CN108807882A - A kind of Fe with porous octahedral structure2O3/Fe3O4The preparation method of@C/G composite materials - Google Patents
A kind of Fe with porous octahedral structure2O3/Fe3O4The preparation method of@C/G composite materials Download PDFInfo
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- CN108807882A CN108807882A CN201810504416.5A CN201810504416A CN108807882A CN 108807882 A CN108807882 A CN 108807882A CN 201810504416 A CN201810504416 A CN 201810504416A CN 108807882 A CN108807882 A CN 108807882A
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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
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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
- H01M4/525—Selection of substances as active materials, active masses, active liquids of inorganic oxides or hydroxides of nickel, cobalt or iron of mixed oxides or hydroxides containing iron, cobalt or nickel for inserting or intercalating light metals, e.g. LiNiO2, LiCoO2 or LiCoOxFy
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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 methods burnt using triethylamine (TEA) to prepare the Fe with porous octahedral structure2O3/Fe3O4@carbon/graphene(Fe2O3/Fe3O4@C/G) composite material.A kind of metal organic frame (Fe-MOF) is used equably to be supported on graphene oxide it for presoma, then lighted with TEA, Fe-MOF is used as from sacrificing template generation Fe2O3/Fe3O4Nano particle, and graphene oxide is reduced to graphene, to obtain Fe2O3/Fe3O4@C/G composite materials.The method that metal oxide and graphene composite material are prepared by way of tube-type atmosphere furnace calcining that this method routine different from the past was reported.Fe made from this method2O3/Fe3O4@C/G composite materials have porous octahedral structure, and this method preparation process is simple and quick, is conducive to the energy saving and time, the porous Fe of preparation2O3/Fe3O4There is@C/G composite materials larger porosity and good electric conductivity, the negative material as lithium ion battery to show preferable feature performance benefit.
Description
Technical field
The Fe with porous octahedral structure is prepared the present invention relates to a kind of2O3/Fe3O4The method of@C/G composite materials belongs to
In technical field of material chemistry.
Background technology
Negative material of the transition metal oxide due to being widely used as lithium ion battery with high theoretical capacity.
But applying for it is limited by big volume expansion and low electric conductivity in charge and discharge process.
Invention content
Capacity attenuation is too fast when in order to solve the problems, such as INVENTIONConventional metal-oxide as lithium ion battery negative material, this hair
It is bright that be designed to provide a kind of metal oxide of the porous octahedral structure formed based on metal organic frame compound
The preparation method of material.
Realize technical scheme of the present invention：
The present invention is used using the uniform carried metal organic framework material Fe-MOF of graphene oxide as the base of presoma
The Fe with porous octahedral structure is prepared for by the method that unique triethylamine burns on plinth2O3/Fe3O4@C/G composite woods
Material.
A kind of Fe2O3/Fe3O4The preparation method of@C/G composite materials, includes the following steps：
(1) graphene oxide (GO) is prepared by improved Hummers methods, graphene oxide obtained is placed in N, N bis-
In methylformamide (DMF), ultrasound a period of time；
(2) ferric chloride hexahydrate is added in above-mentioned solution, stirring and dissolving adds terephthalic acid (TPA), after stirring
3~5h is reacted under the conditions of 110~130 DEG C；After being cooled to room temperature, n,N dimethylformamide, three times water washing, vacuum are used successively
It is dry, obtain forerunner Fe-MOF/GO；
(3) above-mentioned Fe-MOF/GO is taken, triethylamine (TEA) is added, lights, it is dry after its completely burned, finally obtain
Obtain Fe2O3/Fe3O4@C/G composite materials.
Preferably, in step (1), the ultrasonic time is 30min.
Preferably, in step (3), drying carries out at being 60 DEG C in temperature.
By above-mentioned processing mode, it is successfully prepared the Fe with porous octahedral structure2O3/Fe3O4@C/G composite woods
Material, octahedral size is about 800nm, and porous form is presented, and has larger porosity.
The solution have the advantages that：The method for comparing the synthesizing graphite alkene based composites having been reported that, this method
Advantage is that synthetic method is simple, can realize Fast back-projection algorithm, saves time and the energy.What is prepared has porous octahedral structure
Fe2O3/Fe3O4@C/G composite materials have larger porosity, larger specific surface, the cathode material as lithium ion battery
The advantages that material illustrates preferable performance.This method not only has the synthetic method for preparing the metal oxide materials based on MOF
There is directive significance, a frontier has been opened up in the also development for high performance lithium ion battery, is had great significance.
