CN107170985A - A kind of preparation method of lithium ion battery activation three-dimensional grapheme/nickel foam - Google Patents
A kind of preparation method of lithium ion battery activation three-dimensional grapheme/nickel foam Download PDFInfo
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- CN107170985A CN107170985A CN201710334555.3A CN201710334555A CN107170985A CN 107170985 A CN107170985 A CN 107170985A CN 201710334555 A CN201710334555 A CN 201710334555A CN 107170985 A CN107170985 A CN 107170985A
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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
- 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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- 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 relates to a kind of preparation method of lithium ion battery with activation three-dimensional grapheme/nickel foam, it is by the way that nickel foam is immersed in graphene oxide water solution, with the deposited oxide graphene in nickel foam, gained three-dimensional graphene oxide/foam nickel material is impregnated in KOH aqueous slkalis again to be activated, finally mixture is placed in tube furnace and calcined, that is, is obtained for activation three-dimensional grapheme/nickel foam as lithium ion battery negative material.The preparation method of the present invention, not only remains the intrinsic property of two-dimensional graphene piece, and surface produces substantial amounts of nano micropore structure, and resulting materials have bigger specific surface area, so as to significantly improve performance of lithium ion battery;Technique of the invention is simple, the reaction time is short, is adapted to industrialized production.
Description
Technical field
The invention belongs to technical field of lithium ion, and in particular to and a kind of lithium ion battery use activation three-dimensional grapheme/
The preparation method of nickel foam.
Background technology
Graphene individual layer two-dimensional material is because with bigger serface, high electrical conductivity and thermal conductivity and outstanding mechanicalness
Can, cause the extensive concern of people.Graphene is widely used in lithium ion battery, ultracapacitor and solar cell etc.
In energy storage device.There are very strong π-π between layers yet with graphene to interact and Van der Waals for, cause stone
Black alkene lamella would generally reunite and stack, and thus can greatly reduce the effective area of graphene, so that it is applied
Potential is had a greatly reduced quality.
The content of the invention
There is provided a kind of lithium ion battery activation three-dimensional graphite for weak point of the present invention present in prior art
The preparation method of alkene/nickel foam, it is intended to prepare high performance lithium ion battery.
The goal of the invention of the present invention is achieved by following technical solution.
The lithium ion battery of the present invention preparation method of activation three-dimensional grapheme/nickel foam, comprises the following steps:
1) by graphene oxide ultrasonic disperse in water, graphene oxide water solution is obtained;Then nickel foam is immersed in
In the graphene oxide water solution, with the deposited oxide graphene in nickel foam, three-dimensional graphene oxide/nickel foam material is obtained
Material;
2) the three-dimensional graphene oxide/foam nickel material is impregnated in KOH solution, taken out after standing 24-48 hours,
Obtain activating three-dimensional graphene oxide/foam nickel material;
3) the three-dimensional graphene oxide/foam nickel material of the activation is placed in tube furnace, is warming up to 300-800 DEG C, perseverance
Temperature reaction 1-3 hours, then naturally cools to room temperature;Products therefrom is washed with water to neutrality, then the 40-60 in air dry oven
DEG C drying 3-6 hours, that is, obtain for activation three-dimensional grapheme/nickel foam as lithium ion battery negative material.
It is preferred that, step 1) described in graphene oxide water solution concentration be 0.5-6mg/mL.
It is preferred that, step 2) described in KOH solution concentration be 2-6mol/L.
It is preferred that, step 3) in heating rate be 5-10 DEG C/min.
The nickel foam is in the method for the invention as templated deposition three-dimensional grapheme.
Compared with the prior art, beneficial effects of the present invention are embodied in:
The preparation method of present invention activation three-dimensional grapheme/nickel foam, not only remains the inherency of two-dimensional graphene piece
Matter, and surface produces substantial amounts of nano micropore structure, and resulting materials have bigger specific surface area, are electrons/ions, gas
Body and liquid transmission and storage provide more spaces, so as to significantly improve performance of lithium ion battery;The technique of the present invention is simple,
Reaction time is short, is adapted to industrialized production.
