CN109860577A - A kind of carbon/ferriferous oxide composite and flexible electrode material and preparation method thereof - Google Patents
A kind of carbon/ferriferous oxide composite and flexible electrode material and preparation method thereof Download PDFInfo
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- CN109860577A CN109860577A CN201910173101.1A CN201910173101A CN109860577A CN 109860577 A CN109860577 A CN 109860577A CN 201910173101 A CN201910173101 A CN 201910173101A CN 109860577 A CN109860577 A CN 109860577A
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- Y02E—REDUCTION OF GREENHOUSE GAS [GHG] EMISSIONS, RELATED TO ENERGY GENERATION, TRANSMISSION OR DISTRIBUTION
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Abstract
The invention discloses a kind of carbon/ferriferous oxide composite and flexible electrode materials and preparation method thereof, carbon material and ferriferous oxide are configured to dispersion liquid respectively, by polycarbonate perforated membrane after mixing, composite material film is prepared by the way of vacuum filtration, then after high-temperature heat treatment to obtain the final product;Wherein, the carbon material is graphene oxide, and the ferriferous oxide is ferroso-ferric oxide.After composite material is prepared in the compound ferriferous oxide of graphene oxide by the present invention, the graphene oxide restored using the active group that high temperature heat-treats removal surface of graphene oxide keeps nanocomposite constituents more stable;In addition, preparing graphene oxide/silicon/iron oxide composite material film of reduction by the way of filtering by polycarbonate porous vacuum, preparation process simple economy, operation is convenient, is easy to be mass produced.
Description
Technical field
The present invention relates to electrochemical technology field more particularly to a kind of carbon/ferriferous oxide composite and flexible electrode material and its
Preparation method.
Background technique
Ferriferous oxide (predominantly Fe3O4 and α-Fe2O3) have high capacity, reserves abundant, good safety and
Low cost, however, when being used for electrode material, there is very big body in charge and discharge process since its own electric conductivity is poor
Product variation, huge stress make active particle dusting in cyclic process, limit its application in lithium ion battery.And
Graphene possesses high-specific surface area, excellent electric conductivity, excellent mechanical tenacity and special lamellar structure, by itself and nanometer
In the compound obtained composite material of ferriferrous oxide particles, graphene high-specific surface area can load more oxidations of active nano four three
Iron particle, meanwhile, nano ferriferrous oxide granule is attached in graphene sheet layer, and graphene had both been used as the conduction of electronics and ion
Frame, and the buffer layer as the variation of Fe3O4 particle volume.Therefore, the two is compound, respective advantage is played, can be prepared into
To high capacity, the lithium ion battery negative material of flexibility, good cycle.
Currently, graphene and the compound of ferriferous oxide use CVD, electrostatic spinning (such as patent 108630921A) or electrophoresis
It deposits (such as patent 105420794B).Meanwhile graphene used in these methods is mostly graphene oxide, or is used swollen
The mode preparation of swollen graphite ultrasonic disperse in a solvent prepares graphene.
But discovery is using CVD, electrostatic spinning (such as patent 108630921A) or electrophoretic deposition (as specially in practical applications
Sharp 105420794B) composite material is prepared, manufacture craft is relative complex, higher cost, is unfavorable for being mass produced;Using oxygen
Graphite alkene is as raw material, and since its surface is there are a large amount of oxygen groups and hydroxyl, reactivity is higher, easily and external substance
Reaction keeps material rotten;And by the way of graphite ultrasonic disperse, the graphene number of plies of preparation is more and each layer is tightly combined,
It is unfavorable for the insertion of nano-iron oxide particle.
Summary of the invention
The present invention is to solve the above problem in the prior art, proposes a kind of carbon/ferriferous oxide composite and flexible electrode material
And preparation method thereof.
