene nano composite and preparation method thereof and the application in ultracapacitor |
CN107253708A (en) * | 2017-04-29 | 2017-10-17 | 成都博美实润科技有限公司 | A kind of preparation method for the phenolic resin base porous carbon being modified based on graphene |
CN107910192A (en) * | 2017-11-17 | 2018-04-13 | 常州大学 | A kind of electrode material for super capacitor Fe2O3The preparation method of/rGO |
CN108878174A (en) * | 2018-06-19 | 2018-11-23 | 复旦大学 | A kind of preparation method of di-iron trioxide nanometer sheet/Graphene electrodes material |
CN109192550A (en) * | 2018-09-11 | 2019-01-11 | 上海应用技术大学 | A kind of redox graphene self-supporting film of inorganic nanoparticles load, preparation method and application |
CN109295552A (en) * | 2018-09-05 | 2019-02-01 | 山东理工大学 | A kind of preparation method of di-iron trioxide composite graphite alkene cladding cotton carbon fibre material |
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CN102130334A (en) * | 2011-01-15 | 2011-07-20 | 中国矿业大学 | Graphene-based nano iron oxide composite material and preparation method thereof |
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CN105924963A (en) * | 2016-06-06 | 2016-09-07 | 上海应用技术学院 | Preparation method of graphene/ ferric oxide/ polyaniline composite material |
CN105924963B (en) * | 2016-06-06 | 2018-08-10 | 上海应用技术学院 | A kind of preparation method of graphene/iron oxide/polyaniline composite material |
CN106328937A (en) * | 2016-09-13 | 2017-01-11 | 武汉理工大学 | Method molecular self-assembly and preparation of Fe2O3-graphene negative electrode material |
CN106328937B (en) * | 2016-09-13 | 2018-08-07 | 武汉理工大学 | A kind of molecular self-assembling preparation Fe2O3The method of@graphene negative materials |
CN106449157B (en) * | 2016-11-29 | 2018-06-29 | 中国科学院山西煤炭化学研究所 | A kind of preparation method of iron oxide/graphene film electrode material for super capacitor |
CN106449157A (en) * | 2016-11-29 | 2017-02-22 | 中国科学院山西煤炭化学研究所 | Method for preparing iron-oxide/graphene-film super-capacitor electrode material |
CN106854389A (en) * | 2017-01-11 | 2017-06-16 | 山东欧铂新材料有限公司 | A kind of micaceous iron oxide/graphene oxide composite material and preparation method thereof |
CN106854389B (en) * | 2017-01-11 | 2020-06-26 | 山东欧铂新材料有限公司 | Mica iron oxide/graphene oxide composite material and preparation method thereof |
CN107093520A (en) * | 2017-03-03 | 2017-08-25 | 清华大学深圳研究生院 | A kind of three layers of integrated flexible film ultracapacitor and preparation method thereof |
CN107253708A (en) * | 2017-04-29 | 2017-10-17 | 成都博美实润科技有限公司 | A kind of preparation method for the phenolic resin base porous carbon being modified based on graphene |
CN107256810A (en) * | 2017-06-12 | 2017-10-17 | 中科合成油技术有限公司 | A kind of iron oxide/stannic oxide/graphene nano composite and preparation method thereof and the application in ultracapacitor |
CN107910192A (en) * | 2017-11-17 | 2018-04-13 | 常州大学 | A kind of electrode material for super capacitor Fe2O3The preparation method of/rGO |
CN108878174A (en) * | 2018-06-19 | 2018-11-23 | 复旦大学 | A kind of preparation method of di-iron trioxide nanometer sheet/Graphene electrodes material |
CN108878174B (en) * | 2018-06-19 | 2020-09-25 | 复旦大学 | Preparation method of ferric oxide nanosheet/graphene electrode material |
CN109295552A (en) * | 2018-09-05 | 2019-02-01 | 山东理工大学 | A kind of preparation method of di-iron trioxide composite graphite alkene cladding cotton carbon fibre material |
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