CN106129373B - A kind of hollow sphere Fe2O3The preparation method of/rGO lithium ion battery negative material - Google Patents
A kind of hollow sphere Fe2O3The preparation method of/rGO lithium ion battery negative material Download PDFInfo
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- CN106129373B CN106129373B CN201610729908.5A CN201610729908A CN106129373B CN 106129373 B CN106129373 B CN 106129373B CN 201610729908 A CN201610729908 A CN 201610729908A CN 106129373 B CN106129373 B CN 106129373B
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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
- H01M4/523—Selection of substances as active materials, active masses, active liquids of inorganic oxides or hydroxides of nickel, cobalt or iron for non-aqueous cells
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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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- 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
- H01M4/628—Inhibitors, e.g. gassing inhibitors, corrosion inhibitors
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- 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
A kind of hollow sphere Fe2O3The preparation method of/rGO lithium ion battery negative material, adds graphene oxide into deionized water, and suspension A is made;CTAB is added in suspension A, after stirring, obtains mixed liquid B;Soluble divalent iron salt is added in mixed liquid B, mixture C is obtained;The pH value of mixed liquor C is adjusted to 2~7, in microwave hydrothermal reaction, 0.5~3h is reacted at 120~180 DEG C.The present invention with graphene is compound not only can effectively solve Fe2O3The problem of poorly conductive, and the dusting that this special self assembly hollow structure can also effectively alleviate volume expansion, and then prevent oxide from occurring in charge and discharge process, the cycle performance of product can be significantly improved.The present invention uses microwave hydrothermal one-step synthesis method, and method is simple, and easy to operate, the reaction time is short, low in cost, environmental-friendly, is expected to realize industrialized production.
Description
Technical field
The invention belongs to electrochemical technology fields, and in particular to a kind of hollow sphere Fe2O3/ rGO lithium ion battery negative material
Preparation method.
Background technique
Since lithium ion battery has energy density high, long service life, advantages of environment protection becomes recent years
Research hotspot, and it is successfully realized commercialization.It can be applied to electric car to develop the next generation, the large-scale energy is deposited
The more effective lithium ion battery material for storing up equipment, can search out a kind of negative electrode material with excellent chemical property is
A key factor.Fe2O3With high capacity (about 1000mAh g-1), low cost is from a wealth of sources, it is nontoxic the advantages that, and it is existing
Theoretical capacity be only 372mAhg-1Graphite electrode compare, have significant advantage.However Fe2O3Have with most of oxides
There are a same problem, such as poorly conductive, whens charge and discharge easily occurs volume expansion and causes to recycle these unstable disadvantages significantly
Limit its extensive use, it is therefore desirable to find a kind of carbon material of good conductivity come with its it is compound improve its electric conductivity,
Cell reaction activity is improved by controlling the pattern of product, increases the contact surface with electrolyte by subtracting short grained size
Product improves battery performance.
Summary of the invention
The present invention is directed to existing issue, it is therefore an objective to propose a kind of hollow sphere Fe2O3The system of/rGO lithium ion battery negative material
Preparation Method, and graphene is compound not only can effectively solve Fe2O3The problem of poorly conductive, and this special self assembly is hollow
Structure can also effectively alleviate volume expansion, and then the dusting for preventing oxide from occurring in charge and discharge process, can significantly mention
The cycle performance of high product.The present invention uses microwave hydrothermal one-step synthesis method, and method is simple, and easy to operate, the reaction time is short, at
This is cheap, environmental-friendly, is expected to realize industrialized production.
To achieve the above object, technical scheme is as follows:
A kind of hollow sphere Fe2O3The preparation method of/rGO lithium ion battery negative material, comprising the following steps:
1) it adds graphene oxide into deionized water, is uniformly mixed, it is 0.5mg/mL~2mg/mL's that concentration, which is made,
Suspension A;
2) CTAB is added in suspension A under continuous agitation, until the concentration of CTAB is in suspension A
0.001~0.2g/L obtains mixed liquid B after then proceeding to stirring 10~30 minutes;
3) soluble divalent iron salt is added in mixed liquid B, is stirred evenly, obtaining ferrous ion concentration is 0.01mol/
The mixture C of L~0.5mol/L;
4) pH value of mixed liquor C is adjusted to 2~7, obtains mixture D;
5) by mixture D in microwave hydrothermal reaction, temperature control mode is selected to be reacted, reaction temperature is 120~180
DEG C, the reaction time is 0.5~3h, obtains product E;
6) by product E washing, drying, hollow sphere Fe is obtained2O3/ rGO lithium ion battery negative material.
