CN107528046A - Preparation method, negative pole and the lithium ion battery of graphene/ferric oxide nano composite - Google Patents

Preparation method, negative pole and the lithium ion battery of graphene/ferric oxide nano composite Download PDF

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Publication number
CN107528046A
CN107528046A CN201610452712.6A CN201610452712A CN107528046A CN 107528046 A CN107528046 A CN 107528046A CN 201610452712 A CN201610452712 A CN 201610452712A CN 107528046 A CN107528046 A CN 107528046A
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China
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graphene
ferric oxide
oxide nano
nano composite
preparation
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CN201610452712.6A
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Chinese (zh)
Inventor
范佳晨
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Zhangjiagang Si Jie Hardware Tools Co Ltd
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Zhangjiagang Si Jie Hardware Tools Co Ltd
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Priority to CN201610452712.6A priority Critical patent/CN107528046A/en
Publication of CN107528046A publication Critical patent/CN107528046A/en
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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
    • 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
    • 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
    • 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
    • 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
    • H01M4/38—Selection of substances as active materials, active masses, active liquids of elements or alloys
    • 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
    • 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
    • H01M4/58—Selection of substances as active materials, active masses, active liquids of inorganic compounds other than oxides or hydroxides, e.g. sulfides, selenides, tellurides, halogenides or LiCoFy; of polyanionic structures, e.g. phosphates, silicates or borates
    • H01M4/583—Carbonaceous material, e.g. graphite-intercalation compounds or CFx
    • H01M4/587—Carbonaceous material, e.g. graphite-intercalation compounds or CFx for inserting or intercalating light metals
    • 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

This application discloses preparation method, negative pole and the lithium ion battery of a kind of graphene/ferric oxide nano composite, the preparation method of the composite, including step：(1) ultrasonic disperse in the mixed solution of distilled water and ethylene glycol, is added graphene oxide into；(2), ferrous sulfate heptahydrate, polyvinylpyrrolidone are scattered in mixed liquor, stirred；(3), hydrazine hydrate is added to be stirred；(4), mixed solution is placed under sealed environment, 15~20 hours are incubated at 180~200 DEG C；(5), reactant is washed and dried, obtains graphene/ferric oxide nano composite.The composite that the present invention obtains, ferric oxide nano particles are uniformly deposited in graphene nano layer, prevent the reunion of graphene, the composite obtained is applied to lithium battery, the stability of its structure and the electric conductivity of electrode are effectively increased, the composite material exhibits go out higher reversible capacity, good high rate performance and fabulous stability.

