CN109473635A - A kind of graphene composite material and preparation method thereof - Google Patents
A kind of graphene composite material and preparation method thereof Download PDFInfo
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- CN109473635A CN109473635A CN201710803881.4A CN201710803881A CN109473635A CN 109473635 A CN109473635 A CN 109473635A CN 201710803881 A CN201710803881 A CN 201710803881A CN 109473635 A CN109473635 A CN 109473635A
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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
- H01M4/362—Composites
- H01M4/364—Composites as mixtures
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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
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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
- H01M4/50—Selection of substances as active materials, active masses, active liquids of inorganic oxides or hydroxides of manganese
- H01M4/505—Selection of substances as active materials, active masses, active liquids of inorganic oxides or hydroxides of manganese of mixed oxides or hydroxides containing manganese for inserting or intercalating light metals, e.g. LiMn2O4 or LiMn2OxFy
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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
- H01M4/62—Selection of inactive substances as ingredients for active masses, e.g. binders, fillers
- H01M4/624—Electric conductive fillers
- H01M4/625—Carbon or graphite
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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
- Y02E60/10—Energy storage using batteries
Abstract
The invention discloses a kind of graphene composite material and preparation method thereof, the preparation of composite material includes synthesis and the MnO of graphene oxide2‑Cr2O3Graphene composite material prepares the two steps.Composite material provided by the invention has excellent high rate performance and excellent cycle performance, even if recycled material is also able to maintain good structural stability under high current.These advantages of composite material of the present invention may be related with the weight ratio of sodium metasilicate in preparation method and sodium lauryl sulfate, when the weight ratio of the two is 2-5:1, prepared composite material best performance.
Description
Technical field
The invention belongs to field of new materials, are related to graphene battery material, and in particular to MnO2-Cr2O3Graphene is compound
The preparation of material and the application in clang ion battery cathode.
Background technique
Mn oxide due to its abundant raw material, cheap and advantages of environment protection, be widely used in supercapacitor,
In the energy storages such as clang ion battery electrode materials, fuel cell and conversion equipment.Wherein, MnO has height due to stable structure
Up to the theoretical specific capacity of 755mAh/g, it is widely studied as clang ion battery cathode.But with other transition metal oxides
Similar, MnO electronic conductivity is lower, thus high rate performance is poor.Meanwhile during conversion reaction, MnO shows biggish body
Product expansion, causes active material to fall off in charge and discharge process from collector, capacity is decayed rapidly.
In general, the nano particle of transition metal oxide is loaded to such as graphite of the carbon material with highly electron conductive
On the skeletons such as alkene, carbon nanotube, the electronic conductivity of material can be effectively improved, to improve the high rate performance of material.But
It is that, even if transition metal oxide nano particulate load is on the carbon material, volume expansion can not be improved well, greatly
Electric current and compared under the long circulating period, still shows obvious capacity attenuation.
Summary of the invention
The purpose of the present invention is to overcome the above shortcomings and to provide a kind of MnO2-Cr2O3Graphene composite material, with drop
Low volume expansion reduces high current and compared with the capacity attenuation under the long circulating period.
Above-mentioned purpose of the invention is achieved by following technical solution:
A kind of MnO2-Cr2O3The preparation method of graphene composite material, includes the following steps:
Step (1), the synthesis of graphene oxide: taking 1g expanded graphite to be stirred with the 80mL concentrated sulfuric acid, and 1g nitric acid is added
Sodium, and it is slowly added to the mixture of 5g sodium metasilicate and sodium lauryl sulfate, it is stirred overnight;Remove the unreacted of solution upper layer floating
Expanded graphite, will be stirred in the mixed solution ultrapure water of falling 250mL, after beaker is cooling, 15mL mass fraction be added
30% hydrogen peroxide obtains the graphene oxide solution of glassy yellow;It is centrifuged and uses milli-Q water 3-5 times, obtain the oxygen of brown color
Graphite alkene colloidal sol;Wherein, the weight ratio of the sodium metasilicate and sodium lauryl sulfate is 3-5:1.