A further improvement of the present invention lies in that being uniformly mixed in step 1) is realized by ultrasonic shear 10min~90min
's.
A further improvement of the present invention lies in that soluble divalent iron salt is ferrous sulfate, frerrous chloride or vinegar in step 3)
It is sour ferrous.
A further improvement of the present invention lies in that the time stirred in step 3) is 10~60min.
A further improvement of the present invention lies in that using salt acid for adjusting pH value to 2~7 in step 4).
A further improvement of the present invention lies in that the concentration of hydrochloric acid is 2mol/L.
A further improvement of the present invention lies in that being warming up to 120~180 in step 5) with the heating rate of 10~20 DEG C/min
℃。
A further improvement of the present invention lies in that product E is washed using deionized water and dehydrated alcohol in step 6), true
12h is dried in empty drying box at 60 DEG C.
Compared with prior art, the invention has the benefit that
Raw material sources of the present invention are extensive, at low cost, and environmental protection, used method is simple and quick, uses ferrous iron
Reducing agent of the salt as source of iron and redox graphene.Present invention employs the methods of microwave hydrothermal, and heating rate is very fast, together
Shi Weibo also has the function of redox graphene, using CTAB as template, while being also used as alkali source, can be reaction
OH is provided-Ion forms iron oxide.The Fe of self assembly hollow structure produced by the present invention2O3/ rGO composite structure is unique, this
Kind graphene complex can not only improve the electric conductivity of iron oxide well, and can also farthest alleviate iron oxide
The volume expansion occurred when being embedded in and deviating from lithium ion.The raw material that the present invention uses is simple, cheap, apparatus and process letter
It is single, any surfactant is not added in synthesis process, obtained product purity is high.Self assembly prepared by the present invention is hollow
The Fe of spherical structure2O3/ rGO compound electrochemical performance, stable cycle performance, when current density is 200mA/g, circulation
After 65 circles, the capacity of 1120mAh/g can be still maintained, in cyclic process, capacity shows the trend of rising, shows this
The Fe of self assembly hollow structure2O3/ rGO compound largely improves the chemical property of product.
Detailed description of the invention
Fig. 1 is the high power scanning electron microscope (SEM) photograph of the embodiment of the present invention 1.
Fig. 2 is the low power scanning electron microscope (SEM) photograph of the embodiment of the present invention 1.
Fig. 3 is the chemical property figure of the embodiment of the present invention 1.
Specific embodiment
With reference to the accompanying drawing, by specific embodiment, the present invention will be described in detail.
Embodiment 1
(1) it adds graphene oxide into deionized water, ultrasonic shear 10min, it is the outstanding of 0.8mg/mL that concentration, which is made,
Turbid A;
(2) then CTAB (cetyl trimethylammonium bromide) is added in suspension A under conditions of keeping stirring, directly
Into suspension A, the concentration of CTAB is 0.005g/L, then proceedes to stirring after twenty minutes, obtains mixed liquid B;
(3) analytically pure soluble divalent iron salt frerrous chloride is added in mixed liquid B, stirs 30min, obtains ferrous iron
Ion concentration is the mixture C of 0.1mol/L;
(4) mixture C 2mol/L dilute hydrochloric acid is then adjusted into pH value to 3, obtains mixture D;
(5) mixture D being put into and is poured into microwave hydrothermal reaction kettle, volume compactedness is 60%, reaction kettle is then sealed,
It puts it into microwave hydrothermal reaction, selects temperature control mode to be reacted, be warming up to 120 with the heating rate of 10 DEG C/min
DEG C, reaction time 2h naturally cools to room temperature after reaction, obtains product E;
(6) product E is then used into deionized water respectively, dehydrated alcohol washs for several times, does at 60 DEG C in a vacuum drying oven
Dry 12h obtains hollow sphere Fe2O3/ rGO lithium ion battery negative material.
