CN104124442B - A kind of nanometer Fe2O3The preparation method of/rGO composite and application - Google Patents
A kind of nanometer Fe2O3The preparation method of/rGO composite and application Download PDFInfo
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- CN104124442B CN104124442B CN201410311647.6A CN201410311647A CN104124442B CN 104124442 B CN104124442 B CN 104124442B CN 201410311647 A CN201410311647 A CN 201410311647A CN 104124442 B CN104124442 B CN 104124442B
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- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01M—PROCESSES OR MEANS, e.g. BATTERIES, FOR THE DIRECT CONVERSION OF CHEMICAL ENERGY INTO ELECTRICAL ENERGY
- H01M4/00—Electrodes
- H01M4/02—Electrodes composed of, or comprising, active material
- H01M4/36—Selection of substances as active materials, active masses, active liquids
- H01M4/362—Composites
- H01M4/364—Composites as mixtures
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B82—NANOTECHNOLOGY
- B82Y—SPECIFIC USES OR APPLICATIONS OF NANOSTRUCTURES; MEASUREMENT OR ANALYSIS OF NANOSTRUCTURES; MANUFACTURE OR TREATMENT OF NANOSTRUCTURES
- B82Y30/00—Nanotechnology for materials or surface science, e.g. nanocomposites
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B82—NANOTECHNOLOGY
- B82Y—SPECIFIC USES OR APPLICATIONS OF NANOSTRUCTURES; MEASUREMENT OR ANALYSIS OF NANOSTRUCTURES; MANUFACTURE OR TREATMENT OF NANOSTRUCTURES
- B82Y40/00—Manufacture or treatment of nanostructures
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- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01M—PROCESSES OR MEANS, e.g. BATTERIES, FOR THE DIRECT CONVERSION OF CHEMICAL ENERGY INTO ELECTRICAL ENERGY
- H01M10/00—Secondary cells; Manufacture thereof
- H01M10/05—Accumulators with non-aqueous electrolyte
- H01M10/052—Li-accumulators
- H01M10/0525—Rocking-chair batteries, i.e. batteries with lithium insertion or intercalation in both electrodes; Lithium-ion batteries
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- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01M—PROCESSES OR MEANS, e.g. BATTERIES, FOR THE DIRECT CONVERSION OF CHEMICAL ENERGY INTO ELECTRICAL ENERGY
- H01M4/00—Electrodes
- H01M4/02—Electrodes composed of, or comprising, active material
- H01M4/36—Selection of substances as active materials, active masses, active liquids
- H01M4/48—Selection of substances as active materials, active masses, active liquids of inorganic oxides or hydroxides
- H01M4/52—Selection of substances as active materials, active masses, active liquids of inorganic oxides or hydroxides of nickel, cobalt or iron
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- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01M—PROCESSES OR MEANS, e.g. BATTERIES, FOR THE DIRECT CONVERSION OF CHEMICAL ENERGY INTO ELECTRICAL ENERGY
- H01M4/00—Electrodes
- H01M4/02—Electrodes composed of, or comprising, active material
- H01M2004/021—Physical characteristics, e.g. porosity, surface area
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- 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
- Y02E60/10—Energy storage using batteries
Abstract
The present invention relates to the preparation field of nano composite material, be specifically related to a kind of nanometer Fe2O3The preparation method of/rGO composite and application.A kind of nanometer Fe2O3The preparation method of/rGO composite, comprises the steps of FeSO4.7H2O is dissolved in water and formation mixed solution A in the mixing liquid of glycerol；Graphite oxide is scattered in water and ultrasonic disperse, forms solution B；Solution B is added to mixed solution A, is mixing uniformly to form mixed solution C；Described mixed solution C is put in autoclave, described autoclave is placed under the temperature environment of 140 ~ 180 DEG C and reacts after 8 ~ 12 hours obtains product；Finally product is used dehydrated alcohol and water washing for several times respectively, put into dry a few hours in 60～100 DEG C of vacuum drying ovens, obtain described nanometer Fe2O3/ rGO composite.The cheaper starting materials of preparation method provided by the invention is easy to get, and cost is low, and synthesis technique simply easily realizes, and constant product quality and process repeatability can be good.