To achieve the above object, the invention adopts the following technical scheme:
The first aspect of the invention is to provide a kind of preparation method of carbon/ferriferous oxide composite and flexible electrode material, will
Carbon material and ferriferous oxide are configured to dispersion liquid respectively, by polycarbonate perforated membrane after mixing, by the way of vacuum filtration
It is prepared into composite material film, then after high-temperature heat treatment to obtain the final product.
Further, in the carbon/ferriferous oxide composite and flexible electrode material preparation method, the carbon material is oxygen
Graphite alkene, the ferriferous oxide are nano ferriferrous oxide.
Further, in the carbon/ferriferous oxide composite and flexible electrode material preparation method, the nanometer four is aoxidized
The mass ratio of three-iron and graphene oxide is 0.2-1.2:1.
Further, in the carbon/ferriferous oxide composite and flexible electrode material preparation method, following step is specifically included
It is rapid:
(1) graphene oxide dispersion is prepared;
(2) preparation of nano ferroso-ferric oxide dispersion liquid;
(3) after mixing by prepared a certain concentration graphene oxide dispersion, nano ferriferrous oxide dispersion liquid,
Through polycarbonate perforated membrane in the way of vacuum filtration, by ferriferous oxide and graphene it is compound composite material film, it is multiple
The mass ratio of ferroso-ferric oxide and graphene oxide is 0.5-2:1 in condensation material film;
(4) composite material film obtained after vacuum filtration is placed in 550-700 in baking oven under nitrogen atmosphere protection
DEG C heat treatment 1-3h to get.
Further, the carbon/ferriferous oxide composite and flexible electrode material preparation method, oxygen described in step (1)
Graphite alkene dispersion liquid the preparation method is as follows: the 30mL concentrated sulfuric acid is added in dry flask and graphite powder 0.2-0.3g is added,
Flask is placed in ice-water bath, backward flask in be slowly added to potassium permanganate solid 3.5-4g, control mixeding liquid temperature in 25-
35 DEG C, flask is placed in 35 DEG C of water-baths after mixing and heats 2h;Mixed liquor is diluted in 60mL deionized water, and is sequentially added double
Oxygen water 5-10mL and hydrochloric acid 10-15mL is precipitated for solution left standstill 1-3 days later;It takes precipitating ultrasonic disperse in deionized water, utilizes
Centrifuge carries out centrifugal treating, removes supernatant after centrifugation, solid is dissolved in dilute hydrochloric acid, continue centrifugal treating, repeats
After above-mentioned steps 3-5 times, precipitating is placed in baking oven and is dried;Solid ultrasonic disperse is configured to dense in deionized water after drying
Degree is the dispersion liquid of 0.2mg/mL.
Further, the carbon/ferriferous oxide composite and flexible electrode material preparation method, step are received described in (2)
Rice ferroso-ferric oxide dispersion liquid the preparation method comprises the following steps: weighing 1-2g FeCl3·6H2O is dissolved into 40-60mL water and 60 DEG C of water-baths add
Heat takes 0.4-0.5g FeCl2·4H2Solution & stir is added in O, rapidly joins 28% ammonium hydroxide of 1-2mL later, mixed liquor is 80
DEG C heating water bath 1h;After the completion of heating, with Fe of the magnet in one jiao of solution attraction solution3O4Particle, to most of black particle
When gathering near magnet, the clear liquid on upper layer is shifted, cleans precipitating particle using deionized water;By the Fe after cleaning3O4With
The ultrasonic disperse in 80-100mL deionized water is uniform to sulfosalicylic acid potassium by 0.6-0.8g, and mixed liquor is after deionized water is washed
Moisture is filtered off, by deposition solid ultrasonic disperse in a certain amount of deionized water, is configured to the nanometer that concentration is 0.1mg/mL
Fe3O4Dispersion liquid.
Further, the carbon/ferriferous oxide composite and flexible electrode material preparation method is dried described in step (4)
Box temperature degree is 550-700 DEG C, heat treatment time 2h.
The second aspect of the invention is to provide a kind of carbon/ferriferous oxide composite and flexible electrode material of the method preparation
Material.