The JSM-6700F type scanning electron microscope that resulting product is produced with Japanese firm is observed, is schemed from SEM
In it can be seen that prepared product in hollow sphere and the compound structure of flake graphite alkene, it is apparent that hollow sphere be by
Smaller unit self assembly forms, and is attached to the surface of graphene, sees Fig. 1 and Fig. 2.
Resulting product is prepared into button-shaped lithium ion battery, specific encapsulation step is as follows: by activity powder, conductive agent
Slurry is made after bonding agent (carboxyl methyl cellulose) is according to the proportion grinding uniformly that mass ratio is 8:1:1 in (Super P),
Equably slurry is applied on copper foil with coating device, then in 80 DEG C of vacuum oven dry 12h.Electrode slice is assembled into later
Lithium ion half-cell carries out constant current charge-discharge test, test voltage 0.01V- to battery using new prestige electrochemical workstation
3.0V, test current density size are 200mA/g, and test result is shown in Fig. 3, and after the circulation of 50 circles, battery can still be protected
Hold the capacity of 1201 mAh/g, it is seen that the stable cycle performance of the product with hollow ball structure, and have the tendency that slowly rising.
Embodiment 2
(1) it adds graphene oxide into deionized water mixed liquor, ultrasonic shear 60min, it is 1.5mg/ that concentration, which is made,
The suspension A of mL;
(2) then CTAB is added in suspension A under conditions of keeping stirring, up to the concentration of CTAB in suspension A
For 0.05g/L, then proceedes to stirring after twenty minutes, obtain mixed liquid B;
(3) analytically pure soluble divalent iron salt ferrous acetate is added in suspension B, stirs 30min, obtains ferrous iron
Ion concentration is the mixture C of 0.3mol/L;
(4) then by mixed liquor C 2mol/L salt acid for adjusting pH value to 5, mixture D is obtained;
(5) mixture D being put into and is poured into microwave hydrothermal reaction kettle, volume compactedness is 60%, reaction kettle is then sealed,
It puts it into microwave hydrothermal reaction, selects temperature control mode to be reacted, be warming up to 160 with the heating rate of 20 DEG C/min
DEG C, reaction time 1h naturally cools to room temperature after reaction, obtains product E;
(6) product E is then used into deionized water respectively, dehydrated alcohol washs for several times, does at 60 DEG C in a vacuum drying oven
Dry 12h obtains hollow sphere Fe2O3/ rGO lithium ion battery negative material.
By ultrasonic synthetic method, the short time can prepare the lithium ion of electrochemical performance to the present invention at low temperature
Cell negative electrode material.
Embodiment 3
A kind of hollow sphere Fe2O3The preparation method of/rGO lithium ion battery negative material, comprising the following steps:
1) it adds graphene oxide into deionized water, ultrasonic shear 20min, it is the suspended of 0.5mg/mL that concentration, which is made,
Liquid A;
2) CTAB is added in suspension A under continuous agitation, until the concentration of CTAB is in suspension A
0.001 g/L then proceedes to stirring after ten minutes, obtains mixed liquid B;
3) ferrous sulfate is added in mixed liquid B, stirs 10min, obtaining ferrous ion concentration is the mixed of 0.01mol/L
Close object C;
4) pH value of mixed liquor C is adjusted to 2 using 2mol/L hydrochloric acid, obtains mixture D;
5) by mixture D in microwave hydrothermal reaction, temperature control mode is selected to be reacted, with the heating speed of 20 DEG C/min
Rate is warming up to 180 DEG C, and reaction time 0.5h obtains product E;
6) product E is washed using deionized water and dehydrated alcohol, the dry 12h at 60 DEG C, obtains in a vacuum drying oven
To hollow sphere Fe2O3/ rGO lithium ion battery negative material.
