CN107394148A - A kind of preparation method of the sandwich lamellar structure lithium ion battery negative materials of graphene-supported α FeOOH - Google Patents
A kind of preparation method of the sandwich lamellar structure lithium ion battery negative materials of graphene-supported α FeOOH Download PDFInfo
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- CN107394148A CN107394148A CN201710568022.1A CN201710568022A CN107394148A CN 107394148 A CN107394148 A CN 107394148A CN 201710568022 A CN201710568022 A CN 201710568022A CN 107394148 A CN107394148 A CN 107394148A
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- feooh
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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
- H01M4/366—Composites as layered products
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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
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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
- H01M4/58—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
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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
A kind of preparation method of the sandwich lamellar structure lithium ion battery negative materials of graphene-supported α FeOOH, graphene oxide is disperseed to obtain suspension A in deionized water；Salt ferric nitrate is added in deionized water and then suspension B is mixed to obtain with suspension A；Suspension B is poured into homogeneous hydrothermal reaction kettle, then seals reactor, is put it into and is naturally cooled to room temperature after hydro-thermal reaction in homogeneous hydro-thermal reaction instrument and obtain product C；Product C is washed with washing, alcohol respectively, the product after washing is dispersed in water to obtain product D；Product D is freeze-dried to obtain the graphene-supported α FeOOH compounds of sandwich lamellar structure.Because graphene conductive is good, there is larger specific surface area, loaded with it, α FeOOH electric conductivity can be significantly improved, while improve α FeOOH dispersiveness, avoid reuniting.The present invention combines ultrasonic wave added method and homogeneous hydro-thermal method, by improving material conductivity by α FeOOH and graphene are compound, improvement chemical property.Make battery structure more stable, so as to improve the stable circulation performance of battery.
Description
Technical field
The invention belongs to electrochemical technology field, and in particular to a kind of graphene-supported sandwich lamellar structure lithium of alpha-feooh
The preparation method of ion battery cathode material.
Background technology
Alpha-feooh (goethite type FeOOH) is part important in ferriferous oxide, due to its high power capacity (>
1000mAh/g), abundant natural resources, nontoxicity and low cost, are considered as that having for negative material of new generation is uncommon for a long time
The candidate of prestige.But, alpha-feooh conductive difference the same with most of oxide electrodes, volumetric expansion is bright during discharge and recharge
It is aobvious, and then cause active material efflorescence to be come off from collection liquid surface, and cause electrode capacity drastically to decline.Zhang Meng et al.
(Journal of Alloys and Compounds, 2015,648,134-138) is reactant 80 using iron chloride and urea
Reaction 4h obtains FeOOH under DEG C hydrothermal condition, and material conductivity is poor, and specific capacity needs further to be improved；Zhai Yan person of outstanding talent et al.
(Journal of Power Sources, 2016,327,423-431) using iron chloride and cerous nitrate as raw material, PVP etc. is surface
Activating agent, Ce is adulterated on alpha-feooh to improve the cycle performance of material.
The content of the invention
It is an object of the invention to provide one kind by the way that alpha-feooh and graphene is compound so as to improve material conductivity,
Improve the preparation method of the sandwich lamellar structure lithium ion battery negative material of graphene-supported alpha-feooh of chemical property.
To reach above-mentioned purpose, the technical solution adopted by the present invention is：
1) commercially available graphene oxide is dispersed in the solution that 1~5mg/mL is configured in 25~40mL deionized waters, so
Finely dispersed graphene oxide suspension A is formed using ultrasonic generator afterwards；
2) analytically pure soluble ferric iron salt ferric nitrate is added in 10~25mL deionized waters, stirring makes molysite fully molten
Solution, is then added in suspension A, is configured to the mixed solution of molysite and graphene oxide, and the wherein concentration of molysite is 0.05
~0.5mol/L, mixed solution is then disperseed into obtain suspension B using ultrasonic generator；
3) the suspension B of above-mentioned preparation is poured into homogeneous hydrothermal reaction kettle, then seals reactor, put it into homogeneous
Hydro-thermal reaction is carried out in hydro-thermal reaction instrument at 50~150 DEG C, reaction naturally cools to room temperature after terminating and obtains product C；
4) product C is washed with washing, alcohol respectively, the product after washing is dispersed in water to obtain product D；
5) product D is freeze-dried at -20~-50 DEG C, holding vacuum is 10~60Pa, and dried sample is
The sandwich graphene-supported alpha-feooh compound of lamellar structure.
The power of step 1) the excusing from death generator is 300W, and ultrasonic time is 1~3h.
The power of step 2) the excusing from death generator is 300W, and ultrasonic time is 2~5h.
Step 3) the hydrothermal reaction kettle compactedness is 30%~80%.