The present invention by adopting the above technical scheme, compared with prior art, has the following technical effect that
(1) in the composite material being prepared, nano ferriferrous oxide granule is attached in graphene sheet layer, graphene film
Buffer layer of the layer as nano ferriferrous oxide granule volume expansion, improves the cycle performance of ferroso-ferric oxide;
(2) graphene is as main body frame, excellent mechanical tenacity, so that composite material has the spy of flexible self-supporting
Property, it can be used directly as the negative electrode material of flexible battery;
(3) graphene oxide/ferriferous oxide that reduction is prepared by the way of filtering by polycarbonate porous vacuum is multiple
Condensation material film, preparation process simple economy, operation is convenient, is easy to be mass produced;
(4) after composite material filters film forming, high temperature thermal reduction has been carried out, the active group of surface of graphene oxide is effectively reduced
The graphene oxide that group is restored, so that composite properties are more stable.
Figure of description
Fig. 1 is graphene oxide section SEM figure;
Fig. 2 is graphene/ferriferrous oxide composite material section SEM figure;
Fig. 3 is Fe3O4And Fe3O4/ rGO composite material is in 100mA g-1Under cycle performance curve graph.
Specific embodiment
The present invention is described in more detail below by specific embodiment, for a better understanding of the present invention,
But following embodiments are not intended to limit the scope of the invention.
Embodiment 1
The nanometer four that the graphene oxide dispersion and concentration that compound concentration is 0.2mg/mL respectively are 0.1mg/mL aoxidizes
Three-iron dispersion liquid measures two kinds of dispersion liquids of certain volume respectively, makes ferroso-ferric oxide dispersion liquid and graphene oxide dispersion
Volume ratio be 2:1, after mixed liquor magnetic agitation 20min, be filtered by vacuum by polycarbonate perforated membrane, in polycarbonate
Graphene oxide/nano ferriferrous oxide laminated film is self-assembled on perforated membrane.The film being prepared into is 600 in nitrogen atmosphere
After DEG C heat treatment 2h, carbon/ferriferous oxide composite and flexible electrode material is obtained, then with lithium piece be to electrode assembling into 2025 buttons electricity
Pond.Test result shows battery by 50 circulations, and capacity is still able to maintain in 681.2mAh*g-1。
Embodiment 2
The nanometer four that the graphene oxide dispersion and concentration that compound concentration is 0.2mg/mL respectively are 0.1mg/mL aoxidizes
Three-iron dispersion liquid measures two kinds of dispersion liquids of certain volume respectively, makes ferroso-ferric oxide dispersion liquid and graphene oxide dispersion
Volume ratio be 1:1, after mixed liquor magnetic agitation 20min, be filtered by vacuum by polycarbonate perforated membrane, in polycarbonate
Graphene oxide/nano ferriferrous oxide laminated film is self-assembled on perforated membrane.The film being prepared into is 600 in nitrogen atmosphere
After DEG C heat treatment 2h, carbon/ferriferous oxide composite and flexible electrode material is obtained, then with lithium piece be to electrode assembling into 2025 buttons electricity
Pond.Test result shows battery by 50 circulations, and capacity is still able to maintain in 324.1mAh*g-1。
Embodiment 3
The nanometer four that the graphene oxide dispersion and concentration that compound concentration is 0.2mg/mL respectively are 0.1mg/mL aoxidizes
Three-iron dispersion liquid measures two kinds of dispersion liquids of certain volume respectively, makes ferroso-ferric oxide dispersion liquid and graphene oxide dispersion
Volume ratio be 4:1, after mixed liquor magnetic agitation 20min, be filtered by vacuum by polycarbonate perforated membrane, in polycarbonate
Graphene oxide/nano ferriferrous oxide laminated film is self-assembled on perforated membrane.The film being prepared into is 600 in nitrogen atmosphere