Brief description of the drawings
Fig. 1 is the SEM figures of the gained activation three-dimensional grapheme/nickel foam negative material of the embodiment of the present invention 1;
Fig. 2 is the SEM figures of the gained activation three-dimensional grapheme/nickel foam negative material of the embodiment of the present invention 2;
Fig. 3 is the SEM figures of the gained activation three-dimensional grapheme/nickel foam negative material of the embodiment of the present invention 3;
Fig. 4 is the SEM figures of the gained activation three-dimensional grapheme/nickel foam negative material of the embodiment of the present invention 4;
Fig. 5 is the SEM figures of the gained activation three-dimensional grapheme/nickel foam negative material of the embodiment of the present invention 5;
Fig. 6 is the SEM figures of the gained activation three-dimensional grapheme/nickel foam negative material of the embodiment of the present invention 6;
Fig. 7 is the charging and discharging curve figure of the gained activation three-dimensional grapheme/nickel foam negative material of the embodiment of the present invention 7;
Fig. 8 is the charging and discharging curve figure of the gained activation three-dimensional grapheme/nickel foam negative material of the embodiment of the present invention 8;
Fig. 9 is the charging and discharging curve figure of the gained activation three-dimensional grapheme/nickel foam negative material of the embodiment of the present invention 9;
Figure 10 is the charging and discharging curve figure of the gained activation three-dimensional grapheme/nickel foam negative material of the embodiment of the present invention 10.
Embodiment
Embodiments of the invention are elaborated below, the present embodiment is carried out lower premised on technical solution of the present invention
Implement, give detailed embodiment and specific operating process, but protection scope of the present invention is not limited to following implementations
Example.
Embodiment 1
The present embodiment prepares lithium ion battery activation three-dimensional grapheme/nickel foam as follows:
1) by graphene oxide ultrasonic disperse in water, 2mg/mL graphene oxide water solution is obtained;Then by 0.16g
Nickel foam is immersed in 10mL graphene oxide water solutions, with the deposited oxide graphene in nickel foam, obtains three-dimensional oxidation stone
Black alkene/foam nickel material;
2) three-dimensional graphene oxide/foam nickel material is impregnated in 3mol/L KOH solution, taken after standing 48 hours
Go out, obtain activating three-dimensional graphene oxide/foam nickel material;
3) the three-dimensional graphene oxide/foam nickel material of activation is placed in tube furnace, heated up with 5 DEG C/min heating rate
To 300 DEG C, then isothermal reaction 1 hour naturally cools to room temperature;Products therefrom is washed with water to neutrality, then in forced air drying
Dried 6 hours for 60 DEG C in case, that is, obtain activating three-dimensional grapheme/nickel foam negative material.
Fig. 1 schemes for the SEM of the present embodiment products therefrom.
Performance test is carried out as follows to the present embodiment products therefrom:By the activation three-dimensional grapheme of above-mentioned acquisition/
Nickel foam negative material is transferred in glove box, using lithium piece as to electrode and reference electrode, using celgard2400 barrier films,
Electrolyte is 1mol/L LiPF6- EC+DMC+EMC (volume ratios 1:1:1), by negative electrode casing-lithium piece-barrier film-positive plate-steel disc-
The order of spring-anode cover is sequentially placed, and with hand-hydraulic sealing machine under 50Mpa pressure by battery seal, finally assemble
Into CR2032 type button half-cells, 20 circulations are then carried out under current density 50mA/g by the new prestige cell tester in Shenzhen
Performance test.
As a result show, the first discharge specific capacity of the present embodiment products therefrom is that 145mAh/g, charge specific capacity are
Specific discharge capacity is that 100mAh/g, charge specific capacity are 98mAh/g after 108mAh/g, circulation 20 times.
Embodiment 2
The present embodiment prepares lithium ion battery activation three-dimensional grapheme/nickel foam as follows:
1) by graphene oxide ultrasonic disperse in water, 2mg/mL graphene oxide water solution is obtained;Then by 0.16g
Nickel foam is immersed in 10mL graphene oxide water solutions, with the deposited oxide graphene in nickel foam, obtains three-dimensional oxidation stone
Black alkene/foam nickel material;
2) three-dimensional graphene oxide/foam nickel material is impregnated in 6mol/L KOH solution, taken after standing 48 hours
Go out, obtain activating three-dimensional graphene oxide/foam nickel material;
3) the three-dimensional graphene oxide/foam nickel material of activation is placed in tube furnace, heated up with 5 DEG C/min heating rate
To 300 DEG C, then isothermal reaction 1 hour naturally cools to room temperature;Products therefrom is washed with water to neutrality, then in forced air drying
Dried 6 hours for 60 DEG C in case, that is, obtain activating three-dimensional grapheme/nickel foam negative material.
Fig. 2 schemes for the SEM of the present embodiment products therefrom.