Step 3) the hydro-thermal reaction time is 2~5h.
The washing of the step 4) is washed respectively using centrifuge, alcohol is washed 3 times, each 1~4min of centrifugation time, and centrifugation turns
Speed is 3000~9000rpm.
Step 5) the drying time is 10~20h.
Because graphene conductive is good, there is larger specific surface area, loaded with it, alpha-feooh can be significantly improved
Electric conductivity, while the dispersiveness of alpha-feooh is improved, avoid reuniting.The present invention combines ultrasonic wave added method and homogeneous hydro-thermal method, passes through
Material conductivity is improved by alpha-feooh and graphene are compound, improves chemical property.Can effectively it be solved by graphene-supported its
Certainly the problem of alpha-feooh poorly conductive, and can suppresses volumetric expansion, makes battery structure more stable, so as to improve following for battery
Ring stability.
Beneficial effects of the present invention are embodied in：
1) present invention is to improve the electric conductivity of product, for the purpose of alleviating volumetric expansion, and then be prepared for graphene-supported α-
The sandwich lamella compounds of FeOOH.Under 0.2A/g electric current, electric discharge first has reached 1000~1350mAh/g, by 5A/g's
After heavy current impact, capacity restoration to 800~1000mAh/g；And under 0.2C multiplying powers, the capacity stabilization after 100 circle circulations exists
500~600mAh/g.
2) present invention combines ultrasonic wave added method and homogeneous hydro-thermal method, using the coordination of molysite and graphene oxide, realizes
Alpha-feooh and then forms the sandwich lamellar structure of graphene-supported alpha-feooh, experiment side in the growth in situ of graphenic surface
Method is simple, and cost is cheap, it is easy to accomplish.
Brief description of the drawings
Fig. 1 is that product particles prepared by the embodiment of the present invention 1 are analyzed with Rigaku D/max2000PCX- x ray diffractometer xs
Sample drawing；
Fig. 2, Fig. 3 and Fig. 4, it is the JSM-6700F types scanning that the sample of the preparation of the embodiment of the present invention 1 is produced with Japanese firm
Electron micrograph；
Fig. 5 be the embodiment of the present invention 1 prepare sample preparation into button-shaped lithium ion battery chemical property figure.
Embodiment
Embodiment 1：
1) commercially available graphene oxide is dispersed in the solution that 1mg/mL is configured in 25mL deionized waters, then used
300W ultrasonic generator ultrasonic disperse 1h, form finely dispersed graphene oxide suspension A；
2) analytically pure soluble ferric iron salt ferric nitrate being added in 25mL deionized waters, stirring makes molysite fully dissolve,
It is then added in suspension A, is configured to the mixed solution of molysite and graphene oxide, the wherein concentration of molysite is 0.05mol/
L, mixed solution is then disperseed into 2h using 300W ultrasonic generator and obtains suspension B；
3) the suspension B of above-mentioned preparation is poured into homogeneous hydrothermal reaction kettle, compactedness 30%, then sealing reaction
Kettle, puts it into and carries out hydro-thermal reaction 5h in homogeneous hydro-thermal reaction instrument at 50 DEG C, and reaction naturally cools to room temperature after terminating and must produced
Thing C；
4) product C is washed respectively using centrifuge, alcohol is washed 3 times, each centrifugation time 1min, centrifugal rotational speed is
3000rpm, the product after washing is dispersed in water to obtain product D；
5) product D is freeze-dried at -20 DEG C, holding vacuum is 10Pa, dries 10h, and dried sample is
The sandwich graphene-supported alpha-feooh compound of lamellar structure.
Product is goethite type FeOOH, card serial number PDF#29-0713 as seen from Figure 1.
The sandwich lamella compound of made graphene-supported alpha-feooh can be seen that by Fig. 2, Fig. 3 and Fig. 4, while α-
FeOOH particles are wrapped up by graphene uniform, and enwrapped granule size is 1~2um, is evenly distributed on graphene sheet layer, graphene
The stacking that intersected between lamella forms various sizes of hole again.
The product of the gained of embodiment 1 is prepared into button-shaped lithium ion battery, specific encapsulation step is as follows：By activity
Powder, conductive agent (Super P), bonding agent (carboxyl methyl cellulose) are 8 according to mass ratio:1:After 1 proportioning grinding uniformly,
Slurry is made, equably slurry is applied on copper foil with coating device, then in 80 DEG C of dry 12h of vacuum drying chamber.Afterwards by electricity
Pole piece is assembled into lithium ion half-cell, and constant current charge-discharge test, test voltage are carried out to battery using new prestige electrochemical workstation
For 0.01V-3.0V, test result is shown in Fig. 5, when it be 0.2C to test multiplying power, discharges reached 1200mAh/g first, through 0.5C,
Under 1C, 2C, 5C different multiplying after charge and discharge cycles, when multiplying power reverts to 0.5C, capacity restoration is to 900mAh/g.