After DEG C heat treatment 2h, carbon/ferriferous oxide composite and flexible electrode material is obtained, then with lithium piece be to electrode assembling into 2025 buttons electricity
Pond.Test result shows battery by 50 circulations, and capacity is still able to maintain in 442.6mAh*g-1。
Embodiment 4
The nanometer four that the graphene oxide dispersion and concentration that compound concentration is 0.2mg/mL respectively are 0.1mg/mL aoxidizes
Three-iron dispersion liquid measures two kinds of dispersion liquids of certain volume respectively, makes ferroso-ferric oxide dispersion liquid and graphene oxide dispersion
Volume ratio be 1:1, after mixed liquor magnetic agitation 20min, be filtered by vacuum by polycarbonate perforated membrane, in polycarbonate
Graphene oxide/nano ferriferrous oxide laminated film is self-assembled on perforated membrane.The film being prepared into is 550 in nitrogen atmosphere
After DEG C heat treatment 2h, carbon/ferriferous oxide composite and flexible electrode material is obtained, then with lithium piece be to electrode assembling into 2025 buttons electricity
Pond.Test result shows battery by 50 circulations, and capacity is still able to maintain in 681.2mAh*g-1。
Embodiment 5
The nanometer four that the graphene oxide dispersion and concentration that compound concentration is 0.2mg/mL respectively are 0.1mg/mL aoxidizes
Three-iron dispersion liquid measures two kinds of dispersion liquids of certain volume respectively, makes ferroso-ferric oxide dispersion liquid and graphene oxide dispersion
Volume ratio be 1:1, after mixed liquor magnetic agitation 20min, be filtered by vacuum by polycarbonate perforated membrane, in polycarbonate
Graphene oxide/nano ferriferrous oxide laminated film is self-assembled on perforated membrane.The film being prepared into is 700 in nitrogen atmosphere
After DEG C heat treatment 2h, carbon/ferriferous oxide composite and flexible electrode material is obtained, then with lithium piece be to electrode assembling into 2025 buttons electricity
Pond.Test result shows battery by 50 circulations, and capacity is maintained at 554.3mAh*g-1。
Comparative example:
Unlike above-described embodiment 1, using the nano ferriferrous oxide of non-composite graphite alkene as electrode material, then with lithium
Piece is to electrode assembling into 2025 button cells.Test result shows battery by 50 circulations, and capacity is only 222.0mAh*
g-1。
Performance test
Fig. 1 and Fig. 2 is graphene section electron microscope and graphene/ferriferrous oxide composite material section electron microscope;Fig. 3 is
The cycle performance test result of different proportion composite material.
Its cycle performance of the group button cell of above-described embodiment 1-5 preparation is compared as follows shown in table 1:
1 Fe of table3O4And Fe3O4/ rGO composite material is in 100mA g-1Under cycle performance compare
Serial number | Sample | Capacity residue/mAh*g after circulation 50 times-1 |
Comparative example | Fe3O4 | 222.0 |
Embodiment 1 | Fe3O4: GO=1:1 | 681.2 |
Embodiment 2 | Fe3O4: GO=1:2 | 324.1 |
Embodiment 3 | Fe3O4: GO=2:1 | 442.6 |
Embodiment 4 | Fe3O4: GO=1:2 | 681.2 |
Embodiment 5 | Fe3O4: GO=1:2 | 554.3 |
Specific embodiments of the present invention are described in detail above, but it is merely an example, the present invention is simultaneously unlimited
It is formed on particular embodiments described above.To those skilled in the art, any couple of present invention carries out equivalent modifications and
Substitution is also all among scope of the invention.Therefore, without departing from the spirit and scope of the invention made by equal transformation and
Modification, all should be contained within the scope of the invention.
Claims (8)
1. a kind of carbon/ferriferous oxide composite and flexible electrode material preparation method, which is characterized in that by carbon material and ferriferous oxide
It is configured to dispersion liquid respectively, by polycarbonate perforated membrane after mixing, it is thin that composite material is prepared by the way of vacuum filtration
Film, then after high-temperature heat treatment to obtain the final product.