Description

Preparation method, negative pole and the lithium ion battery of graphene/ferric oxide nano composite
Technical field
The application is related to a kind of lithium ion battery negative material, is received more particularly to a kind of graphene/iron oxide Preparation method, negative pole and the lithium ion battery of nano composite material.
Background technology
In order to meet growing energy demand, developing new equipment and its associated materials turns into production and storage Deposit a key issue of electric power, at present, in electric automobile industry, lithium ion battery because its have compared with High energy density, quick charge/discharge efficiency and cycle performance, as attractive power supply, Paid close attention to by market.Therefore small, the safe electrode material of resistance is widely paid close attention to.
Ferroso-ferric oxide rich content, cost is low, and environmentally friendly, has been considered as most promising One of electrode material.However, in electrochemistry cyclic process, generally occur largely to change and serious Particle agglomeration, this cause electrode part crush and structural damage, so as to cause irreversible capacity Loss is big and cyclical stability is poor.
The content of the invention
It is an object of the invention to provide a kind of preparation method of graphene/ferric oxide nano composite, bear Pole and lithium ion battery, to overcome deficiency of the prior art.
To achieve the above object, the present invention provides following technical scheme：
The embodiment of the present application discloses a kind of preparation method of graphene/ferric oxide nano composite, including step Suddenly：
(1) ultrasonic disperse in the mixed solution of distilled water and ethylene glycol, is added graphene oxide into；
(2), ferrous sulfate heptahydrate, polyvinylpyrrolidone are scattered in mixed liquor, stirred；
(3), hydrazine hydrate is added to be stirred；
(4), mixed solution is placed under sealed environment, 15~20 hours are incubated at 180~200 DEG C；
(5), reactant is washed and dried, obtains graphene/ferric oxide nano composite.
Preferably, in the preparation method of above-mentioned graphene/ferric oxide nano composite, step (1) In, mixed solution ultrasonic disperse 2~2.5 hours at 20~25 DEG C.
Preferably, in the preparation method of above-mentioned graphene/ferric oxide nano composite, step (1) In, the volume ratio of deionized water and monoethanolamine is (3~4):1.
Preferably, in the preparation method of above-mentioned graphene/ferric oxide nano composite, step (2) In, graphene oxide：Ferrous sulfate heptahydrate：Polyvinylpyrrolidone=(0.04~0.05)：(1.4~1.5):1.
Disclosed herein as well is a kind of negative electrode of lithium ion battery, including any described graphene/iron oxide to receive Nano composite material.
Disclosed herein as well is a kind of lithium ion battery, including described negative electrode of lithium ion battery.
Compared with prior art, the advantage of the invention is that：The composite that the present invention obtains, iron oxide Nano-particle is uniformly deposited in graphene nano layer, and it further prevents the reunion of graphene, institute The composite of acquisition is applied to lithium battery, effectively increases the stability of its structure and the electric conductivity of electrode, The composite material exhibits go out higher reversible capacity, good high rate performance and fabulous stability.
Embodiment
The present invention is described further by the following example：, can be more preferably geographical according to following embodiments The solution present invention.However, as it will be easily appreciated by one skilled in the art that specific material described by embodiment The present invention is merely to illustrate than, process conditions and its result, without should be also without limitation on claims In the described in detail present invention.
Embodiment 1
The preparation method of graphene/ferric oxide nano composite
(1), add graphene oxide into the mixed solution of distilled water and ethylene glycol, and at 20 DEG C Ultrasonic disperse 2.5 hours, wherein, the volume ratio of deionized water and monoethanolamine is 3:1；
(2), ferrous sulfate heptahydrate, polyvinylpyrrolidone are scattered in mixed liquor, stirred, Wherein graphene oxide：Ferrous sulfate heptahydrate：Polyvinylpyrrolidone=0.05：1.4:1；
(3), hydrazine hydrate is added to be stirred；
(4), mixed solution is placed under sealed environment, 20 hours are incubated at 180 DEG C；
(5), reactant is washed and dried, obtains graphene/ferric oxide nano composite.
Characterization result surface：Ferric oxide nano particles are intensive and are uniformly dispersed on graphene layer, and it has The reunion for preventing graphene of effect.
Prepared composite is applied to the negative material of lithium ion battery, it shows higher fill Anti-electric specific capacity.The composite also shows excellent high rate performance, in addition, the composite also has There is ferromagnetic behavior, effectively can be separated in the presence of externally-applied magnetic field from solution.
Embodiment 2
The preparation method of graphene/ferric oxide nano composite
(1), add graphene oxide into the mixed solution of distilled water and ethylene glycol, and at 20 DEG C Ultrasonic disperse 2.5 hours, wherein, the volume ratio of deionized water and monoethanolamine is 4:1；
(2), ferrous sulfate heptahydrate, polyvinylpyrrolidone are scattered in mixed liquor, stirred, Wherein graphene oxide：Ferrous sulfate heptahydrate：Polyvinylpyrrolidone=0.05：1.4:1；
(3), hydrazine hydrate is added to be stirred；
(4), mixed solution is placed under sealed environment, 20 hours are incubated at 180 DEG C；
(5), reactant is washed and dried, obtains graphene/ferric oxide nano composite.
Embodiment 3
The preparation method of graphene/ferric oxide nano composite
(1), add graphene oxide into the mixed solution of distilled water and ethylene glycol, and at 25 DEG C Ultrasonic disperse 2 hours, wherein, the volume ratio of deionized water and monoethanolamine is 3:1；
(2), ferrous sulfate heptahydrate, polyvinylpyrrolidone are scattered in mixed liquor, stirred, Wherein graphene oxide：Ferrous sulfate heptahydrate：Polyvinylpyrrolidone=0.04：1.5:1；
(3), hydrazine hydrate is added to be stirred；
(4), mixed solution is placed under sealed environment, 15 hours are incubated at 200 DEG C；
(5), reactant is washed and dried, obtains graphene/ferric oxide nano composite.
Finally, it is to be noted that, term " comprising ", "comprising" or its any other variant are intended to Nonexcludability includes, so that process, method, article or equipment including a series of elements are not Only include those key elements, but also the other element including being not expressly set out, or it is this also to include Kind of process, method, article or the intrinsic key element of equipment.