Description
Technical field
The present invention relates to the preparation field of nano composite material, be specifically related to a kind of nanometer Fe2O3The preparation method of/rGO composite and application.
Background technology
Nanometer Fe2O3As a kind of important nano material, owing to it has the physicochemical properties of uniqueness, such as small-size effect, skin effect, interfacial effect etc. so that it is be all widely used in each technical field.At present, nanometer Fe2O3Can also be applied in the middle of secondary cell as the negative material of lithium ion battery, but the nanometer Fe of existing preparation method gained2O3When discharge and recharge owing to it conducts electricity rate variance, the coefficient of cubical expansion is poor, the lithium ion battery obtained often poor effect.
And Graphene is as a kind of excellent material and nanometer Fe2O3Compound can solve the problem that the defect of prior art, and has the nanometer Fe of specific morphology2O3It is embedded in Graphene to be not reported so far.
Summary of the invention
The technical problem to be solved is to provide kind of a nanometer Fe2O3The preparation method of/rGO composite.
It is a further object to provide the Fe of above-mentioned preparation method gained2O3/ rGO composite is as the application of lithium cell cathode material.
The technical problem to be solved is achieved by the following technical programs:
A kind of nanometer Fe2O3The preparation method of/rGO composite, comprises the steps of
A) by FeSO47H2O is dissolved in water and formation mixed solution A in the mixing liquid of glycerol；
B) graphite oxide is scattered in water and ultrasonic disperse, forms solution B；
C) solution B is added to mixed solution A, be mixing uniformly to form mixed solution C；
D) described mixed solution C is put in autoclave, described autoclave is placed under the temperature environment of 140 ~ 180 DEG C and reacts after 8 ~ 12 hours obtains product；
E) product is used dehydrated alcohol and water washing for several times respectively, put into dry a few hours in 60～100 DEG C of vacuum drying ovens, obtain described nanometer Fe2O3/ rGO composite.
Further, the water in described step a) is 3.5 ~ 4:1 with the volume ratio of glycerol.
Further, the concentration of described mixed solution A is 0.035 ~ 0.045mol/L.
Further, in described step b), ultrasonic time is 1.5 ~ 3h.
Further, the concentration of described solution B is 1 ~ 1.5g/L.
The nanometer Fe of described preparation method gained2O3/ rGO composite is as the application of lithium cell cathode material.
There is advantages that
(1) cheaper starting materials of preparation method provided by the invention is easy to get, and cost is low, and synthesis technique simply easily realizes, and constant product quality and process repeatability can be good.
(2) nanometer Fe prepared by the present invention2O3/ rGO composite gauge, pattern are homogeneous, and Fe2O3Nanometer sheet is embedded in Graphene uniformly.
(3) this preparation method any surfactant need not be used, halide ion etc., will not to the nanometer Fe of gained of the present invention2O3/ rGO composite introduces any impurity.
(4) nanometer Fe of this preparation method gained2O3When/rGO composite uses as lithium cell cathode material, charge-discharge performance is good, even if capacity is still up to 429mAh/g after 10C discharge and recharge 1000 weeks.
Accompanying drawing explanation
Fig. 1 is the nanometer Fe prepared by embodiments of the invention 12O3The XRD figure spectrum of/rGO composite.
Fig. 2 is the nanometer Fe prepared by embodiments of the invention 12O3The SEM figure of/rGO composite.
Fig. 3 is the nanometer Fe prepared by embodiments of the invention 12O3The TEM figure of/rGO composite.
Fig. 4 is the nanometer Fe prepared by embodiments of the invention 22O3The SEM figure of/rGO composite.
Fig. 5 is that embodiments of the invention 5 are with nanometer Fe2O3Charge and discharge electrograph under the lithium battery different multiplying that/rGO composite is prepared as negative pole.
Fig. 6 is that embodiments of the invention 5 are with nanometer Fe2O3The lithium battery that/rGO composite is prepared as negative pole circulation figure under 10C discharge and recharge.
Detailed description of the invention
Below in conjunction with drawings and Examples, the present invention will be described in detail.
Graphite oxide used in the present invention all synthesizes with prior art, for instance Hummers method.
