CN108598433A - A kind of SnO2The preparation method of/graphene lithium ion battery negative material - Google Patents
A kind of SnO2The preparation method of/graphene lithium ion battery negative material Download PDFInfo
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- CN108598433A CN108598433A CN201810412000.0A CN201810412000A CN108598433A CN 108598433 A CN108598433 A CN 108598433A CN 201810412000 A CN201810412000 A CN 201810412000A CN 108598433 A CN108598433 A CN 108598433A
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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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- 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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- 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
- H01M4/485—Selection of substances as active materials, active masses, active liquids of inorganic oxides or hydroxides of mixed oxides or hydroxides for inserting or intercalating light metals, e.g. LiTi2O4 or LiTi2OxFy
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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 present invention provides a kind of SnO2The preparation method of/graphene lithium ion battery negative material.High-quality graphene material is prepared using graphite intercalation compound stripping means, oxidative modification is carried out to high-quality graphene by full carbon face oxidation technology, obtain the equally distributed graphene oxide composite material of oxygen-containing group, the hydrochloric acid solution of graphene oxide and stannous chloride is mixed, under electrostatic adsorption, SnO2It is formed in oxygen-containing group site, then through microwave irradiation redox graphene, obtains SnO2/ graphene negative material.The method of the present invention uses the equally distributed graphene oxide composite material of oxygen-containing group, obtains the equally distributed SnO of tin oxide nanoparticles2/ graphene lithium ion battery negative material, overcomes SnO2Reversible capacity that particle agglomeration problem is brought is relatively low, high rate performance and the shortcomings that poor circulation.
Description
Technical field
The present invention relates to field of lithium ion battery cathode material preparation, with the equally distributed graphite oxide of oxygen-containing group
Alkene material obtains the equally distributed SnO of tin oxide nanoparticles under electrostatic adsorption2/ graphene lithium ion battery cathode
Material.
Background technology
The electric vehicle industry of rapid development and portable electronic product active demand high power capacity, high current, long circulation life
Electrode material.Tin oxide (2) SnOx, x=1 have cheap, abundance, environmentally friendly advantage, it is considered to be
The negative material of most potential next generation's commercialization LIBs.But single SnO2Exist not as lithium ion battery negative material
Foot, SnO during charge and discharge cycles2Serious volume expansion (about 400%) phenomenon is will produce, material fragmentation and powder are caused
Change, to lose electrical contact with collector, eventually leads to SnO2The reversible capacity of negative material is relatively low, high rate performance and cyclicity
It can be all poor.Using the unique two-dimensional nanostructure of graphene and its good electric conductivity, by coating nano SnO2It is made
SnO2/ graphene composite negative pole can effectively inhibit single SnO2Existing body when as lithium ion battery negative material
Product expansion and therefore and generate cycle life it is poor the deficiencies of.Graphene can not only be effectively relieved due to SnO2Volume it is swollen
Swollen and generation internal stress, can also provide the specific surface area and conductivity of superelevation, to improve the electric property of material.
Many research work pass through carbon coating, carbon doping and structure design (such as core one in nanometer or micro-meter scale
Shell structure etc.) solve SnO2Existing deficiency.Yao etc. utilizes the good electric conductivity of graphene and preferable lithium storage function,
It is prepared for SnO2/ graphene nanometer composite, the negative material is after 100 cycles, under the current density of 50mA/g,
Discharge capacity remains at 520mAh/g.But the preparation process of the material is complex (to be needed to add NaBH4 or hydrazine hydrate etc.
Other reducing agents, or even also need to flow back), and the influencing mechanism in relation to graphene also remains unknown.Zuo Zhenmin etc. is using temperature
The hydro-thermal method of sum growth in situ nano SnO on graphene oxide (GO) lamella2Particle, by ammonia water conditioning system pH value and right
Graphene carries out nitrating, has successfully prepared SnO2/ nitrogen-doped graphene (N-rGO) and SnO2/ graphene (rGO) is nano combined
Material is distributed in the surfaces N-rGO and rGO SnO2Grain diameter is respectively 50nm and 100nm or so, SnO2Particle is by more tiny
Grain size be 5-7nm SnO2The secondary agglomeration body that particle is formed, SnO2The distributivity of nano particle is poor.The utilizations such as Yu Zhenjun
Using graphite oxide and stannous chloride as raw material, direct in-situ synthesizes SnO2/ graphene nanocomposite material, SnO2Particle can be equal
Disperse on the surface of graphene, to avoid mechanical mix techniques SnO in preparation process evenly2The group of nano-particle or graphene
It is poly-, but SnO2The distribution of particle and the distribution of graphene oxide oxygen-containing functional group are closely related, the reduction journey of graphene oxide
Degree is also related to the reducing power of stannous chloride, and the distributing homogeneity and electric conductivity of material need to be further strengthened.Currently, big portion
Divide SnO2The preparation method of/graphene nano material is compound using stannous chloride and graphene oxide, stannous chloride in-situ reducing
Graphene oxide becomes tin oxide, and site of the oxygen atom on graphene oxide is reaction site, the type of oxygen-containing group with
Distribution determines whether tin oxide can be uniformly distributed in graphene surface, therefore, it is single and uniform to obtain a kind of oxygen-containing group
The graphene oxide composite material of distribution is the key that tin oxide nanoparticles are evenly distributed.