Embodiment 4
A kind of hollow sphere Fe2O3The preparation method of/rGO lithium ion battery negative material, comprising the following steps:
1) it adds graphene oxide into deionized water, ultrasonic shear 30min, the suspension that concentration is 2mg/mL is made
A;
2) CTAB is added in suspension A under continuous agitation, until the concentration of CTAB is in suspension A
0.2g/L obtains mixed liquid B after then proceeding to stirring 30 minutes;
3) frerrous chloride is added in mixed liquid B, stirs 40min, obtaining ferrous ion concentration is the mixed of 0.5mol/L
Close object C;
4) pH value of mixed liquor C is adjusted to 7 using 2mol/L hydrochloric acid, obtains mixture D;
5) by mixture D in microwave hydrothermal reaction, temperature control mode is selected to be reacted, with the heating speed of 15 DEG C/min
Rate is warming up to 140 DEG C, and reaction time 3h obtains product E;
6) product E is washed using deionized water and dehydrated alcohol, the dry 12h at 60 DEG C, obtains in a vacuum drying oven
To hollow sphere Fe2O3/ rGO lithium ion battery negative material.
Embodiment 5
A kind of hollow sphere Fe2O3The preparation method of/rGO lithium ion battery negative material, comprising the following steps:
1) it adds graphene oxide into deionized water, ultrasonic shear 50min, it is the suspended of 1.8mg/mL that concentration, which is made,
Liquid A;
2) CTAB is added in suspension A under continuous agitation, until the concentration of CTAB is 0.1 in suspension A
G/L obtains mixed liquid B after then proceeding to stirring 15 minutes;
3) ferrous sulfate is added in mixed liquid B, stirs 60min, obtaining ferrous ion concentration is 0.061mol/L's
Mixture C;
4) pH value of mixed liquor C is adjusted to 6 using 2mol/L hydrochloric acid, obtains mixture D;
5) by mixture D in microwave hydrothermal reaction, temperature control mode is selected to be reacted, with the heating speed of 10 DEG C/min
Rate is warming up to 150 DEG C, and reaction time 2h obtains product E;
6) product E is washed using deionized water and dehydrated alcohol, the dry 12h at 60 DEG C, obtains in a vacuum drying oven
To hollow sphere Fe2O3/ rGO lithium ion battery negative material.
Claims (3)
1. a kind of hollow sphere Fe2O3The preparation method of/rGO lithium ion battery negative material, which comprises the following steps:
1) it adds graphene oxide into deionized water, is uniformly mixed, it is the suspended of 0.5mg/mL~2mg/mL that concentration, which is made,
Liquid A;Wherein, being uniformly mixed is realized by ultrasonic shear 10min~90min;
2) under continuous agitation by CTAB be added suspension A in, until suspension A in CTAB concentration be 0.001~
0.2g/L obtains mixed liquid B after then proceeding to stirring 10~30 minutes;
3) soluble divalent iron salt is added in mixed liquid B, stirs 10~60min, obtaining ferrous ion concentration is
The mixture C of 0.01mol/L~0.5mol/L;Wherein, soluble divalent iron salt is that ferrous sulfate, frerrous chloride or acetic acid are sub-
Iron;
4) pH value of mixed liquor C is adjusted to 2~7 using hydrochloric acid, obtains mixture D;
5) by mixture D in microwave hydrothermal reaction, temperature control mode is selected to be reacted, with the heating speed of 10~20 DEG C/min
Rate is warming up to 120~180 DEG C, reacts 0.5~3h, obtains product E;
6) by product E washing, drying, hollow sphere Fe is obtained2O3/ rGO lithium ion battery negative material;The material be hollow sphere with
The compound structure of flake graphite alkene, hollow sphere are formed by unit self assembly, and the surface of graphene is attached to.
2. a kind of hollow sphere Fe according to claim 12O3The preparation method of/rGO lithium ion battery negative material, it is special
Sign is that the concentration of hydrochloric acid is 2mol/L.
3. a kind of hollow sphere Fe according to claim 12O3The preparation method of/rGO lithium ion battery negative material, it is special
Sign is, washs product E using deionized water and dehydrated alcohol in step 6), dry at 60 DEG C in a vacuum drying oven
12h。
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CN106854389B (en) * | 2017-01-11 | 2020-06-26 | 山东欧铂新材料有限公司 | Mica iron oxide/graphene oxide composite material and preparation method thereof |
CN108314029B (en) * | 2018-01-18 | 2019-03-12 | 东莞理工学院 | Hollow bowl-shape graphene oxide micro motor and preparation method thereof |
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