(1) step (2), MnO2-Cr2O3The preparation of graphene composite material: 1g polyethylene oxide-polypropylene oxide-is taken
Polyethylene oxide triblock copolymer P123 is dissolved in 150mL water, is vigorously stirred to after generating a large amount of foams, 2g step is added
(1) obtained oxide yellow graphene solution is transferred in 85 DEG C of water-baths then by the graphene oxide colloidal sol prepared after stirring 1h,
Manganese nitrate solution and 5g sodium metasilicate that 5mL mass fraction is 45% are added into graphene oxide solution to add after reacting 15min
Enter 1g pyrroles, obtains presoma through suction filtration, washing, drying after reacting in the 85 DEG C of water-baths of the above mixture;Presoma is transferred to nitrogen
In gas atmosphere tube type furnace, 800 DEG C of calcination 3h to get arrive final product.
Further, the MnO2-Cr2O3The preparation method of graphene composite material, it is characterised in that: step (1)
In, the weight ratio 3:1 of the sodium metasilicate and sodium lauryl sulfate.
The MnO2-Cr2O3Graphene composite material is preparing the application in negative electrode of lithium ion battery.
Advantages of the present invention: MnO provided by the invention2-Cr2O3Graphene composite material is negative as clang ion battery
Pole shows good high rate performance, can reduce volume expansion, reduces high current and declines compared with the capacity under the long circulating period
Subtract.
Specific embodiment
Next combining some specific implementation cases, the present invention is further elaborated, but claim of the invention is not only
It is limited only to following examples.
Embodiment 1
A kind of MnO2-Cr2O3The preparation method of graphene composite material, includes the following steps:
(1) synthesis of graphene oxide: taking 1g expanded graphite to be stirred with the 80mL concentrated sulfuric acid, and 1g sodium nitrate is added, and
It is slowly added to the mixture of 5g sodium metasilicate and sodium lauryl sulfate, is stirred overnight;Remove the unreacted swollen of solution upper layer floating
Swollen graphite will stir in the mixed solution ultrapure water of falling 250mL, after beaker is cooling, be added 30% pair that 15mL mass fraction is
Oxygen water obtains the graphene oxide solution of glassy yellow;It is centrifuged and uses milli-Q water 3-5 times, obtain the graphite oxide of brown color
Alkene colloidal sol;Wherein, the weight ratio of the sodium metasilicate and sodium lauryl sulfate is 3:1.
(2)MnO2-Cr2O3The preparation of graphene composite material: 1g polyethylene oxide-polypropylene oxide-polycyclic oxygen second is taken
Alkane triblock copolymer P123 is dissolved in 150mL water, is vigorously stirred to after generating a large amount of foams, and 2g step (1) preparation is added
Obtained oxide yellow graphene solution is transferred in 85 DEG C of water-baths then, to oxidation stone by graphene oxide colloidal sol after stirring 1h
The manganese nitrate solution and 5g sodium metasilicate that 5mL mass fraction is 45% are added in black alkene solution, after reacting 15min, 1g pyrroles is added,
Presoma is obtained through suction filtration, washing, drying after reacting in the 85 DEG C of water-baths of the above mixture;Presoma is transferred to nitrogen atmosphere tubular type
In furnace, 800 DEG C of calcination 3h to get arrive final product.
Embodiment 2
A kind of MnO2-Cr2O3The preparation method of graphene composite material, includes the following steps:
(1) synthesis of graphene oxide: taking 1g expanded graphite to be stirred with the 80mL concentrated sulfuric acid, and 1g sodium nitrate is added, and
It is slowly added to the mixture of 5g sodium metasilicate and sodium lauryl sulfate, is stirred overnight;Remove the unreacted swollen of solution upper layer floating
Swollen graphite will stir in the mixed solution ultrapure water of falling 250mL, after beaker is cooling, be added 30% pair that 15mL mass fraction is
Oxygen water obtains the graphene oxide solution of glassy yellow;It is centrifuged and uses milli-Q water 3-5 times, obtain the graphite oxide of brown color
Alkene colloidal sol;Wherein, the weight ratio of the sodium metasilicate and sodium lauryl sulfate is 4:1.
(2)MnO2-Cr2O3The preparation of graphene composite material: 1g polyethylene oxide-polypropylene oxide-polycyclic oxygen second is taken
Alkane triblock copolymer P123 is dissolved in 150mL water, is vigorously stirred to after generating a large amount of foams, and 2g step (1) preparation is added
Obtained oxide yellow graphene solution is transferred in 85 DEG C of water-baths then, to oxidation stone by graphene oxide colloidal sol after stirring 1h
The manganese nitrate solution and 5g sodium metasilicate that 5mL mass fraction is 45% are added in black alkene solution, after reacting 15min, 1g pyrroles is added,
Presoma is obtained through suction filtration, washing, drying after reacting in the 85 DEG C of water-baths of the above mixture;Presoma is transferred to nitrogen atmosphere tubular type
In furnace, 800 DEG C of calcination 3h to get arrive final product.