Invention content
The present invention provides a kind of SnO2The preparation method of/graphene lithium ion battery negative material, it is equal with oxygen-containing group
The graphene oxide composite material of even distribution obtains the equally distributed battery cathode of tin oxide nanoparticles under electrostatic adsorption
Material.
The present invention adopts the following technical scheme that：
A kind of SnO2The preparation method of/graphene lithium ion battery negative material, includes the following steps：
(1) by preparing high-quality graphene material to the stripping of graphite intercalation compound, with oxidations such as potassium permanganate
Agent carries out oxidative modification to high-quality graphene, obtains the equally distributed graphene oxide composite material of oxygen-containing group；
(2) hydrochloric acid solution of graphene oxide and two hydrated stannous chlorides is mixed evenly, by microwave irradiation by oxygen
Graphite alkene restores, then after washed, drying, obtains SnO2/ graphene negative material.
The intercalator of graphite intercalation compound includes lodine chloride, Iodide Bromide or anhydrous ferric trichloride etc. in step (1).
Oxidant includes permanganate, chlorate, ferrite, chromate, persulfate etc. in step (1).
Oxygen-containing group includes carboxyl, hydroxyl, carbonyl and epoxy group in step (1).
Oxidizer is the 25-400% of high-quality graphene quality, oxidization time 0.5-6h in step (1).
The quality of two hydrated stannous chlorides is the 200-400% of graphene oxide in step (2).
It is preferably 0.5h that the time is mixed in step (2), and microwave irradiation power is preferably 900W, and microwave irradiation time is excellent
It is selected as 4min.
The present invention has following advantage：
(1) present invention can prepare the equally distributed graphene oxide composite material of oxygen-containing group, overcome conventional oxidation graphite
The inhomogeneities being distributed from the outer layer oxygen-containing group that internally gradually oxidized zone comes in alkene preparation process.
(2) requirement of the preparation method of the present invention to equipment is relatively low, is suitable for industry or laboratory operation.
Description of the drawings
Fig. 1 is that the method for the present invention prepares SnO2The TEM light fields figure and dark field plot of/grapheme material.It is TEM light fields to scheme a, c
As figure, wherein black represents SnO2Particle.Compared with composite material being prepared with conventional method (figure c), the electricity of the method for the present invention preparation
SnO in the composite material of pole2Distribution of particles is smaller and be more evenly distributed as shown in figure a.It is TEM dark field images to scheme b, d, wherein
White represents SnO2Particle.Scheme b, d on the right side of connect cromogram be tetra- kinds of elements of C, Sn, O, Cl distribution map, chosen area with
Scheme b, d correspond to, luminance characterization amount of element number.
Specific implementation mode
Of the invention for ease of understanding, it is as follows that the present invention enumerates embodiment.Those skilled in the art are it will be clearly understood that the implementation
Example is used only for helping to understand the present invention, should not be regarded as a specific limitation of the invention.
Embodiment 1
(1) 60g Iodide Bromide is uniformly mixed with 100mg expanded graphites, is packed into protection gas Ar gas, is enclosed within 100mL glass
In glass bottle, vial is placed in 100 DEG C of oil bath environment, is heated 48h, is prepared graphite intercalation compound.
(2) graphite intercalation compound is taken out and is filtered from vial rapidly, be put into the water heating kettle that volume is 50mL,
10mL aqueous solutions are added into water heating kettle, fix water heating kettle equipment rapidly.
(3) water heating kettle is heated to 180 DEG C, 1h, reaction is kept to finish, take out sample, cleaning sample obtains high quality stone
Black alkene powder aggregates.
(4) 50mg graphenes are put into the concentrated sulfuric acid that volume is 20mL, 100mg sodium chlorate are added, in ice-water bath
4h is reacted, graphene oxide is obtained after cleaning.
(5) 50mg graphite oxides are substantially soluble in 20mL deionized waters and obtain graphite oxide solution.Add 100mg
SnCl2·2H2The hydrochloric acid that O is 37% with 0.5mL mass fractions, magnetic agitation 1h.