Performance test is carried out to the product of the present embodiment by the identical method of embodiment 1, as a result shown, its ratio that discharges first
Capacity is that 125mAh/g, charge specific capacity are 92mAh/g, and specific discharge capacity is that 86mAh/g, charge specific capacity are after circulation 20 times
85mAh/g。
Embodiment 3
The present embodiment prepares lithium ion battery activation three-dimensional grapheme/nickel foam as follows:
1) by graphene oxide ultrasonic disperse in water, 4mg/mL graphene oxide water solution is obtained;Then by 0.16g
Nickel foam is immersed in 10mL graphene oxide water solutions, with the deposited oxide graphene in nickel foam, obtains three-dimensional oxidation stone
Black alkene/foam nickel material;
2) three-dimensional graphene oxide/foam nickel material is impregnated in 3mol/L KOH solution, taken after standing 48 hours
Go out, obtain activating three-dimensional graphene oxide/foam nickel material;
3) the three-dimensional graphene oxide/foam nickel material of activation is placed in tube furnace, heated up with 5 DEG C/min heating rate
To 300 DEG C, then isothermal reaction 1 hour naturally cools to room temperature;Products therefrom is washed with water to neutrality, then in forced air drying
Dried 6 hours for 60 DEG C in case, that is, obtain activating three-dimensional grapheme/nickel foam negative material.
Fig. 3 schemes for the SEM of the present embodiment products therefrom.
Performance test is carried out to the product of the present embodiment by the identical method of embodiment 1, as a result shown, its ratio that discharges first
Capacity is that 195mAh/g, charge specific capacity are 158mAh/g, and specific discharge capacity is 128mAh/g, charge specific capacity after circulation 20 times
For 124mAh/g.
Embodiment 4
The present embodiment prepares lithium ion battery activation three-dimensional grapheme/nickel foam as follows:
1) by graphene oxide ultrasonic disperse in water, 4mg/mL graphene oxide water solution is obtained;Then by 0.16g
Nickel foam is immersed in 10mL graphene oxide water solutions, with the deposited oxide graphene in nickel foam, obtains three-dimensional oxidation stone
Black alkene/foam nickel material;
2) three-dimensional graphene oxide/foam nickel material is impregnated in 6mol/L KOH solution, taken after standing 48 hours
Go out, obtain activating three-dimensional grapheme/foam nickel material;
3) the three-dimensional graphene oxide/foam nickel material of activation is placed in tube furnace, heated up with 5 DEG C/min heating rate
To 300 DEG C, then isothermal reaction 1 hour naturally cools to room temperature;Products therefrom is washed with water to neutrality, then in forced air drying
Dried 6 hours for 60 DEG C in case, that is, obtain activating three-dimensional grapheme/nickel foam negative material.
Fig. 4 schemes for the SEM of the present embodiment products therefrom.
Performance test is carried out to the product of the present embodiment by the identical method of embodiment 1, as a result shown, its ratio that discharges first
Capacity is that 76mAh/g, charge specific capacity are 152mAh/g, and specific discharge capacity is 121mAh/g, charge specific capacity after circulation 20 times
For 116mAh/g.
Embodiment 5
The present embodiment prepares lithium ion battery activation three-dimensional grapheme/nickel foam as follows:
1) by graphene oxide ultrasonic disperse in water, 6mg/mL graphene oxide water solution is obtained;Then by 0.16g
Nickel foam is immersed in 10mL graphene oxide water solutions, with the deposited oxide graphene in nickel foam, obtains three-dimensional oxidation stone
Black alkene/foam nickel material;
2) three-dimensional graphene oxide/foam nickel material is impregnated in 3mol/L KOH solution, taken after standing 48 hours
Go out, obtain activating three-dimensional graphene oxide/foam nickel material;
3) the three-dimensional graphene oxide/foam nickel material of activation is placed in tube furnace, heated up with 5 DEG C/min heating rate
To 300 DEG C, then isothermal reaction 1 hour naturally cools to room temperature;Products therefrom is washed with water to neutrality, then in forced air drying
Dried 6 hours for 60 DEG C in case, that is, obtain activating three-dimensional grapheme/nickel foam negative material.
Fig. 5 schemes for the SEM of the present embodiment products therefrom.
Performance test is carried out to the product of the present embodiment by the identical method of embodiment 1, as a result shown:Its ratio that discharges first
Capacity is that 239mAh/g, charge specific capacity are 188mAh/g, and specific discharge capacity is 150mAh/g, charge specific capacity after circulation 20 times
For 146mAh/g.