Embodiment 3
A kind of MnO2-Cr2O3The preparation method of graphene composite material, includes the following steps:
(1) synthesis of graphene oxide: taking 1g expanded graphite to be stirred with the 80mL concentrated sulfuric acid, and 1g sodium nitrate is added, and
It is slowly added to the mixture of 5g sodium metasilicate and sodium lauryl sulfate, is stirred overnight;Remove the unreacted swollen of solution upper layer floating
Swollen graphite will stir in the mixed solution ultrapure water of falling 250mL, after beaker is cooling, be added 30% pair that 15mL mass fraction is
Oxygen water obtains the graphene oxide solution of glassy yellow;It is centrifuged and uses milli-Q water 3-5 times, obtain the graphite oxide of brown color
Alkene colloidal sol;Wherein, the weight ratio of the sodium metasilicate and sodium lauryl sulfate is 5:1.
(2)MnO2-Cr2O3The preparation of graphene composite material: 1g polyethylene oxide-polypropylene oxide-polycyclic oxygen second is taken
Alkane triblock copolymer P123 is dissolved in 150mL water, is vigorously stirred to after generating a large amount of foams, and 2g step (1) preparation is added
Obtained oxide yellow graphene solution is transferred in 85 DEG C of water-baths then, to oxidation stone by graphene oxide colloidal sol after stirring 1h
The manganese nitrate solution and 5g sodium metasilicate that 5mL mass fraction is 45% are added in black alkene solution, after reacting 15min, 1g pyrroles is added,
Presoma is obtained through suction filtration, washing, drying after reacting in the 85 DEG C of water-baths of the above mixture;Presoma is transferred to nitrogen atmosphere tubular type
In furnace, 800 DEG C of calcination 3h to get arrive final product.
Embodiment 4
A kind of MnO2-Cr2O3The preparation method of graphene composite material, includes the following steps:
(1) synthesis of graphene oxide: taking 1g expanded graphite to be stirred with the 80mL concentrated sulfuric acid, and 1g sodium nitrate is added, and
It is slowly added to the mixture of 5g sodium metasilicate and sodium lauryl sulfate, is stirred overnight;Remove the unreacted swollen of solution upper layer floating
Swollen graphite will stir in the mixed solution ultrapure water of falling 250mL, after beaker is cooling, be added 30% pair that 15mL mass fraction is
Oxygen water obtains the graphene oxide solution of glassy yellow;It is centrifuged and uses milli-Q water 3-5 times, obtain the graphite oxide of brown color
Alkene colloidal sol;Wherein, the weight ratio of the sodium metasilicate and sodium lauryl sulfate is 6:1.
(2)MnO2-Cr2O3The preparation of graphene composite material: 1g polyethylene oxide-polypropylene oxide-polycyclic oxygen second is taken
Alkane triblock copolymer P123 is dissolved in 150mL water, is vigorously stirred to after generating a large amount of foams, and 2g step (1) preparation is added
Obtained oxide yellow graphene solution is transferred in 85 DEG C of water-baths then, to oxidation stone by graphene oxide colloidal sol after stirring 1h
The manganese nitrate solution and 5g sodium metasilicate that 5mL mass fraction is 45% are added in black alkene solution, after reacting 15min, 1g pyrroles is added,
Presoma is obtained through suction filtration, washing, drying after reacting in the 85 DEG C of water-baths of the above mixture;Presoma is transferred to nitrogen atmosphere tubular type
In furnace, 800 DEG C of calcination 3h to get arrive final product.
Embodiment 5
Respectively under different current densities and measurement embodiment 1-3 prepare composite material first circle reversible capacity,
Capacity after 50 circle of 10 circle of circulation and circulation, as a result see the table below:
Upper table explanation, with the increase of current density, capacity reduced for the composite material of embodiment 1-3 preparation, but
Still there is higher conservation rate, and coulombic efficiency is close to 100%, the composite material prepared better than embodiment 4.And embodiment
The composite material of 1-3 preparation is after 50 circle of 10A/g circulation, when current density is recalled to again to 0.5A/g, charge and discharge capacitor
Amount remains to restore to 900 or so, illustrates that composite material still keeps good stable structure after high current charge-discharge
Property.