(6) beaker is placed in micro-wave oven, the microwave irradiation 4min under the power of 900W, after filtration, washing and drying,
Obtain SnO2/ graphene negative material.
Embodiment 2
(1) by the anhydrous FeCl of 0.3g3It being mixed with 0.05g expanded graphites, vacuum tightness, 1h is warming up to 380 DEG C, maintains 12h,
Prepare graphite intercalation compound.Graphite intercalation compound is dissolved in dilute hydrochloric acid solution, filters drying, for use.
(2) graphite intercalation compound is put into rapidly to the supercritical CO that volume is 50mL2In device, to supercritical CO2Device
The middle hydrogen peroxide solution that 5mL mass fractions are added and are 30%, fixes rapidly equipment.
(3) by high supercritical CO2Device is heated to 38 DEG C, and boost in pressure to 75atm keeps 1h, reaction to finish, and takes out sample
Product, cleaning sample obtain graphene powder aggregation.
(4) 50mg graphenes are put into the concentrated sulfuric acid that volume is 20mL, 100mg sodium chlorate are added, in ice-water bath
4h is reacted, graphene oxide is obtained after cleaning.
(5) 50mg graphite oxides are substantially soluble in 20mL deionized waters and obtain graphite oxide solution.Add 100mg
SnCl2·2H2The hydrochloric acid that O is 37% with 0.5mL mass fractions, magnetic agitation 1h.
(6) beaker is placed in micro-wave oven, the microwave irradiation 4min under the power of 900W, after filtration, washing and drying,
Obtain SnO2/ graphene negative material.
Fig. 1 is that the present embodiment prepares SnO2The TEM light fields figure and dark field plot of/grapheme material.
Embodiment 3
(1) by the anhydrous FeCl of 0.3g3It being mixed with 0.05g expanded graphites, vacuum tightness, 1h is warming up to 380 DEG C, maintains 12h,
Prepare graphite intercalation compound.Graphite intercalation compound is dissolved in dilute hydrochloric acid solution, filters drying, for use.
(2) graphite intercalation compound is put into rapidly to the supercritical CO that volume is 50mL2In device, to supercritical CO2Device
The middle hydrogen peroxide solution that 5mL mass fractions are added and are 30%, fixes rapidly equipment.
(3) by high supercritical CO2Device is heated to 38 DEG C, and boost in pressure to 75atm keeps 1h, reaction to finish, and takes out sample
Product, cleaning sample obtain graphene powder aggregation.
(4) 50mg graphenes are put into the concentrated sulfuric acid that volume is 20mL, 100mg sodium chlorate are added, in ice-water bath
2h is reacted, graphene oxide is obtained after cleaning.
(5) 50mg graphite oxides are substantially soluble in 20mL deionized waters and obtain graphite oxide solution.Add 100mg
SnCl2·2H2The hydrochloric acid that O is 37% with 0.5mL mass fractions, magnetic agitation 1h.
(6) beaker is placed in micro-wave oven, the microwave irradiation 4min under the power of 900W, after filtration, washing and drying,
Obtain SnO2/ graphene negative material.
Embodiment 4
(1) by the anhydrous FeCl of 0.3g3It being mixed with 0.05g expanded graphites, vacuum tightness, 1h is warming up to 380 DEG C, maintains 12h,
Prepare graphite intercalation compound.Graphite intercalation compound is dissolved in dilute hydrochloric acid solution, filters drying, for use.
(2) graphite intercalation compound is put into rapidly to the supercritical CO that volume is 50mL2In device, to supercritical CO2Device
The middle hydrogen peroxide solution that 5mL mass fractions are added and are 30%, fixes rapidly equipment.
(3) by high supercritical CO2Device is heated to 38 DEG C, and boost in pressure to 75atm keeps 1h, reaction to finish, and takes out sample
Product, cleaning sample obtain graphene powder aggregation.
(4) 50mg graphenes are put into the concentrated sulfuric acid that volume is 20mL, 200mg sodium chlorate are added, in ice-water bath
2h is reacted, graphene oxide is obtained after cleaning.
(5) 50mg graphite oxides are substantially soluble in 20mL deionized waters and obtain graphite oxide solution.Add 100mg
SnCl2·2H2The hydrochloric acid that O is 37% with 0.5mL mass fractions, magnetic agitation 1h.
(6) beaker is placed in micro-wave oven, the microwave irradiation 4min under the power of 900W, after filtration, washing and drying,
Obtain SnO2/ graphene negative material.