2. carbon according to claim 1/ferriferous oxide composite and flexible electrode material preparation method, which is characterized in that institute
Stating carbon material is graphene oxide, and the ferriferous oxide is nano ferriferrous oxide.
3. carbon according to claim 2/ferriferous oxide composite and flexible electrode material preparation method, which is characterized in that institute
The mass ratio for stating nano ferriferrous oxide and graphene oxide is 0.2-1.2:1.
4. carbon according to claim 1/ferriferous oxide composite and flexible electrode material preparation method, which is characterized in that packet
Include following steps:
(1) graphene oxide dispersion is prepared;
(2) preparation of nano ferroso-ferric oxide dispersion liquid;
(3) after mixing by prepared a certain concentration graphene oxide dispersion, nano ferriferrous oxide dispersion liquid, pass through
Polycarbonate perforated membrane, in the way of vacuum filtration, by ferriferous oxide and graphene it is compound composite material film, composite wood
Expect that the mass ratio of nano ferriferrous oxide and graphene oxide is 0.5-2:1 in film;
(4) composite material film obtained after vacuum filtration is placed in 550-700 DEG C of heat in baking oven under nitrogen atmosphere protection
Handle 1-3h to get.
5. carbon according to claim 4/ferriferous oxide composite and flexible electrode material preparation method, which is characterized in that step
Suddenly graphene oxide dispersion described in (1) the preparation method is as follows: the 30mL concentrated sulfuric acid is added in dry flask and stone is added
Ink powder 0.2-0.3g, flask is placed in ice-water bath, backward flask in be slowly added to potassium permanganate solid 3.5-4g, control is mixed
Flask is placed in 35 DEG C of water-baths by conjunction liquid temperature after 25-35 DEG C, mixing heats 2h;Mixed liquor is diluted in 60mL deionized water
In, and hydrogen peroxide 5-10mL and hydrochloric acid 10-15mL are sequentially added, it precipitates within solution left standstill 1-3 days later;Take precipitating ultrasonic disperse in
In deionized water, centrifugal treating is carried out using centrifuge, supernatant liquor is removed after centrifugation, solid is dissolved in dilute hydrochloric acid, is continued
Centrifugal treating is carried out, after repeating the above steps 3-5 times, precipitating is placed in baking oven and is dried;Solid ultrasonic disperse is in going after drying
In ionized water, it is configured to the dispersion liquid that concentration is 0.2mg/mL.
6. carbon according to claim 4/ferriferous oxide composite and flexible electrode material preparation method, which is characterized in that step
Suddenly nano ferriferrous oxide dispersion liquid described in (2) the preparation method comprises the following steps: weighing 1-2g FeCl3·6H2O is dissolved into 40-60mL
In water and 60 DEG C of heating water baths, 0.4-0.5g FeCl is taken2·4H2Solution & stir is added in O, rapidly joins 1-2mL 28% later
Ammonium hydroxide, mixed liquor is in 80 DEG C of heating water bath 1h;After the completion of heating, with Fe of the magnet in one jiao of solution attraction solution3O4Particle,
When most of black particle gathers near magnet, the clear liquid on upper layer is shifted, cleans precipitating particle using deionized water;It will
Fe after cleaning3O4To sulfosalicylic acid potassium, the ultrasonic disperse in 80-100mL deionized water is uniform with 0.6-0.8g, mixed liquor warp
Moisture is filtered off after deionized water washing, by deposition solid ultrasonic disperse in a certain amount of deionized water, being configured to concentration is
The nanometer Fe of 0.1mg/mL3O4Dispersion liquid.
7. carbon according to claim 4/ferriferous oxide composite and flexible electrode material preparation method, which is characterized in that step
Suddenly oven temperature described in (4) is 550-700 DEG C, heat treatment time 2h.
8. a kind of carbon/ferriferous oxide composite and flexible electrode material prepared such as any one of claim 1-7 the method.
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Application publication date: 20190607 |