Description of the drawings
Fig. 1 is the Fe with porous octahedral structure2O3/Fe3O4The scanning electron microscope diagram of@C/G composite materials.
Fig. 2 is the Fe with porous octahedral structure2O3/Fe3O4The X-ray diffractogram of@C/G composite materials.
Specific implementation mode
Embodiment 1
It first passes through improved Hummers methods and prepares graphene oxide (GO), graphene oxide obtained (10mg) is placed in
In 15mL n,N dimethylformamide (DMF), ultrasonic 30min.0.08g ferric chloride hexahydrates, stirring are added in above-mentioned solution
Dissolving adds 0.05g terephthalic acid (TPA)s, is transferred them in 50mL flasks after stirring a hour, 110 DEG C of oil bath 3h；It is cold
But to after room temperature, DMF, three times water washing are used successively, is put into freeze drier and is dried in vacuo, obtain forerunner Fe-MOF/GO.It takes
25mg Fe-MOF/GO are added 0.5mL TEA, light in surface plate, after its completely burned, are put into baking oven, 60 DEG C of dryings,
Finally obtain Fe2O3/Fe3O4@C/G composite materials.
Embodiment 2
It first passes through improved Hummers methods and prepares graphene oxide (GO), graphene oxide obtained (15mg) is placed in
In 15mL n,N dimethylformamide (DMF), ultrasonic 30min.0.15g ferric chloride hexahydrates, stirring are added in above-mentioned solution
Dissolving adds 0.1g terephthalic acid (TPA)s, is transferred them in 50mL flasks after stirring a hour, 120 DEG C of oil bath 4h；It is cooling
To room temperature, DMF, three times water washing are used successively, is put into freeze drier and is dried in vacuo, obtain forerunner Fe-MOF/GO.It takes
25mg Fe-MOF/GO are added 1.0mL TEA, light in surface plate, after its completely burned, are put into baking oven, 60 DEG C of dryings,
Finally obtain Fe2O3/Fe3O4@C/G composite materials.
Embodiment 3
It first passes through improved Hummers methods and prepares graphene oxide (GO), graphene oxide obtained (15mg) is placed in
In 15mL n,N dimethylformamide (DMF), ultrasonic 30min.0.3g ferric chloride hexahydrates are added in above-mentioned solution, stirring is molten
Solution adds 0.2g terephthalic acid (TPA)s, is transferred them in 50mL flasks after stirring a hour, 130 DEG C of oil bath 4h；It is cooled to
After room temperature, DMF, three times water washing are used successively, is put into freeze drier and is dried in vacuo, obtain forerunner Fe-MOF/GO.Take 25mg
Fe-MOF/GO is added 1.5mL TEA, lights in surface plate, after its completely burned, is put into baking oven, 60 DEG C of dryings, finally
Obtain Fe2O3/Fe3O4@C/G composite materials.
Embodiment 4
It first passes through improved Hummers and prepares graphene oxide (GO), graphene oxide obtained (20mg) is placed in
In 15mL n,N dimethylformamide (DMF), ultrasonic 30min.0.3g ferric chloride hexahydrates are added in above-mentioned solution, stirring is molten
Solution adds 0.2g terephthalic acid (TPA)s, is transferred them in 50mL flasks after stirring a hour, 125 DEG C of oil bath 5h；It is cooled to
After room temperature, DMF, three times water washing are used successively, is put into freeze drier and is dried in vacuo, obtain forerunner Fe-MOF/GO.Take 25mg
Fe-MOF/GO is added 2.0mL TEA, lights in surface plate, after its completely burned, is put into baking oven, 60 DEG C of dryings, finally
Obtain Fe2O3/Fe3O4@C/G composite materials.
In conclusion the method burnt using unique triethylamine, can convert presoma to metal oxide, simultaneously
Again can redox graphene, on the surface of graphene on obtain that there is the equally distributed composite porous of octahedral structure.
This method and the prior art are the difference is that directly prepare Fe-MOF/GO presomas by one kettle way, then pass through triethylamine
Burning, and different from traditional method for calcinating of tube-type atmosphere furnace, the quick and easy Fe for being prepared for that there is porous structure2O3/
Fe3O4@C/G composite materials.As the negative material of lithium ion battery, still there is capacity after 200 circles are recycled under current density
1209.7mAh g-1, there is excellent cyclical stability.