Embodiment 2：
1) commercially available graphene oxide is dispersed in the solution that 2mg/mL is configured in 30mL deionized waters, then used
300W ultrasonic generator ultrasonic disperse 3h, form finely dispersed graphene oxide suspension A；
2) analytically pure soluble ferric iron salt ferric nitrate being added in 20mL deionized waters, stirring makes molysite fully dissolve,
It is then added in suspension A, is configured to the mixed solution of molysite and graphene oxide, the wherein concentration of molysite is 0.3mol/
L, mixed solution is then disperseed into 3h using 300W ultrasonic generator and obtains suspension B；
3) the suspension B of above-mentioned preparation is poured into homogeneous hydrothermal reaction kettle, compactedness 80%, then sealing reaction
Kettle, puts it into and carries out hydro-thermal reaction 4h in homogeneous hydro-thermal reaction instrument at 70 DEG C, and reaction naturally cools to room temperature after terminating and must produced
Thing C；
4) product C is washed respectively using centrifuge, alcohol is washed 3 times, each centrifugation time 4min, centrifugal rotational speed is
4000rpm, the product after washing is dispersed in water to obtain product D；
5) product D is freeze-dried at -30 DEG C, holding vacuum is 60Pa, dries 15h, and dried sample is
The sandwich graphene-supported alpha-feooh compound of lamellar structure.
Embodiment 3：
1) commercially available graphene oxide is dispersed in the solution that 5mg/mL is configured in 35mL deionized waters, then used
300W ultrasonic generator ultrasonic disperse 2h, form finely dispersed graphene oxide suspension A；
2) analytically pure soluble ferric iron salt ferric nitrate being added in 15mL deionized waters, stirring makes molysite fully dissolve,
It is then added in suspension A, is configured to the mixed solution of molysite and graphene oxide, the wherein concentration of molysite is 0.5mol/
L, mixed solution is then disperseed into 4h using 300W ultrasonic generator and obtains suspension B；
3) the suspension B of above-mentioned preparation is poured into homogeneous hydrothermal reaction kettle, compactedness 60%, then sealing reaction
Kettle, puts it into and carries out hydro-thermal reaction 3h in homogeneous hydro-thermal reaction instrument at 150 DEG C, and reaction naturally cools to room temperature after terminating and must produced
Thing C；
4) product C is washed respectively using centrifuge, alcohol is washed 3 times, each centrifugation time 2min, centrifugal rotational speed is
5000rpm, the product after washing is dispersed in water to obtain product D；
5) product D is freeze-dried at -50 DEG C, holding vacuum is 25Pa, dries 20h, and dried sample is
The sandwich graphene-supported alpha-feooh compound of lamellar structure.
Embodiment 4：
1) commercially available graphene oxide is dispersed in the solution that 3mg/mL is configured in 40mL deionized waters, then used
300W ultrasonic generator ultrasonic disperse 3h, form finely dispersed graphene oxide suspension A；
2) analytically pure soluble ferric iron salt ferric nitrate being added in 10mL deionized waters, stirring makes molysite fully dissolve,
It is then added in suspension A, is configured to the mixed solution of molysite and graphene oxide, the wherein concentration of molysite is 0.1mol/
L, mixed solution is then disperseed into 5h using 300W ultrasonic generator and obtains suspension B；
3) the suspension B of above-mentioned preparation is poured into homogeneous hydrothermal reaction kettle, compactedness 80%, then sealing reaction
Kettle, puts it into and carries out hydro-thermal reaction 2h in homogeneous hydro-thermal reaction instrument at 100 DEG C, and reaction naturally cools to room temperature after terminating and must produced
Thing C；
4) product C is washed respectively using centrifuge, alcohol is washed 3 times, each centrifugation time 1min, centrifugal rotational speed is
9000rpm, the product after washing is dispersed in water to obtain product D；
5) product D is freeze-dried at -40 DEG C, holding vacuum is 40Pa, dries 10h, and dried sample is
The sandwich graphene-supported alpha-feooh compound of lamellar structure.