Applicant states that the present invention illustrates detailed process equipment and the technological process of the present invention by above-described embodiment,
But the invention is not limited in above-mentioned detailed process equipment and technological processes, that is, it is above-mentioned detailed not mean that the present invention has to rely on
Process equipment and technological process could be implemented.Person of ordinary skill in the field it will be clearly understood that any improvement in the present invention,
The addition of equivalence replacement and auxiliary element to each raw material of product of the present invention, the selection etc. of concrete mode all fall within the present invention's
Within protection domain and the open scope.
Claims (7)
1. a kind of SnO2The preparation method of/graphene lithium ion battery negative material, includes the following steps：
(1) by preparing high-quality graphene material to the stripping of graphite intercalation compound, with oxidants pair such as potassium permanganate
High-quality graphene carries out oxidative modification, obtains the equally distributed graphene oxide composite material of oxygen-containing group；
(2) hydrochloric acid solution of graphene oxide and two hydrated stannous chlorides is mixed evenly, and stone will be aoxidized by microwave irradiation
Black alkene reduction, then after washed, drying, obtain SnO2/ graphene negative material.
2. preparation method according to claim 1, which is characterized in that graphite intercalation compound described in step (1) is inserted
Layer agent includes lodine chloride, Iodide Bromide or anhydrous ferric trichloride etc..
3. preparation method according to claim 1, which is characterized in that oxidant described in step (1) include permanganate,
Chlorate, ferrite, chromate, persulfate etc..
4. preparation method according to claim 1, which is characterized in that oxygen-containing group described in step (1) includes carboxyl, hydroxyl
Base, carbonyl and epoxy group.
5. preparation method according to claim 1, which is characterized in that oxidizer is high quality described in step (1)
The 25-400% of graphene quality, oxidization time 0.5-6h.
6. preparation method according to claim 1, which is characterized in that the matter of two hydrated stannous chlorides described in step (2)
Amount is the 200-400% of graphene oxide.
7. preparation method according to claim 1, which is characterized in that described in step (2) be mixed the time be preferably
0.5h, microwave irradiation power are preferably 900W, and microwave irradiation time is preferably 4min.
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Cited By (7)
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| CN109411741A (en) * | 2018-10-15 | 2019-03-01 | 合肥国轩高科动力能源有限公司 | A kind of composite negative pole material and its preparation method and application |
| CN109817944A (en) * | 2019-02-18 | 2019-05-28 | 山东星火科学技术研究院 | Lithium ion battery cathode silica/graphene nano material preparation method |
| CN109830665A (en) * | 2019-02-18 | 2019-05-31 | 山东星火科学技术研究院 | A kind of ultrafast charge and discharge large capacity aluminium-graphene battery |
| CN112531171A (en) * | 2020-12-02 | 2021-03-19 | 萝北瑞喆烯碳新材料有限公司 | Graphene-coated silicon carbide negative electrode material and preparation method thereof |
| CN112573508A (en) * | 2020-12-28 | 2021-03-30 | 上海纳米技术及应用国家工程研究中心有限公司 | Preparation method, product and application of graphene-coated core-shell stannous oxide @ tin oxide material |
| CN112751013A (en) * | 2019-10-31 | 2021-05-04 | 中国石油化工股份有限公司 | Nitrogen-doped TiO2/GRA composite material |
| CN112744859A (en) * | 2019-10-31 | 2021-05-04 | 中国石油化工股份有限公司 | Fibrous graphene doped TiO2Composite material |
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| Publication number | Priority date | Publication date | Assignee | Title |
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| CN109411741A (en) * | 2018-10-15 | 2019-03-01 | 合肥国轩高科动力能源有限公司 | A kind of composite negative pole material and its preparation method and application |
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| CN109830665A (en) * | 2019-02-18 | 2019-05-31 | 山东星火科学技术研究院 | A kind of ultrafast charge and discharge large capacity aluminium-graphene battery |
| CN112751013A (en) * | 2019-10-31 | 2021-05-04 | 中国石油化工股份有限公司 | Nitrogen-doped TiO2/GRA composite material |
| CN112744859A (en) * | 2019-10-31 | 2021-05-04 | 中国石油化工股份有限公司 | Fibrous graphene doped TiO2Composite material |
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| CN112531171A (en) * | 2020-12-02 | 2021-03-19 | 萝北瑞喆烯碳新材料有限公司 | Graphene-coated silicon carbide negative electrode material and preparation method thereof |
| CN112573508A (en) * | 2020-12-28 | 2021-03-30 | 上海纳米技术及应用国家工程研究中心有限公司 | Preparation method, product and application of graphene-coated core-shell stannous oxide @ tin oxide material |
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Application publication date: 20180928 |