The transition metal oxide prepared based on metal-organic framework material has larger porosity, more activity
The advantages that site, self supporting structure and be widely used.Graphene has big specific surface and good electrical conductance, therefore often
Frequently as a kind of excellent base material.Therefore, when metal organic frame is carried on graphene, and pass through unique three second
The burning of amine, had finally not only generated the oxide of iron, but also increased the electric conductivity of graphene, and the porous octahedron of formation is uniformly
Ground is supported on graphene, is provided not only the conductive frame of an interconnection, can be improved the transmission rate of electronics, also have
Conducive to the volume expansion of oxide is alleviated, the cyclical stability of lithium ion battery charge and discharge is maintained.
Claims (5)
1. a kind of Fe2O3/Fe3O4The preparation method of@C/G composite materials, includes the following steps：
(1) graphene oxide is prepared by improved Hummers methods, graphene oxide obtained is placed in N, N dimethyl formyl
In amine, ultrasound a period of time；
(2) ferric chloride hexahydrate is added in above-mentioned solution, stirring and dissolving adds terephthalic acid (TPA), after stirring 110~
3~5h is reacted under the conditions of 130 DEG C；After being cooled to room temperature, n,N dimethylformamide, three times water washing are used successively, are dried in vacuo,
Obtain forerunner Fe-MOF/GO；
(3) above-mentioned Fe-MOF/GO is taken, triethylamine is added, lights, it is dry after its completely burned, finally obtain Fe2O3/
Fe3O4@C/G composite materials.
2. according to the method described in claim 1, it is characterized in that：In step (1), the ultrasonic time is 30min.
3. according to the method described in claim 1, it is characterized in that：In step (3), drying carries out at being 60 DEG C in temperature.
4. the Fe that the method according to claims 1 to 3 any claim obtains2O3/Fe3O4@C/G composite materials.
5. Fe according to claim 42O3/Fe3O4Application of the@C/G composite materials in lithium ion battery.
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Cited By (5)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN109573988A (en) * | 2018-12-14 | 2019-04-05 | 东华大学 | A kind of graphene composite aerogel absorbing material and its preparation method and application |
| CN109806912A (en) * | 2019-03-11 | 2019-05-28 | 山西大学 | Can magnetic recycling Nd complex/GO/Fe3O4Ternary complex and its preparation method and application |
| CN109935818A (en) * | 2019-03-28 | 2019-06-25 | 中南大学 | A kind of ferroso-ferric oxide/rGO nanometer anode material and preparation method thereof |
| CN110012656A (en) * | 2019-05-05 | 2019-07-12 | 安徽理工大学 | A kind of preparation method of the derivative ferroso-ferric oxide@carbon/nano combined absorbing material of redox graphene of metal-organic framework |
| CN115849996A (en) * | 2023-01-10 | 2023-03-28 | 延安大学 | Potassium-doped maghemite-coupled graphene composite combustion catalyst, and preparation method and application thereof |
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Cited By (8)
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|---|---|---|---|---|
| CN109573988A (en) * | 2018-12-14 | 2019-04-05 | 东华大学 | A kind of graphene composite aerogel absorbing material and its preparation method and application |
| CN109573988B (en) * | 2018-12-14 | 2022-04-29 | 东华大学 | Graphene composite aerogel wave-absorbing material and preparation method and application thereof |
| CN109806912A (en) * | 2019-03-11 | 2019-05-28 | 山西大学 | Can magnetic recycling Nd complex/GO/Fe3O4Ternary complex and its preparation method and application |
| CN109806912B (en) * | 2019-03-11 | 2021-05-14 | 山西大学 | Neodymium complex/GO/Fe capable of being magnetically recycled3O4Ternary complex and preparation method and application thereof |
| CN109935818A (en) * | 2019-03-28 | 2019-06-25 | 中南大学 | A kind of ferroso-ferric oxide/rGO nanometer anode material and preparation method thereof |
| CN110012656A (en) * | 2019-05-05 | 2019-07-12 | 安徽理工大学 | A kind of preparation method of the derivative ferroso-ferric oxide@carbon/nano combined absorbing material of redox graphene of metal-organic framework |
| CN115849996A (en) * | 2023-01-10 | 2023-03-28 | 延安大学 | Potassium-doped maghemite-coupled graphene composite combustion catalyst, and preparation method and application thereof |
| CN115849996B (en) * | 2023-01-10 | 2024-01-26 | 延安大学 | Potassium-doped maghemite coupled graphene composite combustion catalyst and preparation method and application thereof |
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