Embodiment 6
The present embodiment prepares lithium ion battery activation three-dimensional grapheme/nickel foam as follows:
1) by graphene oxide ultrasonic disperse in water, 6mg/mL graphene oxide water solution is obtained;Then by 0.16g
Nickel foam is immersed in 10mL graphene oxide water solutions, with the deposited oxide graphene in nickel foam, obtains three-dimensional oxidation stone
Black alkene/foam nickel material;
2) three-dimensional graphene oxide/foam nickel material is impregnated in 6mol/L KOH solution, taken after standing 48 hours
Go out, obtain activating three-dimensional graphene oxide/foam nickel material;
3) the three-dimensional graphene oxide/foam nickel material of activation is placed in tube furnace, heated up with 5 DEG C/min heating rate
To 300 DEG C, then isothermal reaction 1 hour naturally cools to room temperature;Products therefrom is washed with water to neutrality, then in forced air drying
Dried 6 hours for 60 DEG C in case, that is, obtain activating three-dimensional grapheme/nickel foam negative material.
Fig. 6 schemes for the SEM of the present embodiment products therefrom.
Performance test is carried out to the product of the present embodiment by the identical method of embodiment 1, as a result shown:Its ratio that discharges first
Capacity is that 126mAh/g, charge specific capacity are 145mAh/g, and specific discharge capacity is 128mAh/g, charge specific capacity after circulation 20 times
For 122mAh/g.
Embodiment 7
The present embodiment prepares lithium ion battery activation three-dimensional grapheme/nickel foam as follows:
1) by graphene oxide ultrasonic disperse in water, 6mg/mL graphene oxide water solution is obtained;Then by 0.16g
Nickel foam is immersed in 10mL graphene oxide water solutions, with the deposited oxide graphene in nickel foam, obtains three-dimensional oxidation stone
Black alkene/foam nickel material;
2) three-dimensional graphene oxide/foam nickel material is impregnated in 3mol/L KOH solution, taken after standing 48 hours
Go out, obtain activating three-dimensional graphene oxide/foam nickel material;
3) the three-dimensional graphene oxide/foam nickel material of activation is placed in tube furnace, heated up with 5 DEG C/min heating rate
To 400 DEG C, then isothermal reaction 1 hour naturally cools to room temperature;Products therefrom is washed with water to neutrality, then in forced air drying
Dried 6 hours for 60 DEG C in case, that is, obtain activating three-dimensional grapheme/nickel foam negative material.
Performance test is carried out to the product of the present embodiment by the identical method of embodiment 1, Fig. 7 is its charge-discharge performance figure.
As a result show, its first discharge specific capacity is that 592mAh/g, charge specific capacity are 146mAh/g, specific discharge capacity after circulation 20 times
It is 104mAh/g for 90mAh/g, charge specific capacity.
Embodiment 8
The present embodiment prepares lithium ion battery activation three-dimensional grapheme/nickel foam as follows:
1) by graphene oxide ultrasonic disperse in water, 6mg/mL graphene oxide water solution is obtained;Then by 0.16g
Nickel foam is immersed in 10mL graphene oxide water solutions, with the deposited oxide graphene in nickel foam, obtains three-dimensional oxidation stone
Black alkene/foam nickel material;
2) three-dimensional graphene oxide/foam nickel material is impregnated in 3mol/L KOH solution, taken after standing 48 hours
Go out, obtain activating three-dimensional graphene oxide/foam nickel material;
3) the three-dimensional graphene oxide/foam nickel material of activation is placed in tube furnace, heated up with 5 DEG C/min heating rate
To 600 DEG C, then isothermal reaction 1 hour naturally cools to room temperature;Products therefrom is washed with water to neutrality, then in forced air drying
Dried 6 hours for 60 DEG C in case, that is, obtain activating three-dimensional grapheme/nickel foam negative material.
Performance test is carried out to the product of the present embodiment by the identical method of embodiment 1, Fig. 8 is its charge-discharge performance figure.
As a result show:Its first discharge specific capacity is that 520mAh/g, charge specific capacity are 230mAh/g, specific discharge capacity after circulation 20 times
It is 104mAh/g for 108mAh/g, charge specific capacity.
Embodiment 9
The present embodiment prepares lithium ion battery activation three-dimensional grapheme/nickel foam as follows:
1) by graphene oxide ultrasonic disperse in water, 6mg/mL graphene oxide water solution is obtained;Then by 0.16g
Nickel foam is immersed in 10mL graphene oxide water solutions, with the deposited oxide graphene in nickel foam, obtains three-dimensional oxidation stone
Black alkene/foam nickel material;
2) three-dimensional graphene oxide/foam nickel material is impregnated in 3mol/L KOH solution, taken after standing 48 hours
Go out, obtain activating three-dimensional graphene oxide/foam nickel material;
3) the three-dimensional graphene oxide/foam nickel material of activation is placed in tube furnace, heated up with 5 DEG C/min heating rate
To 800 DEG C, then isothermal reaction 1 hour naturally cools to room temperature;Products therefrom is washed with water to neutrality, then in forced air drying
Dried 6 hours for 60 DEG C in case, that is, obtain activating three-dimensional grapheme/nickel foam negative material.