Pass through the above experimental result, it can be appreciated that composite material provided by the invention has excellent high rate performance and excellent
Different cycle performance, even if recycled material is also able to maintain good structural stability under high current.Composite material of the present invention
These advantages may be related with the weight ratio of sodium metasilicate in preparation method and sodium lauryl sulfate, the parts by weight of the two it
When than for 3-5:1, prepared composite material best performance.
The effect of above-described embodiment indicates that essentiality content of the invention, but protection of the invention is not limited with this
Range.Those skilled in the art should understand that can with modification or equivalent replacement of the technical solution of the present invention are made,
Without departing from the essence and protection scope of technical solution of the present invention.
Claims (3)
1. a kind of graphene composite material and preparation method thereof, which comprises the steps of:
(1) synthesis of graphene oxide: taking 1g expanded graphite to be stirred with the 80mL concentrated sulfuric acid, 1g sodium nitrate is added, and slowly
The mixture of 5g sodium metasilicate and sodium lauryl sulfate is added, is stirred overnight;Remove the unreacted expansion stone of solution upper layer floating
Ink will stir in the mixed solution ultrapure water of falling 250mL, and after beaker is cooling, 30% hydrogen peroxide that 15mL mass fraction is is added,
Obtain the graphene oxide solution of glassy yellow;It is centrifuged and uses milli-Q water 3-5 times, the graphene oxide for obtaining brown color is molten
Glue;Wherein, the weight ratio of the sodium metasilicate and sodium lauryl sulfate is 3-5:1.
(2)MnO2-Cr2O3The preparation of graphene composite material: 1g polyethylene oxide-polypropylene oxide-polyethylene oxide three is taken
Block copolymer P123 is dissolved in 150mL water, is vigorously stirred to after generating a large amount of foams, the oxidation of 2g step (1) preparation is added
Obtained oxide yellow graphene solution is transferred in 85 DEG C of water-baths then, to graphene oxide by graphene sol after stirring 1h
The manganese nitrate solution and 5g sodium metasilicate that 5mL mass fraction is 45% are added in solution, after reacting 15min, 1g pyrroles is added, it is above
Presoma is obtained through suction filtration, washing, drying after reacting in 85 DEG C of water-baths of mixture;Presoma is transferred to nitrogen atmosphere tube furnace
In, 800 DEG C of calcination 3h to get arrive final product.
2. MnO according to claim 12-Cr2O3The preparation method of graphene composite material, it is characterised in that: step
(1) in, the weight ratio 3:1 of the sodium metasilicate and sodium lauryl sulfate.
3. MnO of any of claims 1 or 22-Cr2O3Graphene composite material is preparing the application in negative electrode of lithium ion battery.
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Cited By (1)
Publication number | Priority date | Publication date | Assignee | Title |
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CN111725528A (en) * | 2020-06-03 | 2020-09-29 | 上海交通大学 | Manganese dioxide composite porous graphene cathode catalyst and preparation method and application thereof |
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CN102185143A (en) * | 2011-04-02 | 2011-09-14 | 浙江大学 | Transition metal oxide/ graphene composite material and preparation method thereof |
CN105762361A (en) * | 2016-05-04 | 2016-07-13 | 刘高志 | Novel graphene composite material and preparation method thereof |
CN105810917A (en) * | 2016-05-24 | 2016-07-27 | 刘高志 | Preparation of SnO2-Cr2O3-graphene composite and application thereof in negative electrode of lithium ion cell |
CN105826529A (en) * | 2016-03-22 | 2016-08-03 | 陈波 | Preparation of MnO-Cr2O3-graphene composite and application of MnO-Cr2O3-graphene composite in lithium ion battery negative electrodes |
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Patent Citations (6)
Publication number | Priority date | Publication date | Assignee | Title |
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US20110033746A1 (en) * | 2009-08-10 | 2011-02-10 | Jun Liu | Self assembled multi-layer nanocomposite of graphene and metal oxide materials |
CN102173414A (en) * | 2011-03-18 | 2011-09-07 | 中国地质大学(武汉) | Method for preparing graphene oxide by chemical peeling |
CN102185143A (en) * | 2011-04-02 | 2011-09-14 | 浙江大学 | Transition metal oxide/ graphene composite material and preparation method thereof |
CN105826529A (en) * | 2016-03-22 | 2016-08-03 | 陈波 | Preparation of MnO-Cr2O3-graphene composite and application of MnO-Cr2O3-graphene composite in lithium ion battery negative electrodes |
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