Embodiment 1
A) by 1.1gFeSO47H2O is dissolved in 80ml water and formation mixed solution A in the mixing liquid of 20ml glycerol；
B) 0.04 graphite oxide is scattered in 40ml water and ultrasonic disperse 2h, forms solution B；
C) solution B is added to mixed solution A, be mixing uniformly to form mixed solution C；
D) described mixed solution C is put in autoclave, described autoclave is placed under the temperature environment of 180 DEG C and reacts after 10 hours obtains product；
E) product is used dehydrated alcohol and water washing for several times respectively, put into dry a few hours in 70 DEG C of vacuum drying ovens, obtain described nanometer Fe2O3/ rGO composite.
Product is accredited as α-Fe through X-ray powder diffraction2O3, powder X-ray diffraction result is as shown in Figure 1；Material morphology passes through scanning electron microscope, transmission electron microscope such as Fig. 2, shown in 3, and the α-Fe of nano-sheet as we know from the figure2O3It is uniformly embedded into Graphene.
In the middle of this preparation method, owing to the graphite oxide surface added has abundant functional group, it is possible to by electrostatic interaction by Fe2+Absorption forms α-Fe from the teeth outwards2O3.And the glycerol added its be not only able to induction α-Fe2O3Form the structure of nanometer sheet, and it contains substantial amounts of hydroxyl and has reproducibility, it is possible to graphite oxide is reduced into Graphene.
Embodiment 2
A) by 1.1gFeSO47H2O is dissolved in 70ml water and formation mixed solution A in the mixing liquid of 20ml glycerol；
B) 0.04 graphite oxide is scattered in 40ml water and ultrasonic disperse 2h, forms solution B；
C) solution B is added to mixed solution A, be mixing uniformly to form mixed solution C；
D) described mixed solution C is put in autoclave, described autoclave is placed under the temperature environment of 140 DEG C and reacts after 10 hours obtains product；
E) product is used dehydrated alcohol and water washing for several times respectively, put into dry a few hours in 70 DEG C of vacuum drying ovens, obtain described nanometer Fe2O3/ rGO composite.
Products therefrom is similar through X-ray powder diffraction such as Fig. 1, and material morphology passes through scanning electron microscope as shown in Figure 4, the α-Fe of nano-sheet as we know from the figure2O3It is uniformly embedded into Graphene.
Embodiment 3
A) by 1.1gFeSO47H2O is dissolved in 80ml water and formation mixed solution A in the mixing liquid of 20ml glycerol；
B) 0.04 graphite oxide is scattered in 40ml water and ultrasonic disperse 2.5h, forms solution B；
C) solution B is added to mixed solution A, be mixing uniformly to form mixed solution C；
D) described mixed solution C is put in autoclave, described autoclave is placed under the temperature environment of 150 DEG C and reacts after 12 hours obtains product；
E) product is used dehydrated alcohol and water washing for several times respectively, put into dry a few hours in 60 DEG C of vacuum drying ovens, obtain described nanometer Fe2O3/ rGO composite.
Products therefrom identifies the (nanometer Fe with embodiment 1 preparation through X-ray powder diffraction, scanning electron microscope2O3/ rGO composite is similar) known its be nanometer Fe2O3/ rGO composite.
Embodiment 4
A) by 1.1gFeSO47H2O is dissolved in 80ml water and formation mixed solution A in the mixing liquid of 20ml glycerol；
B) 0.04 graphite oxide is scattered in 40ml water and ultrasonic disperse 2h, forms solution B；
C) solution B is added to mixed solution A, be mixing uniformly to form mixed solution C；
D) described mixed solution C is put in autoclave, described autoclave is placed under the temperature environment of 160 DEG C and reacts after 9 hours obtains product；
E) product is used dehydrated alcohol and water washing for several times respectively, put into dry a few hours in 60 DEG C of vacuum drying ovens, obtain described nanometer Fe2O3/ rGO composite.
Products therefrom identifies the (nanometer Fe with embodiment 1 preparation through X-ray powder diffraction, scanning electron microscope2O3/ rGO composite is similar) known its be nanometer Fe2O3/ rGO composite.