Claims (7)
1. a kind of preparation method of the sandwich lamellar structure lithium ion battery negative material of graphene-supported alpha-feooh, its feature exist
In：
1) commercially available graphene oxide is dispersed in the solution that 1~5mg/mL is configured in 25~40mL deionized waters, then adopted
Finely dispersed graphene oxide suspension A is formed with ultrasonic generator；
2) analytically pure soluble ferric iron salt ferric nitrate being added in 10~25mL deionized waters, stirring makes molysite fully dissolve,
Be then added in suspension A, be configured to the mixed solution of molysite and graphene oxide, wherein the concentration of molysite be 0.05~
0.5mol/L, mixed solution is then disperseed into obtain suspension B using ultrasonic generator；
3) the suspension B of above-mentioned preparation is poured into homogeneous hydrothermal reaction kettle, then seals reactor, put it into homogeneous hydro-thermal
React and carry out hydro-thermal reaction in instrument at 50~150 DEG C, reaction naturally cools to room temperature after terminating and obtains product C；
4) product C is washed with washing, alcohol respectively, the product after washing is dispersed in water to obtain product D；
5) product D is freeze-dried at -20~-50 DEG C, holding vacuum is 10~60Pa, and dried sample is as sandwich
The graphene-supported alpha-feooh compound of lamellar structure.
2. the system of the sandwich lamellar structure lithium ion battery negative material of graphene-supported alpha-feooh according to claim 1
Preparation Method, it is characterised in that：The power of step 1) the excusing from death generator is 300W, and ultrasonic time is 1~3h.
3. the system of the sandwich lamellar structure lithium ion battery negative material of graphene-supported alpha-feooh according to claim 1
Preparation Method, it is characterised in that：The power of step 2) the excusing from death generator is 300W, and ultrasonic time is 2~5h.
4. the system of the sandwich lamellar structure lithium ion battery negative material of graphene-supported alpha-feooh according to claim 1
Preparation Method, it is characterised in that：Step 3) the hydrothermal reaction kettle compactedness is 30%~80%.
5. the system of the sandwich lamellar structure lithium ion battery negative material of graphene-supported alpha-feooh according to claim 1
Preparation Method, it is characterised in that：Step 3) the hydro-thermal reaction time is 2~5h.
6. the system of the sandwich lamellar structure lithium ion battery negative material of graphene-supported alpha-feooh according to claim 1
Preparation Method, it is characterised in that：The washing of the step 4) is washed respectively using centrifuge, alcohol is washed 3 times, and each centrifugation time 1~
4min, centrifugal rotational speed are 3000~9000rpm.
7. the system of the sandwich lamellar structure lithium ion battery negative material of graphene-supported alpha-feooh according to claim 1
Preparation Method, it is characterised in that：Step 5) the drying time is 10~20h.
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Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN108365192A (en) * | 2018-01-25 | 2018-08-03 | 陕西科技大学 | A kind of α-Fe2O3The preparation method of@alpha-feoohs/rGO composite cathode material for lithium ion cell |
| CN109449422A (en) * | 2018-11-12 | 2019-03-08 | 东北师范大学 | FeOOH nanometer rods/graphene oxide composite material and the preparation method and application thereof |
| CN112933897A (en) * | 2021-01-28 | 2021-06-11 | 深圳市普瑞美泰环保科技有限公司 | Air purification device, manufacturing method thereof and air purification method |
| CN113426465A (en) * | 2021-05-20 | 2021-09-24 | 浙江理工大学 | g-C3N4@ FeOOH heterojunction material and preparation method thereof |
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| CN106356525A (en) * | 2016-08-25 | 2017-01-25 | 陕西科技大学 | Method for preparing graphene in-situ growth FeOOH nano array lithium ion battery cathode material |
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2017
- 2017-07-13 CN CN201710568022.1A patent/CN107394148A/en active Pending
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| Publication number | Priority date | Publication date | Assignee | Title |
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| CN106356525A (en) * | 2016-08-25 | 2017-01-25 | 陕西科技大学 | Method for preparing graphene in-situ growth FeOOH nano array lithium ion battery cathode material |
Non-Patent Citations (1)
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| YUXUE WEI,ET AL.: ""Facile synthesis of self-assembled ultrathin α-FeOOH nanorod/graphene oxide composites for supercapacitors"", 《JOURNAL OF COLLOID AND INTERFACE SCIENCE》 * |
Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN108365192A (en) * | 2018-01-25 | 2018-08-03 | 陕西科技大学 | A kind of α-Fe2O3The preparation method of@alpha-feoohs/rGO composite cathode material for lithium ion cell |
| CN109449422A (en) * | 2018-11-12 | 2019-03-08 | 东北师范大学 | FeOOH nanometer rods/graphene oxide composite material and the preparation method and application thereof |
| CN112933897A (en) * | 2021-01-28 | 2021-06-11 | 深圳市普瑞美泰环保科技有限公司 | Air purification device, manufacturing method thereof and air purification method |
| CN113426465A (en) * | 2021-05-20 | 2021-09-24 | 浙江理工大学 | g-C3N4@ FeOOH heterojunction material and preparation method thereof |
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