Claims (6)

1. the preparation method of a kind of graphene/ferric oxide nano composite, it is characterised in that including step：
(1) ultrasonic disperse in the mixed solution of distilled water and ethylene glycol, is added graphene oxide into；
(2), ferrous sulfate heptahydrate, polyvinylpyrrolidone are scattered in mixed liquor, stirred；
(3), hydrazine hydrate is added to be stirred；
(4), mixed solution is placed under sealed environment, 15~20 hours are incubated at 180~200 DEG C；
(5), reactant is washed and dried, obtains graphene/ferric oxide nano composite.
2. the preparation method of graphene according to claim 1/ferric oxide nano composite, it is special Sign is：In step (1), mixed solution ultrasonic disperse 2~2.5 hours at 20~25 DEG C.
3. the preparation method of graphene according to claim 1/ferric oxide nano composite, it is special Sign is：In step (1), the volume ratio of deionized water and monoethanolamine is (3~4):1.
4. the preparation method of graphene according to claim 1/ferric oxide nano composite, it is special Sign is：In step (2), graphene oxide：Ferrous sulfate heptahydrate：Polyvinylpyrrolidone= (0.04~0.05)：(1.4~1.5):1.
5. a kind of negative electrode of lithium ion battery, including any described graphene/iron oxide of Claims 1-4 Nano composite material.
6. a kind of lithium ion battery, including the negative electrode of lithium ion battery described in claim 5.
CN201610452712.6A 2016-06-21 2016-06-21 Preparation method, negative pole and the lithium ion battery of graphene/ferric oxide nano composite Pending CN107528046A (en)

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Cited By (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN109192930A (en) * 2018-09-10 2019-01-11 深圳技术大学（筹） The preparation method of graphene complex electrode

Citations (6)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
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
CN102185143A (en) * 2011-04-02 2011-09-14 浙江大学 Transition metal oxide/ graphene composite material and preparation method thereof
CN103127929A (en) * 2011-12-01 2013-06-05 百泽(常州)新能源科技有限公司 Lithium air cell by utilizing graphene/oxide composite material as air electrode catalyst
CN103951916A (en) * 2014-04-29 2014-07-30 南昌航空大学 RGO (Reduced Graphene oxide)/ferric oxide-filled polyvinylidene fluoride composite wave-absorbing material and preparation method thereof
CN104269536A (en) * 2014-09-25 2015-01-07 天津大学 Graphene-loaded spherical carbon-cladded iron oxide composite material and preparation method of composite material
CN104733717A (en) * 2015-03-31 2015-06-24 扬州大学 Microwave preparation method of alpha-Fe2O3/rGO composite material

Patent Citations (6)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
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
CN102185143A (en) * 2011-04-02 2011-09-14 浙江大学 Transition metal oxide/ graphene composite material and preparation method thereof
CN103127929A (en) * 2011-12-01 2013-06-05 百泽(常州)新能源科技有限公司 Lithium air cell by utilizing graphene/oxide composite material as air electrode catalyst
CN103951916A (en) * 2014-04-29 2014-07-30 南昌航空大学 RGO (Reduced Graphene oxide)/ferric oxide-filled polyvinylidene fluoride composite wave-absorbing material and preparation method thereof
CN104269536A (en) * 2014-09-25 2015-01-07 天津大学 Graphene-loaded spherical carbon-cladded iron oxide composite material and preparation method of composite material
CN104733717A (en) * 2015-03-31 2015-06-24 扬州大学 Microwave preparation method of alpha-Fe2O3/rGO composite material

Cited By (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN109192930A (en) * 2018-09-10 2019-01-11 深圳技术大学（筹） The preparation method of graphene complex electrode

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