Embodiment 5
Nanometer Fe by embodiment 1 ~ 4 gained2O3/ rGO composite prepares into lithium ion battery (preparation method is the routine techniques of this technical field, is not described in detail in the present invention) as negative pole
As can be seen from Figure 5, due to nanometer Fe2O3For being embedded in the middle of Graphene, so the nanometer Fe of the present invention2O3/ rGO composite has excellent high rate performance as the negative pole of lithium ion battery；And as can be seen from Figure 6, the rice Fe of the present invention2O3/ rGO composite as the negative pole of lithium ion battery when 10C after discharge and recharge 1000 weeks capacity still up to 429mAh/g.
Embodiment described above only have expressed embodiments of the present invention; it describes comparatively concrete and detailed; but therefore can not be interpreted as the restriction to the scope of the claims of the present invention; in every case the technical scheme adopting the form of equivalent replacement or equivalent transformation to obtain, all should drop within protection scope of the present invention.
Claims (6)
1. a nanometer Fe2O3The preparation method of/rGO composite, it is characterised in that comprise the steps of
A) by FeSO4·7H2O is dissolved in water and formation mixed solution A in the mixing liquid of glycerol；
B) graphite oxide is scattered in water and ultrasonic disperse, forms solution B；
C) solution B is added to mixed solution A, be mixing uniformly to form mixed solution C；
D) described mixed solution C is put in autoclave, described autoclave is placed under the temperature environment of 140 ~ 180 DEG C and reacts after 8 ~ 12 hours obtains product；
E) product is used dehydrated alcohol and water washing for several times respectively, put into dry a few hours in 60～100 DEG C of vacuum drying ovens, obtain described nanometer Fe2O3/ rGO composite.
2. a kind of nanometer Fe according to claim 12O3The preparation method of/rGO composite, it is characterised in that the volume ratio of the water in described step a) and glycerol is 3.5 ~ 4:1.
3. a kind of nanometer Fe according to claim 22O3The preparation method of/rGO composite, it is characterised in that the concentration of described mixed solution A is 0.035 ~ 0.045mol/L.
4. according to a kind of nanometer Fe according to claim 32O3The preparation method of/rGO composite, it is characterised in that in described step b), ultrasonic time is 1.5 ~ 3h.
5. according to a kind of nanometer Fe according to claim 42O3The preparation method of/rGO composite, it is characterised in that the concentration of described solution B is 1 ~ 1.5g/L.
6. the nanometer Fe of the preparation method gained described in a claim 12O3/ rGO composite is as the application of lithium cell cathode material.
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Families Citing this family (6)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN104528836B (en) * | 2015-01-23 | 2016-06-01 | 哈尔滨工业大学 | A kind of regulation and control ��-Fe2O3The method of/graphene composite material shape looks |
| 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 |
| CN107452943B (en) * | 2017-07-13 | 2020-12-22 | 陕西科技大学 | Preparation method of graphene-loaded iron oxide self-assembled mulberry-like structure lithium ion battery negative 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 |
| CN112481652B (en) * | 2020-11-20 | 2022-01-21 | 河南大学 | Graphene modified CoOOH/Fe2O3Composite electrode material and preparation method thereof |
| CN114275822B (en) * | 2021-12-31 | 2023-12-22 | 吕梁学院 | Preparation method and application of iron-containing compound modified graphene nanocomposite with different morphologies and crystalline phases |
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| CN103367720A (en) * | 2013-07-09 | 2013-10-23 | 上海交通大学 | Preparation method of graphene and porous ferric oxide composite |
| CN103464740A (en) * | 2013-08-16 | 2013-12-25 | 安徽师范大学 | Micro and nano alpha-Fe2O3 material and preparation method thereof |
| CN103560228A (en) * | 2013-10-29 | 2014-02-05 | 中国石油大学(华东) | Method for compositing iron oxide and graphene by virtue of hydrothermal process |
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Patent Citations (3)
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| CN103367720A (en) * | 2013-07-09 | 2013-10-23 | 上海交通大学 | Preparation method of graphene and porous ferric oxide composite |
| CN103464740A (en) * | 2013-08-16 | 2013-12-25 | 安徽师范大学 | Micro and nano alpha-Fe2O3 material and preparation method thereof |
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