Performance test is carried out to the product of the present embodiment by the identical method of embodiment 1, Fig. 9 is its charge-discharge performance figure.
As a result show:Its first discharge specific capacity is 955mAh/g, and charge specific capacity is 660mAh/g, specific discharge capacity after circulating 20 times
For 683mAh/g, charge specific capacity is 664mAh/g.
Comparative example
The present embodiment prepares lithium ion battery three-dimensional grapheme/nickel foam as follows:
1) by graphene oxide ultrasonic disperse in water, 6mg/mL graphene oxide water solution is obtained;Then by 0.16g
Nickel foam is immersed in 10mL graphene oxide water solutions, with the deposited oxide graphene in nickel foam, obtains three-dimensional oxidation stone
Black alkene/foam nickel material;
2) three-dimensional graphene oxide/foam nickel material is placed in tube furnace, be warming up to 5 DEG C/min heating rate
300 DEG C, then isothermal reaction 1 hour naturally cools to room temperature;Products therefrom is washed with water to neutrality, then in air dry oven
In 60 DEG C dry 6 hours, that is, obtain three-dimensional grapheme/nickel foam negative material.
Performance test is carried out to the product of the present embodiment by the identical method of embodiment 1, Figure 10 is its charge-discharge performance figure.
As a result show:Its first discharge specific capacity is that 153mAh/g, charge specific capacity are 87mAh/g, specific discharge capacity after circulation 20 times
It is 73mAh/g for 77mAh/g, charge specific capacity.
These are only presently preferred embodiments of the present invention, be not intended to limit the invention, it is all the present invention spirit and
Any modifications, equivalent substitutions and improvements made within principle etc., should be included in the scope of the protection.
Claims (4)
1. a kind of lithium ion battery preparation method of activation three-dimensional grapheme/nickel foam, it is characterised in that including following step
Suddenly:
1) by graphene oxide ultrasonic disperse in water, graphene oxide water solution is obtained;Then nickel foam is immersed in described
In graphene oxide water solution, with the deposited oxide graphene in nickel foam, three-dimensional graphene oxide/foam nickel material is obtained;
2) the three-dimensional graphene oxide/foam nickel material is impregnated in KOH solution, takes out, obtain after standing 24-48 hours
Three-dimensional graphene oxide/the foam nickel material of activation;
3) the three-dimensional graphene oxide/foam nickel material of the activation is placed in tube furnace, is warming up to 300-800 DEG C, constant temperature is anti-
Answer 1-3 hours, then naturally cool to room temperature;Products therefrom is washed with water to neutrality, then the 40-60 DEG C of baking in air dry oven
It is dry 3-6 hours, that is, obtain for activation three-dimensional grapheme/nickel foam as lithium ion battery negative material.
2. the lithium ion battery according to claim 1 preparation method of activation three-dimensional grapheme/nickel foam, its feature exists
In:Step 1) described in graphene oxide water solution concentration be 0.5-6mg/mL.
3. the lithium ion battery according to claim 1 preparation method of activation three-dimensional grapheme/nickel foam, its feature exists
In:Step 2) described in KOH solution concentration be 2-6mol/L.
4. the lithium ion battery according to claim 1 preparation method of activation three-dimensional grapheme/nickel foam, its feature exists
In:Step 3) in heating rate be 5-10 DEG C/min.
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CN108063252A (en) * | 2017-12-14 | 2018-05-22 | 合肥国轩电池材料有限公司 | A kind of activation method of cathode material for high capacity lithium ion battery |
CN108417811A (en) * | 2018-03-26 | 2018-08-17 | 电子科技大学 | A kind of carbon coating club shaped structure ternary ferrimanganic sulfide graphene composite material and its synthetic method |
CN108550849A (en) * | 2018-05-08 | 2018-09-18 | 佛山市瑞生海特生物科技有限公司 | A kind of foamable three-dimensional graphene sodium ion battery electrode material and preparation method thereof |
CN109524247A (en) * | 2017-09-18 | 2019-03-26 | 天津大学 | 3D- graphene/nickel foam and its preparation method and application |
CN111807416A (en) * | 2020-07-22 | 2020-10-23 | 哈尔滨工业大学 | Preparation method of hollow tubular structure FeOOH @ rGO lithium ion battery anode material |
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CN111807416A (en) * | 2020-07-22 | 2020-10-23 | 哈尔滨工业大学 | Preparation method of hollow tubular structure FeOOH @ rGO lithium ion battery anode material |
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